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34133 Publications

Spin-Torque Devices Based on MgO-Based Magnetic Tunnel Junctions

Deac, A. M.

Spin-torque nano-oscillators (STNOs) are novel devices which may be exploited for wireless communication applications [1-3]. In particular, it has recently been demonstrated that STNOs utilizing an in-plane magnetized polarizer (also acting as read-out layer) and out-of-plane magnetized free layer allow for the full parallel-to-antiparallel resistance variation to be exploited in the limit of 90° precession angle, thereby maximizing the output power [1]. However, for this specific geometry, steady-state precession can only be sustained if the spin-transfer torque exhibits an asymmetric dependence on the angle between the free and the polarizing layer, such as in the case of fully metallic devices [1]. Nevertheless, it has recently been reported that dynamics have been experimentally observed in similarly designed MgO-based magnetic tunnel junctions (MTJs) under constant applied electrical current, in spite of the fact that such devices do not exhibit any asymmetry in the spin-torque angular dependence [4,5]. These results have so far been interpreted based on the formalism for metallic devices.

Here, we explore potential mechanisms for sustaining steady-state precession in MgO-based STNOs with this specific geometry. To this end, we analytically and numerically solve the Landau-Lifshitz-Gilbert-Slonczewski equation under a constant perpendicular applied current and field. We take into account both the angular and the bias dependence of the resistance of the nanopillar in order to convert the current into voltage, which is the relevant parameter in an MgO-MTJ. The field-like torque is neglected. We demonstrate that the angular dependence of the resistance introduces sufficient asymmetry of the in-plane spin-torque term to sustain precession in this system, but the bias dependence of the resistance gradually quenches this asymmetry as the current is increased and consequently suppresses precession above a given threshold. We furthermore prove that in an STNO with circular cross-section an external field is required to observe steady-state dynamics, but this constraint is lifted when introducing an in-plane easy axis, which opens new avenues to be explored for designing devices for mobile communication.

[1] W. H. Rippard, A. M. Deac, M. R. Pufall, et al., Physical Review B 81, 014426 (2010).
[2] A. M. Deac, A. Fukushima, H. Kubota, et al., Nature Physics 4, 308 (2008).
[3] S. I. Kiselev, J. C. Sankey, I. N. Krivorotov, et al., Nature 425, 380 (2003).
[4] H. Kubota, K. Yakushiji, A. Fukushima, et al., Applied Physics Express 6, 103003 (2013).
[5] T. Taniguchi, H. Arai, S. Tsunegi, et al., Applied Physics Express 6, 123003 (2013).

Keywords: magnetism; magnetic tunnel junctions; spin-transfer torque

  • Invited lecture (Conferences)
    Spin Dynamics in Nanostructures Gordon Research Conference Nanoscale Spintronics with Magnons, Phonons, and Photons, 26.-31.07.2015, The Hong Kong University of Science and Technology, China

Publ.-Id: 22314

International research environment and career development

Deac, A. M.

This talk provides mentoring for students seeking an international career.

Keywords: carrer development

  • Invited lecture (Conferences)
    Spin Dynamics in Nanostructures (GRS) Gordon Research Seminar Interplay of Spin, Charge and Lattice Dynamics, 25.-26.07.2015, The Hong Kong University of Science and Technology, China

Publ.-Id: 22313

Zero-field precession and suppression of the output power due to the biasdependence of the TMR in MgO-based spin-torque oscillators Alina Maria Deac

Kowalska, E.; Sluka, V.; Fowley, C.; Kakay, A.; Aleksandrov, Y.; Lindner, J.; Deac, A. M.; Fassbender, J.

Spin-torque nano-oscillators (STNOs) are novel devices which may be exploited for wireless
communication applications [1-3]. In particular, it has recently been demonstrated that STNOs utilizing an in-plane magnetized polarizer (also acting as read-out layer) and out-of-plane magnetized free layer allow for the full parallel-to-antiparallel resistance variation to be exploited in the limit of 90° precession angle, thereby maximizing the output power [1]. However, for this specific geometry, steady-state precession can only be sustained if the spin-transfer torque exhibits an asymmetric dependence on the angle between the free and the polarizing layer, such as in the case of fully metallic devices [1]. Nevertheless, it has recently been reported that dynamics have been experimentally observed in similarly designed MgO-based magnetic tunnel junctions (MTJs) under constant applied electrical current, in spite of the fact that such devices do not exhibit any asymmetry in the spin-torque angular dependence [4,5]. These results have so far been interpreted based on the formalism for metallic devices.

Here, we explore potential mechanisms for sustaining steady-state precession in MgO-based STNOs with this specific geometry. To this end, we analytically and numerically solve the Landau-Lifshitz-Gilbert-Slonczewski equation under a constant perpendicular applied current and field. We take into account both the angular and the bias dependence of the resistance of the nanopillar in order to convert the current into voltage, which is the relevant parameter in an MgO-MTJ. The field-like torque is neglected. We demonstrate that the angular dependence of the resistance introduces sufficient asymmetry of the in-plane spin-torque term to sustain precession in this system, but the bias dependence of the resistance gradually quenches this asymmetry as the current is increased and consequently suppresses precession above a given threshold. We furthermore prove that in an STNO with circular cross-section an external field is required to observe steady-state dynamics, but this constraint is lifted when introducing an in-plane easy axis, which opens new avenues to be explored for designing devices for mobile communication.

[1] W. H. Rippard, A. M. Deac, M. R. Pufall, et al., Physical Review B 81, 014426 (2010).
[2] A. M. Deac, A. Fukushima, H. Kubota, et al., Nature Physics 4, 308 (2008).
[3] S. I. Kiselev, J. C. Sankey, I. N. Krivorotov, et al., Nature 425, 380 (2003).
[4] H. Kubota, K. Yakushiji, A. Fukushima, et al., Applied Physics Express 6, 103003 (2013).
[5] T. Taniguchi, H. Arai, S. Tsunegi, et al., Applied Physics Express 6, 123003 (2013).

Keywords: magnetism; spin-transfer torque; magnetic tunnel junction

  • Invited lecture (Conferences)
    20th International Conference on Magnetism, 06.-10.07.2015, Barcelona, Spain
  • Poster
    12th Japanese-German Frontiers of Science Symposium 2015, 01.-04.10.2015, Kyoto, Japan

Publ.-Id: 22312

Atomic transport during solid-phase epitaxial recrystallization of amorphous germanium

Radek, M.; Bracht, H.; Mccallum, J. C.; Johnson, B. C.; Posselt, M.; Liedke, B.

The atomic mixing of matrix atoms during solid-phase-epitaxy (SPE) is studied by means of isotopically enriched germanium (Ge) multilayer structures grown by molecular beam epitaxy on natural Ge wafers. The entire isotope structure and parts of the natural Ge wafer were preamorphized by Ge implantation. Recrystallization of the amorphous Ge layer is performed at temperatures between 350 ˚C and 450 ˚C. The position of the amorphous/crystalline (a/c) interface was monitored during SPE regrowth using a time-resolved-reflectivity (TRR) system. The SPE process was stopped before the a/c interface reached the surface, i.e, before the recrystallization of the amorphous layer was completed. Secondary-ion-mass-spectrometry (SIMS) was applied to determine the self-atom distribution within the amorphous and recrystallized part of each sample. An upper limit of 0.5 nm is determined for the displacement length of the matrix atoms. This small displacement length is consistent with theoretical models and atomistic simulations of SPE predicting that bond-switching with nearest-neighbours across the a/c interface controls the SPE regrowth.

Keywords: Germanium; Solid-phase epitaxial recrystallization; atomic transport; isotope multilayers

  • Poster
    28th International Conference on Defects in Semiconductors (ICDS 2015), 27.-31.07.2015, Espoo, Finland

Publ.-Id: 22311

Characterisation and properties of f-element complexes with amide and amidine ligands

März, J.; Schmid, M.; Ikeda-Ohno, A.

The lanthanide (Ln) complexes with N-chelating ligands have attracted considerable attentions because of their unique tuneable steric and electronic properties.[1] Amongst such Ln complexes with N-chelating ligands, amide-based complexes are known to offer a wide range of applications, e.g., as efficient luminescent agents employed in bio-analytical fields.[2] Furthermore, amidine-based complexes enable the Ln metals to stabilise in exotic oxidation states (i.e., di- and tetravalent) with remarkable catalytic activity.[3]
These unique properties of amide- and amidine-based complexes of f-elements motivate us to perform the present study focusing on the synthesis and characterisation of the f-element complexes with newly synthesised amide- and amidine ligands shown in Figure 1. The aim of this study is to investigate the physical/chemical properties (e.g., optical properties) of f-elements (i.e., Ln and actinides (An)) complexed with the amide- and amidine ligands and compare their properties between Ln and An, and between solid and solution states, by means of single-crystal X-ray diffraction, X-ray absorption spectroscopy, etc. A comprehensive overview of the amide- and amidine complexes of f-elements will be presented particularly in terms of structural point of view.

1 A. A. Trifonov, Coord. Chem. Rev. 2010, 254, 1327 –1347.
2 e.g., Y. Tang et al., Inorg. Chem. Commun. 2005, 8, 1018-1021; J. Xu et al., J. Am. Chem. Soc. 2011, 133, 19900–19910.
3 F. T. Edelmann, Chem. Soc. Rev. 2009, 38, 2253-2268.

Keywords: lanthanide; actinide; complex; amide; amidine; single-crystal XRD

  • Poster
    International conference on f-elements, 06.-09.09.2015, Oxford, United Kingdom

Publ.-Id: 22310

Dilute ferromagnetic InMnP

Khalid, M.; Weschke, E.; Skorupa, W.; Helm, M.; Zhou, S.

We have synthesized a new magnetic semiconductor,InMnP, by Mn ion implantation and pulsed laser annealing [1, 2]. Clear ferromagnetic hysteresis loops and a perpendicular magnetic anisotropy are observed up to a Curie temperature of 42 K. Large values of negative magnetoresistance and magnetic circular dichroism as well as anomalous Hall effect are further evidences of a ferromagnetic order in InMnP. An effort is made to understand the transport mechanism in InMnP using the theoretical models. We find that the valence band of InP does not merge with the impurity band of the heavily doped InMnP (8 %). Our results suggest that impurity band conduction is a characteristic of Mn‐doped InP and GaP which have deep Mn‐ cceptor levels. [1] M. Khalid, et al., Phys. Rev. B 89, 121301(R) (2014) [2] M. Khalid, et al., J. Appl. Phys. 117, 043906 (2015).

  • Poster
    20th International Conference on Mangetism, 05.-10.07.2015, Barcelona, Spain

Publ.-Id: 22309

Mid-infrared ridge waveguide in MgO:LiNbO3 crystal produced by combination of swift O5+ ion irradiation and precise diamond blade dicing

Cheng, Y.; Lv, J.; Akhmadaliev, S.; Zhou, S.; Kong, Y.; Chen, F.

We report on the fabrication of ridge waveguide operating at mid-infrared wavelength in MgO:LiNbO3 crystal by using O5+ ion irradiation and precise diamond blade dicing. The waveguide shows good guiding properties at the wavelength of 4 μm along the TM polarization. Thermal annealing has been implemented to improve the waveguiding performances. The propagation loss of the ridge waveguide has been reduced to be 1.0 dB/cm at 4 μm after annealing at 310 °C. The micro-Raman spectra indicate that the microstructure of the MgO:LiNbO3 crystal has no significant change along the ion track after swift O5+ ion irradiation.

Keywords: Optical waveguide; MgO:LiNbO3 crystal; Ion irradiation; Diamond blade dicing; Mid-infrared waveguides

Publ.-Id: 22308

Enhancing Robustness and Applicability of Contactless Inductive Flow Tomography

Ratajczak, M.; Wondrak, T.; Zürner, T.; Stefani, F.

Measuring the flow velocity in hot, chemically aggressive and opaque melts is a challenging task even for today’s measurement techniques. The contactless inductive flow tomography (CIFT) could provide a solution by applying magnetic fields to an electrically conducting melt and measuring the small flow-induced magnetic perturbances outside of the container. In this paper we will demonstrate how the robustness of CIFT can be enhanced by means of excitation with time-harmonic magnetic fields, making it more insensitive to the ubiquitous changes of the environmental magnetic field. Further we will show how the problem of an electrically conducting container can be treated, which is necessary, e.g., for industrial application in continuous casting.

  • Contribution to proceedings
    IEEE Sensors 2015, 01.-04.11.2015, Busan, Südkorea
    Proceedings of IEEE Sensors 2015, 662-665
  • Lecture (Conference)
    IEEE Sensors 2015, 01.-04.11.2015, Busan, Südkorea

Publ.-Id: 22307

Ferromagnetism induced by vacancy clusters in Silicon

Liu, Y.; Zhang, X. H.; Yuan, Q.; Han, J. C.; Zhou, S. Q.; Song, B.

Defect-induced ferromagnetism provides an alternative for organic and semiconductor spintronics. Though it is weak, it can be stable above room temperature. Till now it has been confirmed at least in oxides [1, 2] and carbon based materials [3, 4]. Interestingly, the relation between magnetism and defects in Silicon was demonstrated decades ago [5]. Since then, some progresses were made [6-9] and push forward the research of magnetic Mn doped Si a lot but it is drawn little attention itself. Here, with the latest growth purifying technique and sensitive measurements, we investigated the magnetism in Silicon after neutron irradiation and try to correlate the observed magnetism to particular defects in Si.

Keywords: defect-induced ferromagnetism; silicon; neutron irradiation; semiconductors

  • Poster
    28th International Conference on Defects in Semiconductors, 27.-31.07.2015, Espoo, Finland

Publ.-Id: 22306

Strong Auger scattering in Landau-quantized graphene evidenced by circularly polarized pump-probe spectroscopy

Winnerl, S.; Mittendorff, M.; Wendler, F.; Malic, E.; Knorr, A.; Schneider, H.; Helm, M.

While the carrier dynamics in graphene in absence of magnetic fields is well researched in a large spectral range ranging from UV to THz, the dynamics in Landau quantized graphene is almost unexplored. We investigate the carrier dynamics within the system of Landau levels (LLs) of index n = -1, n = 0 and n = 1 by pump-probe experiments complemented by microscopic modelling. Using circularly polarized terahertz radiation (at 18 THz) allows one to selectively excite the two energetically degenerate transitions LL-1 → LL0 and LL0 → LL1, respectively (at B  4 T). While three of the four possible configurations give intuitive results (bleaching, when pumping and probing with the same polarization, induced absorption with opposite polarizations), surprisingly, one configuration counterintuitively leads to bleaching while pumping and probing with opposite polarizations (Fig. 1 lower panel). This implies that even though LL0 is being optically pumped, its population decreases [1] ! Calculations show that LL0 is actually depleted by strong Auger scattering. Note that the two configurations shown in the Figure are distinguishable only because of the slight (n-type) doping of the graphene sample.
We discuss the role of carrier-carrier and carrier-phonon scattering in Landau quantized graphene and provide an outlook on the application potential of this system for tunable THz lasers.

Keywords: Graphene; Landau levels; carrier relaxation; pump-probe; free electron laser

  • Lecture (Conference)
    Electronic Properties Of Two-Dimensional Electron Systems (EP2DS-21), 26.-31.07.2015, Sendai, Japan

Publ.-Id: 22305

Effect of an upward magnetic field on nanosized sulfide precipitation in ultra-low carbon steel

Duan, K. J.; Zhang, L.; Yuan, X. Z.; Han, S. S.; Liu, Y.; Huang, Q. S.

An induction levitation melting (ILM) refining process is performed to remove most microsized inclusions in ultra-low carbon steel (UCS). Nanosized, spheroid shaped sulfide precipitates remain dispersed in the UCS. During the ILM process, the UCS is molten and is rotated under an upward magnetic field. With the addition of Ti additives, the spinning molten steel under the upward magnetic field ejects particles because of resultant centrifugal, floating, and magnetic forces. Magnetic force plays a key role in removing sub-micrometer-sized particles, composed of porous aluminum titanate enwrapping alumina nuclei. Consequently, sulfide precipitates with sizes less than 50 nm remain dispersed in the steel matrix. These findings open a path to the fabrication of clean steel or steel bearing only a nanosized strengthening phase.

Keywords: ultra-low carbon steel; magnetic field; sulfide precipitation; induction levitation; titanium

Publ.-Id: 22304

Comparative study of ultrafast X-ray tomography and wire-mesh sensors for vertical gas-liquid pipe flows

Banowski, M.; Beyer, M.; Szalinski, L.; Lucas, D.; Hampel, U.

At the Institute of Fluid Dynamics of the Helmholtz-Zentrum Dresden-Rossendorf the wire-mesh sensor and the ultrafast X-ray tomography were developed to investigate two-phase flows with high spatial and temporal resolution. In the TOPFLOW facility, a test section was constructed for a comparative study of wire-mesh sensors and ultrafast X-ray tomography. Due to a minimum vertical distance between X-ray and wire-mesh positions, the results can be compared directly neglecting flow developing effects. Varying water and air superficial velocities in a wide range, flow regimes from bubble flow via slug flow to annular flow were investigated. Four typical experimental results are presented and discussed in this paper. Finally, the application ranges for both measurement techniques are briefly discussed.

Keywords: X-ray tomography; Wire-mesh sensor; vertical pipe; two-phase flow

  • Contribution to proceedings
    7th International Symposium on Process Tomography, 01.-03.09.2015, Dresden, Deutschland
  • Lecture (Conference)
    7th International Symposium on Process Tomography, 01.-03.09.2015, Dresden, Deutschland
  • Flow Measurement and Instrumentation 53(2017), 95-106
    DOI: 10.1016/j.flowmeasinst.2016.02.001

Publ.-Id: 22303

In-situ observation of 3D particle assembly

Josten, E.; Wetterskog, E.; Glavic, A.; Boesecke, P.; Rücker, U.; Bergström, L.; Brückel, T.

The self-assembly of magnetic nanoparticles has a high potential for future applications [1], as it allows mass production processes of very small structures without the use of expensive equipment. The process itself is complex, including several interactions between nanoparticles, solvent, and substrate. A deeper understanding is the key for a better control of the self-organization process.

The present work adds a novel quantitative contribution to the study of the kinetics in 3D long range ordered nanoparticle superstructures. These superstructures have been investigated in-situ during the self-assembly using an optimized GISAXS setup to explore the dynamic growthmodes during deposition. The nanoparticles investigated are well-characterized γ-Fe2O3 nanospheres [2,3], which have been deposited on a substrate to form an ensemble of highly ordered superstructures (mesocrystals) [4].

The time-dependent GISAXS study of the self-assembly process, carried out at the ID01 beamline at ESRF, resulted in an understanding of how the structures evolve with time and how the evaporation can be controlled by external parameters. The in-situ cell (fig.1), which was developed to monitor the structure as well as the height and shape of the droplet, was employed for additional control of the process parameters and the possibility of an accurate identification of key physical parameters governing the process. The time evolution of the ordering process was analyzed by fitting position and width of multiple peaks for all recorded GISAXS patterns (for example fig.2). New insights into the drying and self-assembly process of an ensemble of 3D highly ordered superstructures were obtained and evaporation time-dependent stages of the mesocrystal growth and their spatial positions were identified [5].

Keywords: magnetic nanoparticles; in-situ GISAXS; self-assembly; X-ray scattering; mesocrystals

  • Lecture (Conference)
    GISAS2015, 08.-11.09.2015, Nice, Frankreich
  • Poster
    GISAXS2016 workshop, 16.-18.11.2016, Hamburg, Deutschland

Publ.-Id: 22302

Reduction of phase noise in nanowire spin orbit torque oscillators

Yang, L.; Verba, R.; Tiberkevich, V.; Schneider, T.; Smith, A.; Duan, Z.; Youngblood, B.; Lenz, K.; Lindner, J.; Slavin, A. N.; Krivorotov, I. N.

Spin torque oscillators (STOs) are compact, tunable sources of microwave radiation that serve as a test bed for studies of nonlinear magnetization dynamics at the nanometer length scale. In particular, the spin torque in an STO can be created by spin-orbit interaction, but low spectral purity of the microwave signals generated in spin orbit torque oscillators hinders practical applications of these magnetic nanodevices. Here we demonstrate a method for decreasing the phase noise of spin orbit torque oscillators based on Pt/Ni80Fe20 nanowires. We experimentally demonstrate that tapering of the nanowire, which serves as the STO active region, significantly decreases the spectral linewidth of the generated signal. We explain the observed linewidth narrowing in the framework of Ginzburg-Landau auto-oscillator model. The model reveals that spatial non-uniformity of the spin current density in the tapered nanowire geometry hinders the excitation of higher order spin-wave modes, thus stabilizing the single-mode generation regime. This non-uniformity also generates a restoring force acting on the excited self-oscillatory mode, which reduces thermal fluctuations of the mode spatial position along the wire. Both these effects improve the STO spectral purity.

Keywords: n.n

Publ.-Id: 22301

Stability of MR brain-perfusion measurement using arterial spin labeling

Petr, J.; Hofheinz, F.; Platzek, I.; Schramm, G.; van den Hoff, J.

Arterial spin labeling (ASL) is an MR technique for assessment of cerebral blood flow (CBF) that does not require use of contrast agents which makes it a less invasive alternative to the 15O-H2O-PET measurement. The repeatability of ASL has been studied extensively but mainly in young healthy volunteers. We have tested repeatability of ASL under realistic clinical conditions in elderly brain tumor patients acquired with a Philips Ingenuity TF PET/MR in the context of an ongoing 11C-Methionine PET/MR study. Twenty three patients (age 54.8±13.0 y) were scanned on two or more session. The patients underwent 6 weeks of concurrent radiochemotherapy with Temozolomide between the first session and second measurement. The mean relative difference of gray matter CBF was 18.6% between the first two session and 13.0% for the second session and further on. The mean gray matter CBF was 46.6±7.2 mL/min/100 g on the first sessions and there was a significant decrease of 9.8% between first and second session (p=0.027). In summary, the ASL presents measurement of CBF with reasonable repeatability also in elderly patients under clinical conditions when it is not possible to control for all sources of variation. Significant decrease of CBF in healthy tissue was observed after the radiochemotherapy. Prospectively, the ASL data together with the also acquired 11C-Methionine PET will be evaluated regarding their separate and combined ability to predict patient outcome and effectiveness of the performed radiochemotherapy.

  • Lecture (Conference)
    PSMR 2015: 4th Conference on PET/MR and SPECT/MR, 17.-21.05.2015, La Biodola, Isola d’Elba, Italy
  • Open Access Logo Abstract in refereed journal
    EJNMMI Physics 2(2015)Suppl. 1, A67
    DOI: 10.1186/2197-7364-2-S1-A67

Publ.-Id: 22300

Measuring the Influence of Vessel Geomery on PCASL Labeling Efficiency

Petr, J.; Schramm, G.; van den Hoff, J.

TARGET AUDIENCE: Clinicians and researcher interested in efficient planning of the pseudo-continuous arterial spin labeling (ASL).
PURPOSE: The labeling efficiency of pseudo-continuous ASL1 (pCASL) and its inter- and intra-subject reproducibility is a crucial point for reliable cerebral-blood-flow (CBF) measurements with ASL. Potential causes of varying labelling efficiency are, for example, B0 field inhomogeneity2, blood velocity3, or labeling-plane positioning3. The common recommendation is to position the labeling plane on a straight part of the vessel and perpendicular to them6. However, it is not always possible to avoid tortuous parts of the vessels if angiography is not available. Here, we study the effect of vessel geometry on the labeling efficiency both trough simulations and experiments.
METHODS: Simulations: Labeling efficiency was calculated for three cases of vessels geometry using numerical simulations as described by Wu4. Blood velocities between 1 and 40 cm/s were investigated and laminar flow was assumed. First, efficiency was calculated for a plane perpendicular to a straight vessel and angulated at 12.5°, 22.5°, or 45°. Second, a simple bend of the vessel was assumed with a length of the horizontal section of 0, 5, or 10 mm and the labeling plane positioned on the center of it and 2, 6, or 12 mm below (see Fig. 1a). Third, the bend was rotated 0°, 12.5°, 22.5°, or 45° so that the labeling plane intersected the vessel three times (Fig. 1b). Acquisitions: Five healthy young volunteers (age 31.8±3.9 y) were scanned at 3T using an eight-channel head-coil. A 3D TFE T1-weighted sequence and five pCASL sequences (pCASL1-pCASL5) with different position of the labeling plane were acquired. The T1-weighted sequence had voxel size 1×1×1 mm3. The common parameters of the pCASL sequence were: TR/TE = 3765/11 ms, FOV = 220×220 mm2,
pixel size = 2.75×2.75×6 mm3, 17 slices (0.6 mm gap), flip angle = 90°, 20 averages, background suppression with 2 pulses, 2D multi-slice EPI readout, labeling with a Hanning RF-pulse with duration 0.5 ms, tip angle 18°, and inter-pulse pause 0.5 ms, labeling time/post-labeling delay 1525/1650 ms. A reference image was acquired 5000 ms after saturation. For pCASL1, the labeling plane was set parallel with the imaged slices and the gap
was set in a way that the labeling plane intersected vertebral arteries (VA) at the level of siphon. The labeling plane was placed as parallel to the horizontal section of the VAs as possible (Fig. 1c). For pCASL2,3, the labeling plane was positioned 6 and 12 mm lower, respectively, than in pCASL1 (Fig. 1c). In pCASL4, 5 the labeling plane was positioned as in pCASL3 and rotated in the sagittal plane -30° and 30° with the center of rotation in the internal
carotid arteries (ICA), see Fig. 1c.
Preprocessing: The dynamics of all sequences were aligned with the first dynamics of pCASL1, thus coregistering the sequences and compensating for motion within each sequence. The T1-weighted image was aligned to the mean control image and segmented to obtain partial volume fractions for gray matter (GM). CBF was quantified according to the ASL white-paper6. Mean CBF (GM > 70%) in the vascular territories corresponding to the anterior cerebral artery (ACA), posterior cerebral artery (PCA), middle cerebral artery (MCA), and vertebral artery (VA) were computed for each sequence and subject. For pCASL1,2,4,5, the relative difference of the
mean CBF for each region was calculated relative to pCASL3 which was considered optimal as it contained no twists or angulations.
RESULTS: According to the numerical simulations, the decrease in labeling efficiency due to plane angulation is under 5% for most blood velocities and angle up to 30°, but it can go up to 10% for 45° angulation (Fig. 2c). For a bend in the vessel (Fig. 1a) of length 10 mm, the labeling efficiency can be decreased 20-25% (Fig. 2b). With increasing distance of the labeling plane, the decrease is only about 10% at 2mm (Fig. 2a), under 3% at 6mm and under 1% at 12 mm distance. For multiple intersections (Fig. 1b), the labeling efficiency decreased 25-30% regardless of the examined angle. The mean relative difference from sequence pCASL3 for different vascular territories is displayed in Tab. 2.
DISCUSSION: The experiments confirmed that labeling plane shift (pCASL1,2 in Tab. 1) or angulation up to 30° on ICA (pCASL4,5) produced less than 4% change of CBF in the ACA and MCA regions. Positioning the labeling plane on a section of VA parallel with it (pCASL1) caused 5.0% and 14.7% CBF decrease in PCA and VA regions respectively, although only in VA the change was significant. By increasing the distance from the bend (pCASL2), the CBF decrease became lower and not significant. Significant decrease of CBF of 8.4% and 16.9% in both PCA and VA regions, respectively, was achieved by positioning the labeling plane in a way to intersect VA at siphon multiple times. More significant decrease was expected from the simulations. The reason can be, that the actual vessel geometry was different from the worst modeled case. More measurements need to be done to find out why the decrease was lower in PCA than in VA. There are several limitations in this study. The magnetization transfer effects on the label were not taken into account5. Laminar flow profile was assumed, however the vessel thickness with regards to gradient fields was neglected for simplicity. By angulating the labeling plane, it is possible that it can intersect the imaged volume and thus directly or by magnetization transfer effects lower the measured perfusion signal. To minimize influence of this, the pixels where minimal-maximal intensity difference for all sequences was more than 10% were excluded from the analysis.
CONCLUSION: Reasonable angulation of the labeling plane causes only insignificant changes in labeling efficiency and measured CBF. On the other hand, twist and loops of the vessels as well as multiple crossing of the vessels by a labeling plane can cause significant changes of up to 25% and possibly even more, although this has been experimentally demonstrated only in VA region and not in PCA region.
1. W Dai, et al. Magn Reson Med, 2008;60(6):1488–97.
2. H Jahanian, et al. NMR in Biomedicine, 2011;24(10):1202–9.
3. S Aslan, et al. Magn Reson Med, 2010;63(3):765–71.
4. WC Wu, et al. Magn Reson Med, 2007;58(5):1020–7.
5. L Hernandez-Garcia, et al. NMR in Biomedicine, 2007;20(8):733–42.
6. Alsop, et al. Magn Reson Med, 2014; DOI: 10.1002/mrm.25197.

  • Poster
    23rd Annual Meeting of the International Society for Magnetic Resoonance in Medicine (ISMRM), 30.05.-05.06.2015, Toronto, Canada
  • Contribution to proceedings
    23rd Annual Meeting of the International Society for Magnetic Resonance in Medicine (ISMRM), 30.05.-05.06.2015, Toronto, Canada
    ISMRM '15: Proceedings of the 23rd Scientific Meeting and Exhibition of International Society for Magnetic Resonance in Medicine, 2952

Publ.-Id: 22299

An implementation of dead-time corrections in microbeam measurements on a pixel by pixel basis

Munnik, F.

In microbeam measurements on inhomogeneous samples large variations in count-rate can occur. These variations result in variations in dead-time that have to be used to correct elemental distribution maps. However, the dead-time is usually not available on a pixel by pixel basis. In this work, a simple model is proposed to calculate the dead-time for each pixel. Measurements to determine the dead-time per event, needed in the model, are presented and the dead-time corrections are presented for real samples.

  • Poster
    Workshops für Ionenstrahlen und Nanostrukturen, 22.-24.07.2015, Heidelberg, Deutschland

Publ.-Id: 22298

Ionenstrahlanalyseverfahren in der Materialforschung

Schmidt, B.; Wetzig, K.

Der Schwerpunkt der Materialanalyse mittels Ionenstrahlen ist die Bestimmung der Zusammensetzung und Struktur von oberflächennahen Festkörperschichten im Tiefenbereich von wenigen nm bis zu einigen µm. Charakteristisch für die verschiedenen Ionenstrahlanalysetechniken sind die Verwendung geeigneter Ionenstrahlen (z.B. Ionenart, Ionenenergie und -strom, Strahlfokus usw.), die Art der Ionen-Festkörper-Wechselwirkung (und deren Wirkungsquerschnitt), die entstehende Strahlungsart (z.B. gesputterte Sekundärionen, gestreute Ionen sowie Ionen-induzierte Photonen- und Elektronenemission). Die Vielzahl der Ionenstrahl-analyseverfahren kann bezüglich der verwendeten Ionenenergien in drei Gruppen eingeteilt werden [1]: 1) niedrige Ionenenergien von einigen keV, 2) mittlere Ionenenergien im Bereich 30-300 keV, und 3) hohe Ionenenergien im Bereich ~0,5-100 MeV. Schwere Ionen (Mi > Moxygen) für eine hinreichende Sputterausbeute an Targetatomen sind notwendig im weit verbreiteten Verfahren der Sekundärionen-Massen-Spektrometrie (SIMS). Leichte Ionen (M < 10, meistens H+, He+) werden in einem breiten Energiebereich für verschiedene Ionenstreuverfahren (LEIS, MEIS, RBS) sowie verschiedene Verfahren der Ionen-induzierten Photonenemission (PIXE, PIGE) eingesetzt. Dagegen werden schwerere, hochenergetische Ionen (z.B. N, O, Cl usw.) hauptsächlich für NRA und ERDA verwendet.
Im Vortrag werden die verschiedenen Ionenstrahlanalyseverfahren mit ihren charakteristischen Analyseparametern und Einsatzgebieten kurz vorgestellt und miteinander verglichen. Dabei wird besonders auf die hochauflösende Tiefen-profilierung für Dotierungsprofile in Halbleitern und die Elementanalyse von Dünnschichtsystemen eingegangen. Hierfür sind besonders die modernen Mikroelektronik- und Dünnschichttechnologien mit Forderungen nach immer dünneren Schichtsystemen und somit nach steigender Tiefenauflösung sowie kleineren Nachweisgrenzen die treibende Kraft. Weiterhin werden ausgewählte Beispiele für den Einsatz von Ionenstrahlanalyseverfahren in anderen Gebieten der Materialwissenschaften, z.B. in der Kunst und Archäometrie sowie in der Medizin diskutiert.

  • Invited lecture (Conferences)
    18. Tagung Festkörperanalytik, 06.07.2015, Wien, Österreich

Publ.-Id: 22297

Probing defect driven tunable spontaneous magnetization in paramagnetic Zn0.95Co0.05O epitaxial films by X-ray absorption investigations

Satyarthi, P.; Ghosh, S.; Wang, Y.; Zhou, S.; Kumar, P.; Kanjilal, D.; Olivi, L.; Bürger, D.; Skorupa, I.; Schmidt, H.; Srivastava, P.

In order to address existing unresolved issues related to intrinsic and extrinsic origins of ferromagnetism in Zn1−xCoxO based diluted magnetic semiconductors for varying x, the present work aims to investigate the tunable ferromagnetism triggered in paramagnetic Zn0.95Co0.05O films using 500 KeV inert xenon ion irradiation of different fluences. The origin of ferromagnetism in post irradiated Zn0.95Co0.05O films is understood from different densities of bound magnetic polarons (BMPs) formation through correlated spins of tetrahedrally substituted Co2+ ions and anionic vacancies. The alteration in crystallographic positions of Zn, Co cations, and O anions in the tetrahedral environment as analyzed from Zn and Co K-edgeX-ray absorption and O 1s photoemission is a crucial factor for the stabilization of different density of BMPs. Magnetic field and temperature dependence of X-ray magnetic circular dichroism at the Co L2,3 edge provide experimental evidence of purely paramagnetic contribution from well localized Co2+ ions of Co sublattice for paramagnetic Zn0.95Co0.05O film. The paramagnetic Co2+ ions of Co sublattice persist in irradiated films, which reveal BMPs formation as the origin of ferromagnetism.

Keywords: Diluted magnetic semiconductors; X-ray absorption; Spintronics

Publ.-Id: 22296

Identification and quantification of PGMs by combining MLA and EPMA with a new approach to the offline overlap correction of major and trace PGE concentrations

Osbahr, I.; Krause, J.; Bachmann, K.; Gutzmer, J.

The identification and accurate characterisation of platinum-group minerals (PGMs) is usually a very cumbersome procedure due to their small grain size (typically below 10 µm) and inconspicuous appearance under reflected light. A novel strategy for finding and quantifying PGMs by combining mineral liberation analysis (MLA), a point logging system and electron probe microanalysis (EPMA) was thus developed.
As a first step, the PGMs are identified using the MLA. Grains identified as PGMs are then marked and coordinates recorded with the point logger are then transferred to the EPMA. Case studies e.g. from the platiniferous reefs (Merensky Reef and UG2) of the Bushveld Complex (South Africa) illustrate that the combination of MLA, point logger and EPMA results in the identification of a significantly (up to 20 times) higher number of PGM grains than by careful reflected light microscopy.
The analysis of PGEs as major elements in PGMs or as trace elements in e.g. base metal sulfides by EPMA requires considerable effort. Due to the often significant overlaps between the X-ray spectra of almost all platinum-group and associated elements, X-ray lines suitable for quantitative analysis need to be carefully selected. As peak overlaps cannot be avoided completely, an offline overlap correction based on weight proportions has been developed. A reliable overlap correction is of particular importance e.g. in Ru-sulfides as laurite if the overlapped element is a trace element (Rh) and the overlapping element is a major constituent (Ru). Results obtained with the procedure attain acceptable totals and atomic proportions, indicating that the applied corrections are appropriate.

Keywords: Mineral Liberation Analyser; Electron Probe Microanalyser; Offline Overlap Correction; Platinum-Group Minerals

  • Poster
    Goldschmidt2015, 16.-21.08.2015, Prag, Tschechien

Publ.-Id: 22295

A novel approach for efficient identification and accurate chemical characterisation of platinum-group minerals by combining Electron Probe Microanalysis and Mineral Liberation Analysis

Osbahr, I.; Krause, J.; Bachmann, K.; Gutzmer, J.

The identification and accurate characterisation of platinum-group minerals (PGMs) is usually a very cumbersome procedure due to their small grain size (typically below 10 µm) and inconspicuous appearance under reflected light. A novel strategy for finding PGMs and quantifying their composition was developed. It combines SEM-based automated mineralogy, in this study mineral liberation analyser (MLA) Quanta 650F by FEI, a point logging system (JEOL) and a FE-EPMA (JEOL JXA-8530F). Thin sections from a layered intrusion (UG2) in the Bushveld Complex and from two Uralian-Alaskan-type complexes in the Ural Mountains, Russia, were investigated as case studies.
As a first step, the PGMs are identified using the MLA. Grains identified as PGMs are then marked and coordinates recorded and transferred to the EPMA. Case studies illustrate that by introducing MLA for the efficient and largely automated identification of PGM grains in polished thin sections, up to 20 times more PGM grains were identified, whilst shortening time needed and avoiding the effects of human error invariably associated with reflected light microscopy. This is mainly due to the facts that (a) PGM with grain sizes < 5µm are reliably identified and (b) PGM and closely associated base metal sulfides and sulfosalts are well differentiated with the MLA. The analysis of PGMs by EPMA requires considerable effort due to the often significant overlaps between the X-ray spectra of almost all platinum-group and associated elements (e.g. OsMβ on IrMα and AuMβ on HgMα). X-ray lines suitable for quantitative analysis need to be carefully selected. As peak overlaps cannot be avoided completely, an offline overlap correction based on weight proportions has been developed. Considerable variations in the repeatedly determined overlap factors illustrate the need for a re-determination of the overlap factors with each calibration. Results obtained with the procedure proposed in this study attain acceptable totals and atomic proportions, indicating that the applied corrections are appropriate.

Keywords: Mineral Liberation Analyser; Electron Probe Microanalyser; Platinum-Group Minerals; Platinum-group Elements; offline overlap correction

  • Poster
    Geoanalysis 2015 - The 9th International Conference on the Analysis of Geological and Environmental Materials, 09.-14.08.2015, Leoben, Österreich

Publ.-Id: 22294

Working with uncertainty in adaptive process optimisation

van den Boogaart, K. G.; Tolosana Delgado, R.; Matos Camacho, S.

This contribution is concerned with adaptive processing decisions, where the process parameters are optimally adapted to the varying properties of the material input stream. Our starting point is the geometallurgical paradigm that the varying properties of the input stream are considered known e.g. from a geometallurgical model of the mined ore body, and optimal processing parameters are computed from them, by finding the parameter seaming optimal in a computer simulation.
This approach however has to work with a lot of uncertainties: The prediction of the geometallurgical ore parameters can only be done with some geostatistical uncertainty. The parameters themselves are only proxies for true ore properties. Model prediction can differ relevantly from actual process results, due to model simplifications. Due to these uncertainties the computed processing choices can turn out to be inferior to simple non-adaptive processing.
We systematically analysed this effect, by modelling this uncertainty effect mathematically and in computer simulations.
The most important findings are:
(a) Processing choices not taking into account the uncertainty sometimes even perform worse than simple non-adaptive processing, for the sole reason of ignoring the uncertainty effect.
(b) Ore properties, not adequately reflected in the ore description, might require different approaches, in which the observed processing behaviour feeds back into process control.
(c) Bayesian decision theory allows computing optimal processing choices combining the information from the mine (geostatistical predictions) and from the process feedback. These choices give much more robust choices and do not suffer from the drawbacks described for the simple approach we started from.
This new approaches can substantially improve the performance of adaptive processing in existing plants.

Keywords: Geometallurgy; Adpative Processing; Bayesian Optimisation

  • Lecture (Conference)
    IMPC 2016, XXVIII International Mineral Processing Congress, 11.-15.09.2016, Québec, Canada
  • Contribution to proceedings
    IMPC 2016, XXVIII International Mineral Processing Congress, 11.-15.09.2016, Quebec, Canada
    IMPC 2016: XXVIII International Mineral Processing Congress Proceedings: Canadian Institute of Mining, Metallurgy and Petro, 978-1-926872-29-2

Publ.-Id: 22293

Programme IAMG 2015 Freiberg, Germany, September 5-13, 2015, The 17th Annual Conference of the International Association for Mathematical Geosciences

Schaeben, H.; Tolosana Delgado, R.; van den Boogaart, K. G.; van den Boogaart, R.; (Editors)

Das ist das Programmheft der IAMG2015 Konferenz

  • Book (Editorship)
    Freiberg: IAMG Office, 2015
    40 Seiten

Publ.-Id: 22292

Proceedings IAMG 2015 Freiberg, Germany, September 5-13, 2015, The 17th Annual Conference of the International Association for Mathematical Geosciences

Schaeben, H.; Tolosana Delgado, R.; van den Boogaart, K. G.; van den Boogaart, R.; (Editors)

These are the proceedings with the long Abstracts of the IAMG 2015 conference

Keywords: Mathematical Geosciences; Mathematical Geology; Geoinformatics

  • Book (Editorship)
    Freiberg: IAMG Office, 2015
    1372 Seiten
    ISBN: 978-3-00-050337-5

Publ.-Id: 22291

Short Abstracts IAMG 2015 Freiberg, Germany, September 5-13, 2015, The 17th Annual Conference of the International Association for Mathematical Geosciences

Schaeben, H.; Tolosana Delgado, R.; van den Boogaart, K. G.; van den Boogaart, R.; (Editors)

This is the shorts abstracts volume of the IAMG2015 Conference

Keywords: Mathematical Geosciences; Mathematical Geology; Geoinformatics

  • Book (Editorship)
    Freiberg: IAMG Office, 2015
    249 Seiten

Publ.-Id: 22290

Two-photon quantum well infrared photodetectors below 6 THz

Franke, C.; Walther, M.; Helm, M.; Schneider, H.

Two-photon quantum well infrared photodetectors (QWIPs) are nonlinear detectors for the mid-infrared and terahertz regimes optimized for resonant two-photon absorption. Here we present first results on two-photon QWIP samples based on the GaAs/AlGaAs material system with intersubband energies between 25 and 12 meV (6 to 3 THz) confirmed by photocurrent spectra. The dark current showed large discontinuities, presumably caused by impact ionization. We performed interferometric autocorrelation experiments at the free-electron laser FELBE and observed nonlinear interferograms for all samples.

Keywords: quantum well infrared photodetector; QWIP; interferometric autocorrelation; nonlinear optics; two-photon absorption

Publ.-Id: 22289

Innovative once-through thorium fuel cycle for the PTVM LWR concept

Rachamin, R.; Fridman, E.; Galperin, A.

An advanced once-through thorium fuel cycle for the novel reactor concept, termed the pressure tube light water reactor with variable moderator control (PTVM LWR), is proposed. The main innovation of the concept is described. The PTVM LWR makes use of a seed-blanket geometry, whereby the core is divided into separated regions of thorium fuel channel assemblies (blanket) and low-enriched uranium fuel channel assemblies (seed). A scheme based on two separate fuel flow routes (i.e., seed route and blanket route) is proposed. Neutronic analysis indicates that the novel scheme has the potential to utilize both seed and blanket in an efficient manner.

Keywords: pressure tube reactor; “breed & burn”; moderator variation; seed-blanket geometry; once-through thorium fuel cycle

  • Open Access Logo Contribution to proceedings
    Thorium Energy Conference 2015 (ThEC15), 12.-15.10.2015, Mumbai, India
  • Poster
    Thorium Energy Conference 2015 (ThEC15), 12.-15.10.2015, Mumbai, India

Publ.-Id: 22288

Liquid metal modelling of continuous steel casting

Gerbeth, G.; Wondrak, T.; Stefani, F.; Shevchenko, N.; Eckert, S.; Timmel, K.

Model experiments with low melting point liquid metals are an important tool to investigate the flow structure and related transport processes in melt flows relevant for metallurgical applications. We present recent results from the three LIMMCAST facilities working either with room-temperature alloy GaInSn or with the alloy SnBi at temperatures of 200-350°C. The main value of cold metal laboratory experiments consists in the capabilities to obtain quantitative flow measurements with a reasonable spatial and temporal resolution, which is essential for code validation. Experimental results are presented covering the following phenomena: contactless electromagnetic tomography of the flow in the mold, flow monitoring by ultrasonic sensors, mold flow under the influence of an electromagnetic brake, injection of argon bubbles through the stopper rod, X-ray visualization of gas bubble two-phase flow in the nozzle and in the mold.

Keywords: Continuous casting; physical modeling; flow measurements; magnetic field; flow control; electromagnetic brake

  • Invited lecture (Conferences)
    6th Baosteel Biannual Academic Conference and the 10th CSM Steel Congress, 21.-23.10.2015, Shanghai, China
  • Contribution to proceedings
    The 10th CSM Steel Congress and the 6th Baosteel Biennial Academic Conference, 21.-23.10.2015, Shanghai, China
    Proceedings of the 10th CMS Steel Congress & the 6th Baosteel Biennial Academic Conference: Metallurgical Industry Press, Book of Abstracts: 978-7-5024-7006-7, 8-13

Publ.-Id: 22287

Experimentelle Modellierung von Stranggussprozessen mit niedrig schmelzenden Legierungen

Timmel, K.; Wondrak, T.; Röder, M.; Shevchenko, N.; Miao, X.; Stefani, F.; Eckert, S.

Die Strömung der Metallschmalze beim kontinuierlichen Stranggießen hat wesentlichen Einfluss auf das erreichte Gussergebnis. Probleme entstehen beispielsweise durch Einschlüsse von Oxiden, intermetallischen Verbindungen oder Gasblasen, die durch eine unkontrollierte Strömung in die Erstarrungszone gelangen. Die Untersuchung und Optimierung der Strömungsvorgänge erfolgte bisher vorwiegend anhand von numerischen Simulationen sowie Wassermodellen und lieferte bereits viele Erkenntnisse. Aufgrund der Materialeigenschaften sind jedoch Wassermodelle in ihrer Anwendung begrenzt und können nicht alle im Prozess auftretende physikalische Phänomene abdecken, wie z.B. Temperaturgradienten in der Schmelze, Interaktion mit elektromagnetischen Feldern oder Mehrphasenströmungen. In diesen Fällen unterscheiden sich die Kennzahlen z.T. um mehrere Größenordnungen.
Am Helmholtz-Zentrum Dresden-Rossendorf stehen drei Anlagen zur Verfügung, welche sich mit der Modellierung des Stranggussprozesses unter der Verwendung niedrigschmelzender Legierungen befassen. Die Anlagen unterscheiden sich z.T. in der Ausrichtung ihrer Untersuchungsschwerpunkte und ergänzen sich so gegenseitig ideal. Das Mini-LIMMCAST Experiment arbeitet mit einer bei Raumtemperatur flüssigen Legierung und ist sehr flexibel aufgebaut. Viele unterschiedliche Untersuchungen können und sind hier bereits durchgeführt worden. Die große LIMMCAST-Anlage ist insbesondere für einen längeren kontinuierlichen Betrieb ausgelegt und operiert im Temperaturbereich von 200 – 350 °C. Die dritte Anlage X-LIMMCAST ist speziell für die Röntgenbildgebung und die Visualisierung der Zweiphasenströmung mit Gasblasen konzipiert. Die Flexibilität der Anlagen erlaubt eine Anpassung an konkrete Gegebenheiten.
Neben den experimentellen Anlagen müssen für einen sinnvollen Betrieb auch entsprechende Messtechniken zu Erfassung der Strömungsvorgänge in flüssigen Metallen zur Verfügung stehen. Für die Geschwindigkeitsmessung sind dazu in den Versuchen die Ultraschall-Doppler-Velocimetry, die kontaktlose, induktive Strömungstomographie und die Potentialsondenmethode zum Einsatz gekommen. Für die Auflösung der Zweiphasenströmung sind wiederum eine tomographische Methode als auch die Röntgenbildgebung verwendet worden. Ziel ist neben einem tieferen Verständnis des Prozesses, die Bereitstellung eine breiteren Datenbasis für die Validierung numerischer Modelle.
Es sollen in diesem Beitrag die drei Versuchsanlagen und ausgewählte Messtechniken beispielhaft anhand von Messergebnissen vorgestellt werden.

Keywords: Stranggießen; Flüssigmetallmodell; Strömungsmessung; elektromagnetische Strömungsbeeinflussung; Zweiphasenströmung

  • Lecture (Conference)
    WERKSTOFFWOCHE, 14.-17.09.2015, Dresden, Deutschland

Publ.-Id: 22286

Dipole strength distribution of 74Ge

Massarczyk, R.; Schwengner, R.; Bernstein, L. A.; Anders, M.; Bemmerer, D.; Beyer, R.; Elekes, Z.; Hannaske, R.; Junghans, A. R.; Kögler, T.; Röder, M.; Schmidt, K.; Wagner, A.; Wagner, L.

The dipole strength distribution of 74Ge was studied in photon-scattering experiments using bremsstrahlung produced with electron beams of energies of 7.0 and 12.1 MeV at the linear accelerator ELBE. We identified 94 levels with spin J = 1 up to an excitation energy of 8.9 MeV and analyzed the strength in the quasi-continuum of states. Simulations of statistical gamma-ray cascades were performed to estimate intensities of inelastic transitions and to correct the intensities of the ground-state transitions for their branching ratios. The photoabsorption cross section below the neutron-separation energy derived in this way is combined with the photoabsorption cross section obtained from an earlier (gamma, n) experiment and compared with phenomenological approximations.

Keywords: Nuclear resonance fluorescence; photon scattering; bremsstrahlung; photoabsorption cross section

Publ.-Id: 22285

Nanofabrication of self-organized periodic ripples by ion beam sputtering

Iacob, E.; Dell’Anna, R.; Giubertoni, D.; Demenev, E.; Secchi, M.; Böttger, R.; Pepponi, G.

Ion beam sputtering of solid surfaces with ions of low keV energies can produce self-organized periodic ripple patterns of nanometer size on the surface of semiconductors, metals and insulators, therefore looking to be a single-step, cost-effective method to fabricate surface topographies over large areas for various electronic and bio-devices.
To date, a comprehensive theoretical understanding of the ripple development is still missing, and the achievement of the application-specific surface topography still relay on properly tuning different ion-beam parameters, since the experiments have highlighted the dependence of ripple characteristics on them.
The success of technological applications often requires an a-priori defined ratio of ripple height to wavelength. Here we discuss how to obtain regular ripples of height h~10 nm and wavelength λ<=50 nm on silicon surfaces. Xe+ and O+ ions were used to also investigate the role of the surface chemical reactivity.
The results show the development of regular ripples with wavelengths of ~40 nm and heights of ~2 nm superimposed on a less regular periodic topography for O+ bombardment on Si; the Xe+ on Si bombardment produced structures of regularity below the expected values. We discuss the gained insights and the best recipe for the required nano-patterns.

Keywords: ion bombardment; self-organization; silicon; ripples

  • Lecture (Conference)
    41st Micro and Nano Engineering, 21.-24.09.2015, The Hague, The Netherlands
  • Microelectronic Engineering 155(2016), 50-54
    DOI: 10.1016/j.mee.2016.02.025

Publ.-Id: 22284

Nanoporous Ge surface decomposition under ion bombardment: towards settling the dispute about driving forces

Böttger, R.; Liedke, B.; Liedke, M. O.; Heinig, K.-H.; Bischoff, L.

First detailed studies of the nanoporous decomposition of Ge under ion irradiation date back more than 30 years. Irradiated Ge alters its (near-)surface morphology into a nanostructure, which remains stable after irradiation even under thermal treatment up to several hundred degrees Celsius. In recent years, this peculiar transformation of Ge has been studied extensively. However, a conclusive assessment of the driving force for the nanoporous Ge decomposition has not been reached yet.

We show that hole patterns and sponge-like layers of irradiated Ge surfaces originate from the same driving force, namely the kinetics of irradiation-induced defects in amorphous Ge layers. Ge hole patterns reported earlier for irradiation with low ion energies around 5 keV were reproduced for low energy Bi+ but also for Ge+ self-irradiation, which proves that the dominating driving force for morphology evolution cannot originate from the implanted impurities. At higher ion energies up to 100 keV the well-known formation of sponge-like Ge surface layers after heavy ion irradiation was found for Bi+ irradiation and Ge+ self-irradiation, too. The transition from smooth surfaces via hole patterns to sponge-like morphologies with increasing ion energy has been studied in detail. A model based on the kinetics of ion beam-induced defects was developed and implemented in 3D kinetic Monte Carlo simulations, which reproduce the transition from hole patterns to sponge-like layers with increasing ion energy. Finally, the proposed defect kinetics driven mechanism is undergird by a systematic positron annihilation spectroscopy investigation.
The authors acknowledge financial funding by the German Research Foundation via the Research Unit 845 “Selforganized nanostructures induced by low-energy ion beam erosion.”

Keywords: porous germanium; ion irradiation; defect kinetic; kinetic Monte-Carlo

  • Lecture (Conference)
    Workshop Ionenstrahlen und Nanostrukturen, 22.-24.07.2015, Heidelberg, Deutschland
  • Lecture (Conference)
    8th International Workshop on Nanoscale Pattern Formation at Surfaces, 12.-16.07.2015, Krakow, Poland
  • Lecture (Conference)
    The 19th International Conference on Surface Modification of Materials by Ion Beams, 22.-27.11.2015, Chiang Mai, Thailand

Publ.-Id: 22283

Interactions of natural occurring eukaryotic microorganisms isolated from the uranium mine Königstein (Saxony, Germany) with U(VI)

Gerber, U.; Krawczyk-Bärsch, E.; Arnold, T.; Merroun, M. L.

Despite high uranium concentrations (up to 14 mg L-1) and low pH (2.5 - 3.0) a high microbial diversity was detected by culture independent methods in the flooding water of the former uranium mine Königstein (Saxony, Germany). In this study we used culture dependent techniques for the isolation of eukaryotic microorganisms from the flooding water. It was possible to isolate different eukaryotic fungi with a glucose riche medium. The microbial isolates identified by 16S rDNA and 18S rDNA analysis were tested for their uranium tolerance abilities by the determination of the minimal inhibitory concentration (MIC) on solid media. The results showed high tolerances of uranium (up to 6 mM) on solid agar plates. Based on these results isolate KS5 (Rhodosporidium toruloides) and one reference organism DSM 10134 (Rhodosporidium toruloides) were selected for further uranium interaction experiments. Uranium biosorption tests indicated that the cells of the strain KS5 remove high amounts of uranium (120 mg uranium/ 1 g dry biomass). Temperature dependent biosorption tests with a U(VI) concentration of 100 µM showed significant differences: KS5 revealed twice as much uranium removal at 30°C compared to at 4°C (s. Fig. 1). Since active processes, e.g., bioaccumulation do not occur at low temperature, only minor amounts of U(VI) are taking up in the cytoplasm of the cells. Hence, U(VI) is preferentially sorbed on the cell membrane by the passive process of biosorption.
In order to test the uranium tolerance quantitatively in liquid media flow cytometry experiments with the strains KS5 and DSM 10134 were performed. For this purpose live-dead staining were done to test the cell viability. The cells were stained with Propidium Iodid (PI - non viable cells) and Fluorescein Diacetate (FDA - viable cells). Furthermore the oxidative stress response was measured with the fluorescent dye 3,3'-Dihexyloxacarbocyanine Iodide (DiOC6 - cell membrane of living cells). The results showed that the isolate KS5 are able to tolerate higher U(VI) concentrations compared to the reference culture DSM 10134. More than 50 % of the KS5 cells are viable at an initial U(VI) concentration of 100 µM. In contrast less than 10 % of the reference cells are viable at the same uranium concentration. The results of the oxidative stress response showed a slight difference to the cell viability test. The isolate KS5 showed that nearly 50 % of the cells are active, like the cell viability test. Whereas the results for the reference DSM 10134 revealed that more than 30 % of the cells are active and exhibit an active membrane potential, in contrast to the results of the cell viability test. This can be explained by the stress response in the presence of heavy metals. Some cells produce mechanic-sensitive receptors which are permeable for Propidium Iodide, resulting in a wrong fluorescent staining signal. Thus, it would be an asset to combine both methods, like cell viability test and oxidative stress response tests.
Summarizing the results of this study, we were able to prove that eukaryotic microorganisms within a uranium-contaminated environment exhibit adaption mechanisms against high U(VI) concentrations. The expensive chemical treatment of the flooding water in Königstein could take a long time probably for the next 100 years. For that reason, these isolated eukaryotic microorganisms might play an important role in the bioremediation of radionuclides within the waste water treatment in Königstein.

Keywords: Uranium; Bioremediation; Biosorption; Tolerance

  • Lecture (others)
    Remediation Symposium 2015, 30.09.-01.10.2015, Jena, Deutschland

Publ.-Id: 22282

Stratified and Segregated Flow Modelling - AIAD

Höhne, T.

Today: Limits in simulating stratified & segregated two phase flow
Algebraic Interfacial Area Density Model (AIAD)
Free Surface Drag
Turbulence Damping
Sub-grid wave turbulence (SWT)
Verification and Validation is going on – more experimental data are required for the validation

Keywords: AIAD; Free Surface Drag; Sub-grid wave turbulence (SWT)

  • Contribution to proceedings
    13th Short Course “Multiphase Flow: Simulation,Experiment and Application”, 24.-26.11.2015, Dresden, Deutschland
  • Lecture (Conference)
    13th Short Course “Multiphase Flow: Simulation,Experiment and Application”, 24.-26.11.2015, Dresden, Deutschland

Publ.-Id: 22281

IAEA CRP Benchmark of ROCOM Boron Dilution and PTS test cases

Höhne, T.

The last decade has seen an increasing use of three-dimensional CFD codes to predict steady state and transient flows in nuclear reactors because a number of important phenomena such as pressurized thermal shocks, coolant mixing, and thermal striping cannot be predicted by traditional one-dimensional system codes with the required accuracy and spatial resolution.

The nuclear industry now also recognizes that CFD codes have reached the desired level of maturity (at least for single-phase applications) for them to be used as part of the NPP design process, and it is the objective of a IAEA CRP to assess the current capabilities of such codes in this regard, and contribute to the technology advance in respect to their verification and validation. CFD is already well-established in addressing certain safety issues in NPPs, as reported and discussed at various international workshops. The development, verification and validation of CFD codes in respect to NPP design necessitates further work on the complex physical modelling processes involved, and on the development of efficient numerical schemes needed to solve the basic equations. In parallel, it remains an overriding necessity to benchmark the performance of the CFD codes, and for this experimental databases need to be established, both for separate-effect tests and for full-size integral tests.

At the IAEA it was decided to set up a benchmark of ROCOM boron dilution and PTS test cases. All the test data had previously been opened, so only an ‘open’ benchmark exercise could be contemplated. Two sets of test data could be made available, relating to Pressurized Thermal Shock (PTS) and boron dilution (pump start-up). The ROCOM facility is at 1:5 scale, based on the 4-loop Konvoi reactor concept. There are 4000 measuring points by means of the Wire-Mesh Sensor (WMS) measurement technique, for which data collection is available up to a frequency of 10 kHz. It was noted that each experiment had been repeated five times to ensure authenticity of the data. In both cases, initial and boundary conditions are specified. Data have been recorded at P1 and P2 confidence levels. A CAD file of the test geometry is also available – it has recently been updated. All test data are available in tabular form, for ease of interpretation.

The Benchmark will help to analyze the CFD code capabilities for CFD in nuclear reactor design applications.

Keywords: IAEA; ROCOM; Benchmark; PTS; Boron Dilution

  • Contribution to proceedings
    25th SYMPOSIUM of AER on VVER Reactor Physics and Reactor Safety, 13.-16.10.2015, Balatongyörök, Ungarn
  • Lecture (Conference)
    25th SYMPOSIUM of AER on VVER Reactor Physics and Reactor Safety, 13.-16.10.2015, Balatongyörök, Ungarn

Publ.-Id: 22280

Distribution of Sb minerals in the Cu and Zn flotation of Rockliden massive sulphide ore in north-central Sweden

Minz, F. E.; Bolin, N.-J.; Lamberg, P.; Bachmann, K.; Gutzmer, J.; Wanhainen, C.

The Rockliden massive sulphide Zn-Cu deposit contains minor amounts of Sb minerals. The Sb mineralogy is complex in terms of composition, micro textures and mineral associations. The main Sb minerals comprise tetrahedrite, bournonite, gudmundite and Sb-Pb sulphides such as meneghinite. The presence of these minerals is especially critical to the quality of the Cu-Pb concentrate. To study how they are distributed in a simplified flotation circuit and what controls their process behaviour Sb-rich drill core samples were selected from the Rockliden deposit and a standard laboratory flotation test was run on the composite samples. Scanning electron microscope-based automated mineralogy was used to measure the Sb mineralogy of the test products, and the particle tracking technique was applied to mass balance the different liberation classes to finally trace the distribution of liberated and locked Sb minerals. The mineralogical factors controlling the distribution of Sb minerals are mineral grain size, the degree of liberation, and associated minerals. Similarities in the distribution of specific particle types from the tested composites point towards systematics in the behaviour of particles and predictability of their distribution which is suggested to be used in a geometallurgical model of the deposit.

Keywords: Sulphide ores; Antimony; Liberation analysis; Particle tracking; Froth flotation


Publ.-Id: 22279

Turbulence treatment at the interface of horizontal gas-liquid flows

Höhne, T.

Stratified two-phase flows are relevant in many industrial applications, e.g. pipelines, horizontal heat exchangers and storage tanks. The numerical simulation of free surface flows can be performed using phase-averaged multi-fluid models, like the homogeneous and the two-fluid approaches, or non-phase-averaged variants. The approach shown in this paper within the two-fluid framework is the Algebraic Interfacial Area Density (AIAD) model. It allows the macroscopic blending between different models for the calculation of the interfacial area density and improved models for momentum transfer in dependence on local morphology. A further step of improvement of modelling the turbulence was the consideration of sub-grid wave turbulence (SWT) that means waves created by Kelvin-Helmholtz instabilities that are smaller than the grid size. A first CFD validation of the approach was done for an adiabatic case of the HAWAC channel. More verification and validation of the approach is necessary – more CFD grade experimental data are required for the validation.

Keywords: CFD; horizontal annular flow; AIAD; droplet entrainment; two-phase flow

  • Contribution to proceedings
    Turbulence, Heat and Mass Transfer 8, 15.-18.09.2015, Sarajevo, Bosnien Herzogowina
  • Lecture (Conference)
    Turbulence, Heat and Mass Transfer 8, 15.-18.09.2015, Sarajevo, Bosnien Herzogowina
  • Book chapter
    K. Hanjalic, T. Miyauchi, D. Borello, M. Hadzabdic and P. Venturini: Turbulencem Heat and Mass Transfer 8, New York: Begell Haus Inc., 2015, 978-1-56700-427-4, 141-145

Publ.-Id: 22278

Numerical modeling of horizontal annular flows using a droplet entrainment model

Höhne, T.

One limitation in current simulating horizontal annular flows is the lack of treatment of droplet formation mechanisms. For self-generating annular flows in horizontal pipes, the interfacial momentum exchange and the turbulence parameters have to be modelled correctly. Furthermore the understanding of the mechanism of droplet entrainment in annular flow regimes for heat and mass transfer processes is of great importance in the chemical and nuclear industry.

A new entrainment model within the AIAD framework is proposed. It assumes that due to liquid turbulence the interface gets rough and wavy and forms droplets. The new approach is validated with HZDR annular flow experiments. Important phenomena like the pressure drop, the wave pumping effect, the droplet entrainment, the liquid film formation and the transient flow behavior could be calculated, analyzed and some of the phenomena compared with the measurement.

Keywords: CFD; horizontal annular flow; AIAD; droplet entrainment; two-phase flow

  • Contribution to proceedings
    The 16th International Topical Meeting on Nuclear Reactor Thermal Hydraulics (NURETH-16), 30.08.-04.09.2015, Chicago, USA
  • Lecture (Conference)
    The 16th International Topical Meeting on Nuclear Reactor Thermal Hydraulics (NURETH-16), 30.08.-04.09.2015, Chicago, USA

Publ.-Id: 22277

Sediment Generation in humid Mediterranean setting: Grain-size and Source-rock Control on Sediment Geochemistry and Mineralogy (Sila Massif, Calabria)

von Eynatten, H.; Tolosana-Delgado, R.; Karius, V.; Bachmann, K.; Caracciolo, L.

Grain-size control on sediment composition is investigated in modern proximal sediment from the Sila Massif, where basic to felsic intrusive rocks are exposed in a Mediterranean humidtemperate upland climate. Samples were taken from small creeks and weathering profiles from three areas reflecting different bed rock composition. Samples were separated into eleven grain size fractions from very coarse sand to clay and analyzed by (i) X-ray fluorescence for chemical composition, and (ii) X-ray diffraction and Mineral Liberation Analysis for mineralogical composition. The chemical composition vs. grain size relations were modelled by compositional linear regression. Mineralogical composition from selected samples is used to substantiate the interpretations based on geochemistry. Results reveal a high degree of chemical weathering with chemical index of alteration (CIA) up to 92. High CIA values are restricted to the fine-grained fractions, while sand-sized sediment average at low to moderate CIA values (~ 60). Although strongly weathered, the three sample suites reflecting basic to felsic plutonic bed rock can be effectively discriminated across all grain-size classes using trace elements such as V, Rb, and Sr. Linear trend modelling and mineralogical data reflect similar patterns for all sample suites implying similar processes independent of source rock composition. This includes overall decrease of quartz and K-feldspar over the entire grain-size range from coarse to fine, which is contrasted by overall increase of sheet silicates from coarse to fine. Among the latter, increase of clay minerals strongly outpaces the increase of micas in silt to clay fractions. A more complex behaviour is shown by plagioclase, which is most abundant in intermediate grain-size fractions for all sample suites. This is caused by initial hydrolysis along cleavage planes and subsequent breakage of plagioclase crystals into smaller fragments. Towards finer grain size, intense hydrolysis has destroyed almost all feldspars. In contrast to a similar study in glacial setting Si/Al ratios constantly decrease with decreasing grain size, reflecting the cumulative effects of minor mechanical forces, quartz leaching, and intense hydrolysis.

Keywords: geochemistry; mineralogy; chemical weathering; comminution; provenance; compositional linear regression

  • Sedimentary Geology (2015)

Publ.-Id: 22276

Entwicklung und Anwendung analytischer Methoden in der Kupferschiefer Aufbereitung

Rahfeld, A.; Möckel, R.; Gutzmer, J.

Kupferschiefer ist eine Ressource mit großer Bedeutung in Europa. Im Zuge neuer Entwicklungen in der Aufbereitungstechnik, einer gesteigerten Ressourcen- und Energieeffizienz und einem Interesse an alternativen Verfahren, besteht die Nachfrage nach detaillierten geochemischen und mineralogischen Informationen. Dementsprechend werden analytische Methoden benötigt die in der Lage sind Kupferschiefer nicht nur zu charakterisieren sondern auch durch Zerkleinerung, Flotation und Biolaugung hervorgerufene Änderungen nachzuweisen.
Klassische analytische Verfahren sind gänzlich ungeeignet für die Analyse von Kupferschiefer, aufgrund seiner komplexen Zusammensetzung bestehend aus einem hohen Anteil an Sulfiden und organischem Kohlenstoffverbindungen, sowie seines außergewöhnlich feinkörnigen Aufbaus der Matrix aus Tonen und Karbonaten. Nur der Einsatz moderner quantitativer Analysemethoden aus der Erz - und Gesteinsmineralogie und die Entwicklung neuer Vorgehensweisen ermöglicht eine verlässliche Untersuchung des Materials. Zum Einsatz kommen hierbei quantitative Röntgendiffraktometrie (QXRD), automatisierte Mineralidentifikation (MLA), Röntgenfluoreszenz (XRF), Atomemissionsspektrometrie (ICP-OES) und Neutronenaktivierung (INAA).

Keywords: Analytik Kupferschiefer Aufbereitung

  • Poster
    Jahrestagung Aufbereitung und Recycling 2015, 11.-12.11.2015, Freiberg, Deutschland

Publ.-Id: 22275

Pulsed high-field magnets – An efficient way of shaping laser accelerated proton beams for application

Kroll, F.; Bagnoud, V.; Blažević, A.; Brabetz, C.; Busold, S.; Deppert, O.; Jahn, D.; Karsch, L.; Kraft, S.; Masood, U.; Roth, M.; Schumacher, D.; Schramm, U.

Compact laser-driven proton accelerators are a potential alternative to complex, expensive conventional accelerators, enabeling unique beam properties, like ultra-high pulse dose. Nevertheless, they still require substantial development in reliable beam generation and transport.

We present experimental studies on capture, shape and transport of laser and conventionally accelerated protons via pulsed high-field magnets. These magnets, common research tools in the fields of solid state physics, have been adapted to meet the demands of laser acceleration experiments.Our work distinctively shows that pulsed magnet technology makes laser acceleration more suitable for application and can facilitate compact and efficient accelerators, e.g. for material research as well as medical and biological purposes.

  • Lecture (Conference)
    DPG-Frühjahrstagung, Wuppertal, 2015, 09.-13.03.2015, Wuppertal, Deutschland

Publ.-Id: 22274

A laser-driven ion beamline for generating well-defined ultra-short ion bunches at highest intensities

Kroll, F.; Busold, S.; Schumacher, D.; Brabetz, C.; Jahn, D.; Deppert, O.; Kraft, S.; Schramm, U.; Cowan, T. E.; Blažević, A.; Bagnoud, V.; Roth, M.

The LIGHT collaboration [1] has installed a laser-driven ion beamline at GSI Helmholtz Center for Heavy Ion Research. For the first time it is now possible to study the feasibility and potential of shaping laser-driven ion beams for future applications. We report on the temporal recompression of a laser-accelerated ion bunch.
In the presented experiment (c.f. Fig. 1), a dedicated arm of the high-power laser PHELIX was used to drive a TNSA proton source using gold and titanium foils. The 650 fs short, 20 J laser pulse produces the typical exponentially decaying energy spectrum with about 10^10 particles at an energy of 10±0.5 MeV and energy cut-off at 28.4 MeV. The protons are captured by a pulsed high-field solenoid, energy selected and modulated in a conventional radiofrequency cavity and transported along a drift line to the end station by means of permanent magnetic quadrupoles. However, the long drift between the laser target and the cavity introduces a temporal spread-out of the polychromatic beam.
Most recently, we accomplished a recompression of the ion bunch by a well-chosen acceleration voltage of the rf cavity achieving phase-focusing in the following 3.5 meter long drift behind the cavity. At the end station we measured a central energy of 7.8 MeV; up to 5×10^8 protons could be temporally compressed to a bunch with duration of 462±40 ps (FWHM). The bunches show a moderate energy spread between 10 % and 15 % and are available at 6 m distance to the source, thus well separated from the harsh laser-acceleration environment. Such well-defined sub-nanosecond intense ion bunches are ideal for the generation and study of warm dense matter and can probe transient phenomena with unprecedented time resolution.
Fig. 1. LIGHT beamline experiment setup: a) TNSA proton source driven by the PHELIX laser and captured by the high-field solenoid b). The transported particles are rotated in longitudinal phase space by the cavity c). The permanent magnetic quadrupole doublets d), e) and optionally f) transport the beam towards the end station g) where the beam was diagnosed.
[1] S. Busold et al., Nucl. Instr. Meth. Phys. Res. A 740, 94 (2014).

  • Lecture (Conference)
    Laser Plasma Acceleration Workshop 2015, 10.-15.05.2015, Deshaies, Guadeloupe, Frankreich

Publ.-Id: 22273

Towards highest peak intensities for ultra-short MeV-range ion bunches

Busold, S.; Schumacher, D.; Brabetz, C.; Jahn, D.; Kroll, F.; Deppert, O.; Schramm, U.; Cowan, T. E.; Blažević, A.; Bagnoud, V.; Roth, M.

A laser-driven, multi-MeV-range ion beamline has been installed at the GSI Helmholtz center for heavy ion research. The high-power laser PHELIX drives the very short (picosecond) ion acceleration on μm scale, with energies ranging up to 28.4MeV for protons in a continuous spectrum. The necessary beam shaping behind the source is accomplished by applying magnetic ion lenses like solenoids and quadrupoles and a radiofrequency cavity. Based on the unique beam properties from the laser-driven source, high-current single bunches could be produced and characterized in a recent experiment: At a central energy of 7.8MeV, up to 5×10^8 protons could be re-focused in time to a FWHM bunch length of τ=(462±40) ps via phase focusing. The bunches show a moderate energy spread between 10% and 15% (ΔE/E0 at FWHM) and are available at 6m distance to the source und thus separated from the harsh laser-matter interaction environment. These successful experiments represent the basis for developing novel laser-driven ion beamlines and accessing highest peak intensities for ultra-short MeV-range ion bunches.

Publ.-Id: 22272

Radiolabelling - A versatile tool for tracking nanoparticle release, uptake and transport

Schymura, S.; Hildebrand, H.; Fricke, T.; Holzwarth, U.; Bellido, E.; Ojea-Jiménez, I.; Cydzik, I.; Kulenkampff, J.; Kozempel, J.; Dalmiglio, M.; Bulgheroni, A.; Cotogno, G.; Simonelli, F.; Gibson, N.; Franke, K.; Lippmann-Pipke, J.

A major challenge in nanosafety research is the sensitve detection of nanoparticles at environmentally relevant concentration in the complex systems involved. It is said that many studies in the field of nanosafety research „do not offer any kind of clear statement on the safety of nanomaterials“, in part because of the unrealistically high concentrations used. The radiolabelling of nanoparticles can help overcoming this obstacle as it provides an easy way of reliably detecting nanoparticles in minute concentrations despite the complexity of the matrix.

We have developed various methods of introducing radiotracers into some of the most common nanoparticles, such as Ag, carbon, CeO2, Silica and TiO2 nanoparticles. The labelling techniques are the synthesis of the nanoparticles using radioactive starting materials, the binding of the radiotracer to the nanoparticles, the activation of the nanoparticles using proton irradiation, the recoil labelling utilizing the recoil of a nuclear reaction to introduce a radiotracer into the nanoparticles, and the in-diffusion of radiotracers into the nanoparticles at elevated temperatures. Using these methods we have produced [105/110mAg]Ag0, [124/125/131I]CNTs, [139Ce]CeO2, [48V]TiO2, [7Be]MWCNT, [7Be]SiO2, [44/45Ti]TiO2, etc.. All the particles were evaluated for radiolabel stability and alteration of the particle properties.

Using the so-labelled nanoparticles we achieved to measure the release of nanoparticles from surface coatings, the transport of nanoparticles in porous media, the interaction of nanoparticles with complex media such as sewage sludge and the uptake of nanoparticles in plants. The easy quantification of nanoparticle fractions inside the various systems allows the extraction of crucial information in order to understand and evaluate the different processes involved.

Keywords: Nanopartikel/Nanoparticle; Radiomarkierung/Radiolabelling

  • Lecture (Conference)
    10th International Conference on the Environmental Effects of Nanoparticles and Nanomaterials, 06.-10.09.2015, Wien, Österreich

Publ.-Id: 22271

Flash-Lamp-Enhanced Atomic Layer Deposition of Thin Films

Henke, T.; Knaut, M.; Hossbach, C.; Geidel, M.; Rebohle, L.; Albert, M.; Skorupa, W.; Bartha, J.

Within this work flash lamp annealing (FLA) is utilized to thermally enhance the film growth in atomic layer deposition (ALD). First, the basic principles of flash-lamp-enhanced ALD (FEALD) are presented in detail, the technology is reviewed and classified. Thereafter, results of our studies on the FEALD of aluminum-and ruthenium-based thin films are presented. These depositions were realized by periodically flashing on a substrate during the precursor exposure. It is shown that the film growth is induced by the flash heating and that the processes exhibit typical ALD characteristics. The obtained relations between flash parameters and film growth parameters are discussed with the main focus on the impact of the FLA-caused temperature profile on the film growth.
Besides, this work addresses technical challenges for the practical realization of this method and demonstrates the potential of this technology to extend the capabilities of thermal ALD.

Keywords: flash lamp annealing; atomic layer deposition; thin film

Publ.-Id: 22270

European activities on crosscutting thermal-hydraulic phenomena for innovative nuclear systems

Cheng, X.; Batta, A.; Bandini, G.; Roelofs, F.; van Tichelen, K.; Gerschenfeld, A.; Prasser, M.; Papukchiev, A.; Hampel, U.; Ma, W. M.

Thermal-hydraulics is recognized as a key scientific subject in the development of innovative reactor systems. In Europe, a consortium is established consisting of 24 institutions of universities, research centers and nuclear industries with the main objectives to identify and to perform research activities on important crosscutting thermal-hydraulic issues encountered in various innovative nuclear systems. For this purpose the large-scale integrated research project THINS (Thermal-Hydraulics of Innovative Nuclear Systems) is launched in the 7th Framework Programme FP7 of European Union. The main topics considered in the THINS project are (a) advanced reactor core thermal-hydraulics, (b) single phase mixed convection, (c) single phase turbulence, (d) multiphase flow, and (e) numerical code coupling and qualification. The main objectives of the project are:
Generation of a data base for the development and validation of new models and codes describing the selected crosscutting thermal-hydraulic phenomena.
Development of new physical models and modeling approaches for more accurate description of the crosscutting thermal-hydraulic phenomena.
Improvement of the numerical engineering tools for the design analysis of the innovative nuclear systems.
This paper describes the technical tasks and methodologies applied to achieve the objectives. Main results achieved so far are summarized.

Publ.-Id: 22269

Hyperspectral remote sensing for mineral mapping of structural related mineralizations around Mount Isa, Queensland, Australia

Jakob, S.; Salati, S.; Gloaguen, R.

Alone or combined with other remote sensing data, hyperspectral mineral mapping can be used to investigate mineralizations and deposits via alteration minerals. Their kind, abundance and spatial distribution can deliver important statements about the occurrence and formation of mineralizations and their relation to structural features. The high spectral and spatial resolution of HyMap data exceeds multispectral data distinctly and makes the recognition of even smaller geological structures possible. The spectral unmixing of single endmembers can be used for the accurate mapping of specific materials or minerals.The support of hyperspectral imaging by spectral data gathered in the field and the analysis of the composition of rock samples can help to determine endmembers and to identify absorption features.
This study demonstrates the possibilities and limitations of remote sensing, especially hyperspectral data, for mineral mapping purposes, using the example of the Mount Isa Inlier. This geological area is situated in Northern Queensland, Australia, and is known for its considerable ore deposits and consequent mining of predominantly copper, zinc, lead, silver and gold. Beside hyperspectral HyMap data, multispectral Landsat 8 and SRTM digital elevation data were analyzed. A three-week field study in 2014 supported the investigations.
After preprocessing and vegetation masking the data were analyzed using Spectral Feature Fitting (SFF) and Mixture Tuned Matched Filtering (MTMF) for alteration mineral mapping. The outcomes were combined with results from decorrelation stretch, band ratioing, topographic indices and automated lineament analysis. Additional information was provided by field spectrometer measurements and the XRF and XRD analysis of rock samples.
Throughout the study, mineral mapping using remote sensing data, especially hyperspectral data, turned out to deliver high qualitative results when it is supported by additional information. In situ investigation of the observed mineralizations for validation is important and can deliver such data, for instance by the investigation of rock samples or spectral measurements. Since mineralizations and alterations are often related to structures, their analysis and consideration can provide crucial hints.
The most significant result throughout the study was the determination of a new site of gossanous, silicified ridges south of the Mount Isa mining complex. Their occurrence was validated through fieldwork observations including rock sampling and spectral measurements. The gathered information additionally supported the accurate mapping of those ridges using HyMap data, which confirmed the connection between the north-south trending ridges and the Mount Isa mine deposits. The observed ridges coincide compositionally and spectrally with the outcrops of mineralized parts of the Urquhart Shale, which form the mined Pb-Zn-Ag deposits and are probably related to structures. In samples of the new site, amounts of Pb, Zn, Ag and other metals could be detected. Contrary to the mineralized outcrops of the Urquhart Shale deposits, those ridges occur outside of the common host rock and are not mentioned as mineralizations in any available map or publication.

  • Poster
    EGU General Assembly 2015, 14.04.2015, Wien, Österreich

Publ.-Id: 22268

Formation of Ge-0 and GeOx nanoclusters in Ge+-implanted SiO2/Sithin-film heterostructures under rapid thermal annealing

Zatsepin, A. F.; Zatsepin, D. A.; Zhidkov, I. S.; Kurmaev, E. Z.; Fitting, H. J.; Schmidt, B.; Mikhailovich, A. P.; Lawniczak-Jablonska, K.

The results of X-ray photoelectron spectra (XPS valence band and core levels) measurements for Ge+ implanted SiO2/Si heterostructures are presented. These heterostructures have a 30 nm thick Ge+ ion implanted amorphous SiO2 layer on p-type Si. The chemical-state transformation of the host-matrix composition after Ge+ ion implantation and rapid thermal annealing (RTA) are discussed. The XPS-analysis performed allows to conclude the formation of Ge-o and GeOx clusters within the samples under study. It was established, that the annealing time strongly affects the degree of oxidation states of Ge-atoms


Publ.-Id: 22267

Modelling of the electromagnetic braking effect in the continuous casting process of steel

Timmel, K.; Willers, B.; Kratzsch, C.; Schwarze, R.; Eckert, S.; Gerbeth, G.

It is known from industry and from scientific studies that the steel quality is significantly governed by the melt flow in the mold. Therefore, big efforts are made to adjust and to control the flow in the mold in a proper way by plant design or by the contactless, adjustable and flexible use of electromagnetic fields. These electromagnetic fields are already in industrial use for decades, but direct flow measurements about the actual effect are still rather scarce.
Three experimental facilities operating with low melting liquid metals were built at HZDR to investigate the continuous casting process of steel and to provide data for the validation of numerical simulations. The effect of the electromagnetic brake was one of the topics investigated in these low melting liquid metal experiments [1]. This paper will present new results from the LIMMCAST liquid metal experiments. Compared to previous results, the new experiments are operated in a continuous mode, providing a possibility to study the flow behavior in the stationary regime. Additional measurements focus on the behavior of the free liquid metal surface in the mold and the effect of the bulk flow on it. The paper also presents numerical results using Scale Adaptive Simulations (SAS).

Keywords: Continuous casting of steel; electro-magnetic flow control; liquid metal models; numerical simulation; scale adaptive simulations

  • Lecture (Conference)
    8th International Conference on Electromagnetic Processing of Materials (EPM2015), 12.-16.10.2015, Cannes, Frankreich
  • Contribution to proceedings
    8th International Conference on Electromagnetic Processing of Materials (EPM2015), 12.-16.10.2015, Cannes, Frankreich, 978-2-9553861-0-1, 373-376

Publ.-Id: 22266

Simulating Multi-Scale Physics in Solid Target Laser-Ion Acceleration

Huebl, A.; Kluge, T.; Hilz, P.; Bussmann, M.

Laser-ion acceleration from solid targets with ultra-intense laser pulses on the fs time scale is a central research topic for next generation particle accelerators. Accompanying processes are highly non-linear and require precise knowledge about the influence of both ab-initio electro-magnetic and atomic evolution of the plasma.

Consequently, modeling the acceleration process with simulations does not only require kinetic models with very high resolution (from the order of the inverse plasma frequency to the ns acceleration process) but also self-consistent models for non-equilibrium plasma and ionization processes.

We present large scale, 3D3V simulations with the fully-relativistic particle-in-cell code PIConGPU on the ORNL Titan cluster of mass-limited droplet targets related to recent experiments levitating these in Paul-traps.
In comparison with large 2D surveys the dependence of plasma instabilities and resulting ion energies under the variation of target material and laser properties is shown.

Keywords: laser particle acceleration; ion acceleration; mass limited targets; HPC; GPU; simulation; PIConGPU

  • Lecture (Conference)
    42nd EPS Conference on Plasma Physics 2015, 22.-26.06.2015, Lisbon, Portugal

Publ.-Id: 22265

Photocapacitive light sensor based on metal-YMnO3-insulator-semiconductor structures

Bogusz, A.; Choudhary, O. S.; Skorupa, I.; Bürger, D.; Lawerenz, A.; Lei, Y.; Zeng, H.; Abendroth, B.; Stäcker, H.; Schmidt, O. G.; Schmidt, H.

Technology of light sensors, due to the wide range of applications, is a dynamically developing branch of both, science and industry. This work presents a novel concept of photodetectors based on a metal-ferroelectric-insulator-semiconductor, a structure which has not been explored yet in the field of photodetectors. Functionality of the presented light sensor exploits the effect of ferroelectric polarization, charge trapping and photocapacitive phenomena. This is accomplished by an interplay between polarization alignment, subsequent charge distribution and charge trapping processes under given illumination condition and gate voltage. Change of capacitance serves as a read out parameter indicating the wavelength and intensity of illuminating light. The operational principle of the proposed photocapacitive light sensor is demonstrated in terms of capacitance-voltage and capacitance-time characteristics of an Al/YMnO3/SiNx/p-Si structure exposed to green, red, and near infrared light. Obtained results are discussed in the terms of optical properties of YMnO3 and SiNx layers contributing to the performance of photodetectors. Presented novel concept of light sensing might serve as the basis for the development of more advanced photodetectors.

Keywords: light; sensor; photodetector; YMnO₃; photocapacitance

Publ.-Id: 22264

Annual Report 2014 - Institute of Ion Beam Physics and Materials Research

Fassbender, J.; Heera, V.; Helm, M.; Zahn, P.

This past year 2014 was the year when we finally completely arrived as a “full member” in the Helmholtz Association. This is related to the successfully passed research evaluation in the framework of the Program Oriented Funding (POF), which will give us a stable and predictable funding for the next five years (2015 – 2019). This is particularly true for our large-scale user facilities, like the Ion Beam Center (IBC) and the electron accelerator ELBE with the free-electron laser. Most of our activities are assigned to the program “From Matter to Materials and Life” within the research area “Matter”, in cooperation with several other German Helmholtz Centers. Our in-house research is performed in three so-called research themes, as depicted in the schematic below. What is missing there for simplicity is a small part of our activities in the program “Nuclear Waste Management and Safety” within the research area “Energy”.

Our research and facilities were well appreciated by the evaluation committee, who made the following judgement about the Ion Beam Center:
“The Ion Beam Centre (IBC) of HZDR is an internationally leading ion-beam facility (with ion energies ranging from several eV to several tens of MeV). At both the national and international level it is one of the key players and is unique in its kind. The synergy between forefront research and user service has been leading to a very good publication output for both in-house research and user research. …
The very broad range of beam energies, the versatility of techniques and applications – both for ion beam modification of materials and for ion-beam analysis – makes the IBC unique in its kind. …
The strength of IBC is that its activities are based on a combination of forefront research and user service, which mutually interact in synergy and strengthen one another. In turn, this synergy has been leading to a very good publication output for both in-house research and user research.”
In order to make our Annual Report a bit more compact, we have decided to include only four full journal papers this year. This was also triggered by the fact that our publication activities have turned out be become more diverse, in more diverse journals than in the past, and often through longer papers, which would be too long to reprint them here. However, apart from the constantly quantitatively high publication output, we succeeded to publish in excellent journals such as Nature Physics, Nano Letters and Physical Review Letters, in fields as diverse as ion beam physics, magnetism and terahertz spectroscopy.
Two of our scientists, Dr. Artur Erbe and Dr. Alexej Pashkin obtained their Habilitation in 2014, both at University of Konstanz. For the first time, we are hosting an Emmy Noether Young Investigator Group funded by the Deutsche Forschungsgemeinschaft (DFG); the group works on the hot topic of magnonics and is headed by Dr. Helmut Schultheiß.
Finally we would like to cordially thank all partners, friends, and organizations who supported our progress in 2014. Special thanks are due to the Executive Board of the Helmholtz-Zentrum Dresden-Rossendorf, the Minister of Science and Arts of the Free State of Saxony, and the Minister of Education and Research of the Federal Government of Germany. Numerous partners from universities, industry and research institutes all around the world contributed essentially, and play a crucial role for the further development of the institute. Last but not least, the directors would like to thank again all IIM staff for their efforts and excellent contributions in 2014.

  • Open Access Logo Wissenschaftlich-Technische Berichte / Helmholtz-Zentrum Dresden-Rossendorf; HZDR-060 2015
    ISSN: 2191-8708, eISSN: 2191-8716


Publ.-Id: 22263

Destination and transport of engineered nanoparticles along the process wastewater – sludge – plant

Fricke, T.; Schymura, S.; Hildebrand, H.; Franke, K.

The presence of engineered nanomaterials in various consumer products leads to a significant load of nanoparticles (NP) also in urban and industrial wastewater. Consequently, wastewater treatment plants (WWTP) play a key role in managing these NP-loaded wastewaters considering that the purified WWTP effluent must be harmless when entering the recipient and the (aquatic) environment. Up to now, there is little information or practical guidelines available to safeguard these ambitious provisions. As another product of wastewater treatment (WWT), sewage sludge is considered to act as a sink for NPs during WWT process. Quite often, sewage sludge is used as an organic fertilizer in the agriculture and horticulture. Under these purposes, it cannot be excluded that a significant amount of engineered NPs might find their way into the treated soil and finally into plants and the way back in the human food chain.
Within the project “nanoSuppe” (sludge uptake particle plant environment) guidelines for WWTP and for the usage of sewage sludge as fertilizer will be created based on laboratory studies to support WWTP companies and authorities in terms of this difficile problem. To reach this goal a strong consortium from WWTPs, related companies and a research centre is formed. The project is focused on the usage of engineered NPs like TiO2, CeO2 multiwalled carbon nanotubes (MWCNT) and quantum dots. These NPs are representatives for nanomaterials that are used in many consumer products like sunscreens, paints and also in the industry.
The process of characterization of NP from the lab into the scale of a field is one of the important focuses. It includes the radio labelling of NP as a strong detection tool, the characterization of these NP in liquid phase and sewage sludge and the uptake of NP into plants. The use of radiolabeled NPs guarantee a highly sensitive identification, localisation and quantification of NPs even at the low environmentally concentrations. It is independent of the used matrices (sewage, sludge, soil, plant) and background levels of natural NPs, colloids or substances of the same elemental composition.
Within this presentation, latest results on translocation of NPs from different matrices like tap water, sewage and sewage sludge into the plant will be shown and discussed. Furthermore the chemical and physical interactions of these matrices might have a huge impact on the destination of the NP in the different media. So the uptake of NP into the plants is limited to their availability in the media. Different approaches with four plant species such as lamb’s lettuce, sunflowers, ryegrass and red radish are under investigation. These test plants cover a wide spectrum of agricultural and horticultural interest. Lamb’s lettuce and red radish end up directly in the human food chain. Besides that ryegrass functioned as animal food for cows, goats and other animals which can end up in the food chain as well.

  • Poster
    ICCE 2015, 15th EuCheMS International Conference on Chemistry and the Environment, 20.-24.09.2015, Leipzig, Deutschland

Publ.-Id: 22262

Measuring at relevant concentrations - Radiolabelling as a versatile tool for sensitive nanoparticle detection in complex systems

Hildebrand, H.; Schymura, S.; Holzwarth, U.; Bellido, E.; Ojea-Jimènez, I.; Dalmiglio, M.; Cotogno, G.; Gibson, N.; Franke, K.

The employment of radiotracers is a versatile tool for the detection of nano-particulate materials in complex systems such as environmental samples or organisms. With the increasing usage of nanoparticles in applications outside of research laboratories, a careful risk assessment of their release into the environment becomes mandatory. However, the monitoring of nanoparticles in such complex natural systems as geological formations, ground water or organisms is nearly impossible or at least extremely laborious in terms of sample preparation using conventional methods, especially at environmentally relevant concentrations. This obstacle can be overcome by radiolabelling, which may be of crucial value in enabling such research under laboratory conditions. Radiolabelling allows to localize, to trace and to detect nanoparticles in complex media without intensive sample pre-treatment for the measurements.

We have developed various methods of introducing radiotracers into some of the most common nanoparticles, such as Ag, carbon, CeO2, Silica and TiO2 nanoparticles. The labelling techniques are the synthesis of the nanoparticles using radioactive starting materials, the binding of the radiotracer to the nanoparticles, the activation of the nanoparticles using proton irradiation, the recoil labelling utilizing the recoil of a nuclear reaction to introduce a radiotracer into the nanoparticle, and the in-diffusion of radiotracers into the nanoparticles at elevated temperatures. Using these methods we have produced [105/110mAg]Ag0 [1], [124/125/131I]CNTs, [139Ce]CeO2, [48V]TiO2 [2], [7Be]MWCNT, [7Be]SiO2 [3], [44/45Ti]TiO2 [4], etc.. The radiolabelled nanoparticles were intensively tested concerning radiolabel stability and nanoparticle properties (size, zeta potential) were compared with the original (non-labelled) material. It could be shown, that radiolabels are suitable for application in scientific studies under the individual experimental conditions and nanoparticle properties remained largely unalterd by the radiolabelling procedure.

The developed radiolabelling methods are adaptable for a wide range of other nanoparticles. The so-labelled nanoparticles can be detected at minimal concentrations well in the ng/L range even with a background of the same element and without complicated sample preparations necessary. This means that nanoparticles can be localized also in e.g. intact geological samples or during transport studies using appropriate detector arrangement.

Using our methods one can radiolabel commercial nanoparticle samples for sensitive detection in environmentally relevant trace concentrations.

[1] H. Hildebrand and K. Franke: A new radiolabeling method for commercial Ag0 nanopowder with 110mAg for sensitive nanoparticle detection in complex media, J Nanopart Res (2012) 14:1142.
[2] K. Abbas, I. Cydzik, R. Del Torchio, M. Farina, E. Forti, N. Gibson, U. Holzwarth, F. Simonelli, W. Kreyling: Radiolabelling of TiO2 nanoparticles for radiotracer studies, J Nanopart Res (2010) 12:2435–2443.
[3] U. Holzwarth, E. Bellido, M. Dalmiglio, J. Kozempel, G. Cotogno, N. Gibson: 7Be-recoil radiolabelling of industrially manufactured silica nanoparticles, J Nanopart Res (2014) 16:2574.
[4] H. Hildebrand, S. Schymura, U. Holzwarth, N. Gibson, M. Dalmiglio, K. Franke: Strategies for radiolabeling of commercial TiO2 nanopowder as a tool for sensitive nanoparticle detection in complex matrices, J Nanopart Res (2015) 17:278.

  • Lecture (Conference)
    ICCE 2015, 15th EuCheMS International Conference on Chemistry and the Environment, 20.-24.09.2015, Leipzig, Deutschland

Publ.-Id: 22261

Building a New Assessment Tool for Potential Rare Earth Underground Mining Projects

Barakos, G.; Mischo, H.

Once an ore body has been probed and outlined and initial resource indications deserve further attention, the evaluation stage has to begin to determine the potential exploitation. This analysis is a sophisticated process, let alone when it comes to underground mining projects and especially on rare earth deposits that are governed by notable boundary conditions. However, the significant numbers of the parameters to be considered and their complexity, as well as the solvency of the outcomes, often result in questioning the suitability of common evaluation methods. This has created a necessity for a new evaluation procedure that focuses on potential rare earth underground mining projects. This paper describes the construction development of an assessment tool that considers not only the mining method selection process but identifies social, economic and environmental impact factors and Rare Earth Element industry-specific criteria as well. Based on the philosophy of previous linguistic and numerical approaches, this combined tool is based on a step-by-step numerical analytical hierarchical process with weighted criteria. The purpose of building this tool is to adjust to the specifications of rare earth underground mining projects and to contribute into having accurate and secure con-clusions for if and when investment decisions should be made and minimize the potential risks regarding the viability of any mining project.

Keywords: rare earths; underground mining method selection; viability; assessment tool

  • Open Access Logo Contribution to proceedings
    7th Sustainable Development In Minerals Industry Conference (SDIMI 2015), 12.-15.07.2015, Vancouver, Canada
    Proceedings of SDIMI 2015, Vancouver: University of British Columbia

Publ.-Id: 22260

Setting the REE industry-specific criteria and their significant role in the viability of rare earth underground mining projects

Barakos, G.; Mischo, H.

To evaluate the feasibility of a future underground mining operation is a complex problem in itself, with several different parameters to be accounted for and evaluated to secure investment decisions over the viability of any potential underground mining project. This procedure gets even more complicated when it comes to exploiting rare earth deposits. Various concerns are expressed regarding the environmental impacts that an underground mining operation may cause due to the radioactivity of the rare earth elements during mining and in waste treatment. Furthermore, the fragile market and the diversified supply and demand of the different rare earth elements can significantly affect the viability of such a venture, among other factors. This paper deals with the definition and classification of the specific criteria that govern the REE mining industry. Moreover, a thorough investigation is made of how these criteria can determine not only the selection of the underground mining method to be applied, but also of the impact that they may have to the overall feasibility of any given potential project.

Keywords: rare earth elements; underground mining; sustainability; environmental impacts; balance problem

  • Open Access Logo Contribution to proceedings
    26th Annual Meeting & Conference of the Society of Mining Professors, 21.-26.06.2015, Freiberg, Deutschland
    Proceedings of the 26th Annual Meeting & Conference of the Society of Mining Professors, Backnang, Stuttgart: WIRmachenDRUCK, 978-3-86012-505-2

Publ.-Id: 22259

Broken vertex symmetry and finite zero-point entropy in the artificial square ice ground state

Gliga, S.; Kákay, A.; Heyderman, L. J.; Hertel, R.; Heinonen, O. G.

We study degeneracy and entropy in the ground state of artificial square ice. In theoretical models, individual nanomagnets are typically treated as single spins with only two degrees of freedom, leading to a twofold degenerate ground state with intensive entropy and thus no zero-point entropy. Here, we show that the internal degrees of freedom of the nanostructures can result, through edge bending of the magnetization and breaking of local magnetic symmetry at the vertices, in a transition to a highly degenerate ground state with finite zero-point entropy, similar to that of the pyrochlore spin ices. We find that these additional degrees of freedom have observable consequences in the resonant spectrum of the lattice, and predict the occurrence of edge “melting” above a critical temperature at which the magnetic symmetry is restored.

Keywords: zero-point entropy; artificial spin-ice

Publ.-Id: 22258

Compton camera and prompt gamma ray timing: two methods for in vivo range assessment in proton therapy

Hueso-González, F.; Fiedler, F.; Golnik, C.; Kormoll, T.; Pausch, G.; Petzoldt, J.; Römer, K. E.; Enghardt, W.

Proton beams are promising means for treating tumours. Such charged particles stop at a defined depth, where the ionization density is maximum. As the dose deposit beyond this distal edge is very low, proton therapy minimises the damage to normal tissue compared to photon therapy. Nevertheless, inherent range uncertainties cast doubts on the irradiation of tumours close to organs at risk and lead to the application of conservative safety margins. This constrains significantly the potential benefits of protons over photons. In this context, several research groups are developing experimental tools for range verification based on the detection of prompt gammas, a nuclear by-product of the proton irradiation. At OncoRay and Helmholtz-Zentrum Dresden-Rossendorf, detector components have been characterised in realistic radiation environments as a step towards a clinical Compton camera. Corresponding experimental methods and results obtained during the ENTERVISION training network are reviewed. On the other hand, a novel method based on timing spectroscopy has been proposed as an alternative to collimated imaging systems. The first tests of the timing method at a clinical proton accelerator are summarised, its applicability in a clinical environment for challenging the current safety margins is assessed, and the factors limiting its precision are discussed.

Keywords: proton therapy; range verification; in vivo dosimetry; Compton imaging; block detector; scintillation; prompt gamma ray timing

Publ.-Id: 22257

Simulation studies for the in-vivo dose verification of particle therapy

Rohling, H.

An increasing number of cancer patients is treated with proton beams or other light ion beams which allow to deliver dose precisely to the tumor. However, the depth dose distribution of these particles, which enables this precision, is sensitive to deviations from the treatment plan, as e.g. anatomical changes. Thus, to assure the quality of the treatment, a non-invasive in-vivo dose verification is highly desired. This monitoring of particle therapy relies on the detection of secondary radiation which is produced by interactions between the beam particles and the nuclei of the patient’s tissue.
Up to now, the only clinically applied method for in-vivo dosimetry is Positron Emission Tomography which makes use of the beta+-activity produced during the irradiation (PT-PET). Since from a PT-PET measurement the applied dose cannot be directly deduced, the simulated distribution of beta+-emitting nuclei is used as a basis for the analysis of the measured PT-PET data. Therefore, the reliable modeling of the production rates and the spatial distribution of the beta+-emitters is required. PT-PET applied during instead of after the treatment is referred to as in-beam PET. A challenge concerning in-beam PET is the design of the PET camera, because a standard full-ring scanner is not feasible. For instance, a double-head PET camera is applicable, but low count rates and the limited solid angle coverage can compromise the image quality. For this reason, a detector system which provides a time resolution allowing the incorporation of time-of-flight information (TOF) into the iterative reconstruction algorithm is desired to improve the quality of the reconstructed images.
Secondly, Prompt Gamma Imaging (PGI), a technique based on the detection of prompt gamma-rays, is currently pursued. Concerning the emissions of prompt gamma-rays during particle irradiation, experimental data is not sufficiently available, making simulations necessary. Compton cameras are based on the detection of incoherently scattered photons and are investigated with respect to PGI. Monte Carlo simulations serve for the optimization of the camera design and the evaluation of criteria for the selection of measured events.
Thus, for in-beam PET and PGI dedicated detection systems and, moreover, profound knowledge about the corresponding radiation fields are required. Using various simulation codes, this thesis contributes to the modelling of the beta+-emitters and photons produced during particle irradiation, as well as to the evaluation and optimization of hardware for both techniques.
Concerning the modeling of the production of the relevant beta+-emitters, the abilities of the Monte Carlo simulation code PHITS and of the deterministic, one-dimensional code HIBRAC were assessed. The Monte Carlo tool GEANT4 was applied for an additional comparison. For irradiations with protons, helium, lithium, and carbon, the depth-dependent yields of the simulated beta+-emitters were compared to experimental data. In general, PHITS underestimated the yields of the considered beta+-emitters in contrast to GEANT4 which provided acceptable values. HIBRAC was substantially extended to enable the modeling of the depth-dependent yields of specific nuclides. For proton beams and carbon ion beams HIBRAC can compete with GEANT4 for this application. Since HIBRAC is fast, compact, and easy to modify, it could be a basis for the simulations of the beta+-emitters in clinical application. PHITS was also applied to the modeling of prompt gamma-rays during proton irradiation following an experimental setup. From this study, it can be concluded that PHITS could be an alternative to GEANT4 in this context.
Another aim was the optimization of Compton camera prototypes. GEANT4 simulations were carried out with the focus on detection probabilities and the rate of valid events. Based on the results, the feasibility of a Compton camera setup consisting of a CZT detector and an LSO or BGO detector was confirmed. Several recommendations concerning the design and arrangement of the Compton camera prototype were derived. Furthermore, several promising event selection strategies were evaluated. The GEANT4 simulations were validated by comparing simulated to measured energy depositions in the detector layers. This comparison also led to the reconsideration of the efficiency of the prototype. A further study evaluated if electron-positron pairs resulting from pair productions could be detected with the existing prototype in addition to Compton events. Regarding the efficiency and the achievable angular resolution, the successful application of the considered prototype as pair production camera to the monitoring of particle therapy is questionable.
Finally, the application of a PET camera consisting of Resistive Plate Chambers (RPCs) providing a good time resolution to in-beam PET was discussed. A scintillator-based PET camera based on a commercially available scanner was used as reference. This evaluation included simulations of the detector response, the image reconstructions using various procedures, and the analysis of image quality. Realistic activity distributions based on real treatment plans for carbon ion therapy were used. The low efficiency of the RPC-based PET camera led to images of poor quality. Neither visually nor with the semi-automatic tool YaPET a reliable detectability of range deviations was possible. The incorporation of TOF into the iterative reconstruction algorithm was especially advantageous for the considered RPC-based PET camera in terms of convergence and artifacts.
The application of the real-time capable back projection method Direct TOF for the RPCbased PET camera resulted in an image quality comparable to the one achieved with the iterative algorihms. In total, this study does not indicate the further investigation of RPC-based PET cameras with similar efficiency for in-beam PET application.
To sum up, simulation studies were performed aimed at the progress of in-vivo dosimetry. Regarding the modeling of the beta+-emitter production and prompt gamma-ray emissions, different simulation codes were evaluated. HIBRAC could be a basis for clinical PT-PET simulations, however, a detailed validation of the underlying cross section models is required. Several recommendations for the optimization of a Compton Camera prototype resulted from systematic variations of the setup. Nevertheless, the definite evaluation of the feasibility of a Compton camera for PGI can only be performed by further experiments. For PT-PET, the efficiency of the detector system is the crucial factor. Due to the obtained results for the considered RPC-based PET camera, the focus should be kept to scintillator-based PET cameras for this purpose.

Keywords: Monte-Carlo Simulation; Partikeltherapie; in-vivo Reichweitenkontrolle; GEANT4; PHITS; Prompt Gamma Imaging; Compton-Kamera; Positronen-Emissions-Tomographie; Paarbildungskamera; Monte Carlo simulation; particle therapy; in-vivo range verification; GEANT4; PHITS; Prompt Gamma Imaging; Compton camera; positron emission tomography

  • Open Access Logo Wissenschaftlich-Technische Berichte / Helmholtz-Zentrum Dresden-Rossendorf; HZDR-062 2015
    ISSN: 2191-8708, eISSN: 2191-8716


Publ.-Id: 22256

Surface modification with focused polyatomic ion beams

Bischoff, L.; Böttger, R.; Pilz, W.; Heinig, K.-H.

In the last decades Focused Ion Beams (FIB) have evolved from a sophisticated idea to a distinguished standard technique for sample preparation for SEM and TEM, prototyping in research and development and analytics in fields like microelectronics or nanotechnology. Most of FIB systems work with Ga beams, but liquid metal ion sources (LMIS) provide a much broader spectrum of other ion species using different source materials and an ion optical column equipped with an ExB mass separator [1]. From the source tip, beside single and double charged monatomic ions also dimers, trimers and heavier projectiles are extracted, which play an increasing role due to their special properties, like shallow penetration depth, enhanced sputtering efficiency and the huge energy deposition due to the simultaneous impact of several atoms in the same point of the sample surface.
Beside others heavy elements or alloys, those containing Au but in particular Bi are very suitable for the emission of polyatomic ions. Such projectiles with masses up to about 1000 amu have an energy spread in the range of EFWHM = 30 … 150 eV, which restrict the final FIB resolution (spot size) due to chromatic aberration to 10 … 100 nm. This is a result of the complex appearance of polyatomic species in the area around the emission point.
One of the main application fields at present is SIMS, which increasingly works with polyatomic Bi beams for defined surface erosion of inorganic as well as organic specimens. Another exciting field of application is the surface modification in terms of surface patterning by heavy dimer and trimer ions (e.g. Aunm+, Binm+). Due to the enormous, surface-near energy density deposition of cluster ions a self-organization process of hexagonally ordered dot arrays on Ge and Si based on transient melt pool formation can be triggered (Fig. 1) [2].
The authors would like to thank S. Facsko and B. Schmidt from HZDR for fruitful contributions to this work.

[1] L. Bischoff, Nucl. Instr. Meth. B 2008, 266, 1846.
[2] R. Böttger, L. Bischoff, K.-H. Heinig, W. Pilz, B. Schmidt, J. Vac. Sci. Technol. B 2012, 30, 06FF12.

Keywords: Surface modification; ion; cluster; FIB; sputtering

  • Lecture (Conference)
    Workshop Ionenstrahlen und Nanostrukturen, 22.-24.07.2015, Heidelberg, Germany

Publ.-Id: 22255

Polyatomic Focused Ion Beams – Origin and Applications

Bischoff, L.

In the last four decades Focused Ion Beams (FIB) have evolved from a sophisticated idea to a distinguished standard technique for sample preparation for SEM and TEM, prototyping in research and development and analytics in fields like microelectronics or nanotechnology. Most of the FIB systems works with Ga beams, but liquid metal ion sources (LMIS) provide a much broader spectrum of other ion species using different source materials and an ion optical column equipped with an ExB mass separator [1]. From the source tip beside single and double charged monatomic ions also dimers, trimers and heavier projectiles are extracted, which play an increasing role due to their special properties, like slight penetration depth, enhanced sputtering efficiency and the huge energy deposition due to the simultaneous impact of several atoms in the same point of the surface.
Beside others heavy elements or alloys, those containing Au but in particular Bi are very appropriate for the emission of polyatomic ions. Such projectiles with masses up to about 1000 amu have an energy spread in the range of ΔEFWHM = 30 … 150 eV, which restrict the final FIB resolution (spot size) due to chromatic aberration to 10 to 100 nm. This is a result of the complex appearance of polyatomic species in the area around the emission point.
One of the main application fields at present is SIMS, which increasingly works with polyatomic Bi beams for defined surface erosion on inorganic as well as organic specimen [2]. A second exciting field of application is the surface modification in terms of surface patterning by heavy dimer and trimer ions (e.g. Aunm+, Binm+). Due to the enormous energy transfer by the cluster ions to the surface a self-organization process of hexagonal ordered dot arrays on Ge and Si could be found surprisingly for pure elemental targets at normal incidence, described by the formation of tiny melt pools [3] shown in the figure.

[1] L. Bischoff, Nucl. Instr. Meth. B 266 (2008) 1846.
[2] F. Kollmer, Appl. Surf. Sci. 231-232 (2004) 153.
[3] R. Böttger, L. Bischoff, K.-H. Heinig, W. Pilz and B. Schmidt, JVST B 30 (2012) 06FF12.

Keywords: FIB; Cluster ions; LMIS; self-assembly

  • Lecture (Conference)
    10. Dreiländer-FIB-Workshop, 29.-30.06.2015, Halle, Germany

Publ.-Id: 22254

Uptake of Selenium Oxyanions by δ-alumina at elevated Temperatures

Franzen, C.; Jordan, N.

One major process controlling the mobility and bioavailability of selenium, a long-lived fission product in nuclear waste, is the adsorption onto mineral surfaces of both the engineered and geological barrier. In this context, it is important to understand to what extent this sorption is influenced particularly by characteristic parameters as expected in deep underground repositories for high level and long-lived radioactive waste. These parameters include inter alia elevated temperatures originating from heat generating waste and natural ground heat. For the investigation of the sorption processes, δ−Al2O3 was chosen because it is omnipresent in the environment and it represents a model oxide for more complex aluminosilicates.
In the present study, a combination of macroscopic sorption experiments, electrophoretic mobility and in-situ ATR FT-IR spectroscopy measurements was used to study the interaction of selenate and selenite with aged δ-Al2O3 at different temperatures between 25°C and 60°C. From in-situ ATR FT-IR spectra, a change in the symmetry of the aqueous tetrahedral selenate anion can be derived evidencing the formation of a surface complex on δ-Al2O3. From batch experiments, we observe a decreasing sorption of both selenate and selenite upon increasing temperature.
The isoelectric point (pHIEP) of δ-Al2O3 was located at pH 9.6 at 25°C. At higher temperatures, the pHIEP was shifted towards lower pH with a value of 8.6 at 60 °C. In addition, the absolute values of the zeta potential were lowered at higher temperatures. Both findings were in good agreement with the batch experiments.
The observed decrease in selenate and selenite sorption at higher temperatures could be assigned to a change in the surface properties of δ−Al2O3.
This effect may significantly increase the mobility of these Se−species and must be taken into account in future safety assessments of nuclear waste repositories.

Keywords: selenate; selenite; sorption

  • Poster
    GDCh-Wissenschaftsforum Chemie 2015, 30.08.-02.09.2015, Dresden, Deutschland

Publ.-Id: 22253

Spin-transfer effects in MgO-based tunnel junctions with an out-of-plane free layer and in-plane polarizer

Kowalska, E.; Sluka, V.; Fowley, C.; Kakay, A.; Aleksandrov, Y.; Lindner, J.; Fassbender, J.; Deac, A. M.

Spin-torque nano-oscillators (STNOs) are novel devices which may be exploited for wireless communication applications [1-3]. In particular, it has recently been demonstrated that STNOs utilizing an in-plane (IP) magnetized polarizer (also acting as read-out layer) and out-of-plane (OOP) magnetized free layer allow for the full parallel (P)-to-antiparallel (AP) resistance variation to be exploited in the limit of 90° precession angle, thereby maximizing the output power [1]. However, for this specific geometry, steady-state precession can only be sustained if the spin-transfer torque exhibits an asymmetric dependence on the angle between the free and the polarizing layer, such as in the case of fully metallic devices [1]. Nevertheless, it has recently been reported that dynamics have been experimentally observed in similarly designed MgO-based MTJs under constant applied electrical current, in spite of the fact that such devices do not exhibit any asymmetry in the spin-torque angular dependence [4,5]. These results have so far been interpreted based on the formalism for metallic devices, including the spin-torque angular dependence.
Here, we explore potential mechanisms for sustaining steady-state precession in MgO-based MTJs with an IP polarizer and an OOP free layer. To this end, we analytically and numerically solve the Landau-Lifshitz-Gilbert-Slonczewski equation for a nano-pillar MTJ with circular cross-section, under a constant perpendicular applied current and field. To sustain steady-state precession, the energy supplied by the in-plane spin-torque term and energy dissipated through damping must compensate over a full precession period.
In an MgO-MTJ, the magnitude of the STT is determined by the voltage across the barrier [6]. As the magnetization of the free layer precesses around the put-of-plane direction, the angle between the magnetic moments of the two layers changes and through the magnetoresistance effect the voltage changes if the experiment is conducted at constant applied current [7,8]. This cosine-like angular dependence of the MTJ resistance effectively introduces a spin-torque angle dependence asymmetry. In addition, for a given angle, the resistance exhibits a specific bias dependence, with the resistance of the AP state decreasing approximately linearly with increasing bias, while remaining mostly constant in the P configuration. In this work, we demonstrate that the spin-torque angular asymmetry exhibited in such systems is sufficient to sustain STT-driven dynamics.
Fig. 1 shows dynamic and static phase diagrams of the STNO obtained when neglecting (Fig. 1(a) and 1(c)) and taking into account (Fig. 1(b) and 1(d)) the bias dependence of the AP state resistance. In both cases, stable dynamics occur only for positive currents (colored area), defined as electrons flowing from the free to the reference layer. In MTJs exhibiting no bias dependence of the resistance (dRAP/dV = 0 Ω/V), the onset current for steady-state dynamics (solid lines) scales linearly with the applied current. High output powers can be obtained for relatively low values of applied currents and fields for realistic MTJ parameters, which is beneficial from the point of view of applications. Introducing an experimentally realistic value of dRAP/dV affects mostly the steady-state dynamics, while most of the trends observed for static states are maintained (Fig. 1(b) and 1(d)). Indeed, in this case current-driven precession is only excited for fields lower than the effective anisotropy of the free layer (but still only for positive currents). Moreover, while the symmetry versus field sign is conserved, the onset current no longer increases linearly with the field, but rather exhibits a parabolic-like dependence.

Keywords: spin-torque nano-oscillators (STNOs); magnetic tunnel junctions (MTJs)

  • Poster
    International Colloquium on Magnetic Films and Surfaces (ICMFS 2015), 12.-17.07.2015, Cracow, Poland

Publ.-Id: 22252

Tomographic investigations on centrifugal pumps conveying gas-liquid two phase flow

Schäfer, T.; Neumann, M.; Bieberle, A.; Hampel, U.

This contribution presents an investigation study of two-phase flow distribution in an industrial centrifugal pump and its effect to the hydrodynamic behaviour. Therefore, high-resolution gamma-ray computed tomography has been applied especially in the impeller region of an industrial centrifugal pump. To observe gas-liquid phase distributions within a sharply mapped impeller wheel, which rotates with up to 1900 rpm, time-averaged rotation-synchronized computed tomography as well as radiography has been applied. The accumulation of the gas phase was studied for varying injected gas volume fractions and flow regimes. Furthermore, various internally accumulated gas holdup patterns could be identified and, eventually, associated with characteristic pump performance behaviours. Moreover, the measuring method allowed gas holdup analysis in each chamber of the impeller wheel along selected streamlines. As a result, specific phase holdup profiles could be evaluated.

Keywords: gamma-ray computed tomography; centrifugal pump; two-phase flow; gas entrainment

  • Lecture (Conference)
    7th International Symposium on Process Tomography (ISPT7), 01.-03.09.2015, Dresden, Deutschland
  • Contribution to proceedings
    7th International Symposium on Process Tomography (ISPT7), 01.-03.09.2015, Dresden, Deutschland
    Proceedings of the 7th International Symposium on Process Tomography

Publ.-Id: 22251

Ion microprobe PIXE and PIGE analysis of standards’ trace elements for electron microprobe calibration.

Le Bras, L.; Munnik, F.; Renno, A. D.

The purpose of this study is, with the recorded data, to be able to calibrate microanalytical methods, in particular electron microprobe with high precision chemical data standards. Analysis on selected standards by ion microprobe Particle-Induced-X-ray-Emission (PIXE) and Particle-Induced-Gamma-ray-Emission (PIGE) are used to detect and quantify the trace and light elements present in these samples. The presence of those elements makes a specific calibration of the machines necessary.
Electron- and X-ray measurements need good standards for a good quantification of the elements of interest. Actually, certified reference materials for microanalytical methods are very rare. In addition they are mainly glass samples. Utilisation of chosen minerals fixed in a matrix instead of glasses for calibration makes possible the application of the matrix-matched principle and the detection and quantification of trace elements in natural minerals for a resource technology application.
The widespread utilisation of Smithsonian Microbeam Standards makes this study relevant. That is why a 10 sample selection has been made in this collection. The samples’ theoretical compositions in major and trace elements are very important for the achievement of the analysis. In addition to the given element concentrations [1], a bibliographic study has also been performed for each standard in order to find possible trace elements which could be detected.
The standards received from the Smithsonian Institute are composed of crushed particles (500 µm diameter). The sample preparation is also essential. It consists in the fixation of three particles with epoxy resin into a 3 mm diameter messing cylinder.
The analyses are performed with an incident proton beam of 3.5 MeV in order to acquire simultaneously X- and Gamma-ray spectra. The data analysis is performed with GeoPIXE in order to add qualitative and quantitative data about trace elements to the given composition of the major elements. Preliminary results on apatite (NMNH 104021) are in agreement with the literature and show the presence of vanadium, arsenic, strontium, yttrium and light Rare Earth Elements such as lanthanum, cerium and neodymium. These trace elements are important for mineral resources analysis. Elemental mapping is also achieved in order to check the homogeneity of the samples’ particles.

Acknowledgements: Special thanks to Andreas Bartzsch, from the sample’s preparation laboratory of the Helmholtz Institute Freiberg, Germany, for his expertise.

[1] E. Jarosewich, J. A. Nelen, J. A. Norberg, Geostandards Newsletter 4 1980, p. 43-47

Keywords: Mineral standards; PIXE; PIGE; calibration; electron microprobe

  • Lecture (Conference)
    Workshop für Ionenstrahlen und Nanostrukturen, 22.-24.07.2015, Heidelberg, Germany

Publ.-Id: 22249

A comprehensive study on iodine uptake by selected LDH phases via coprecipitation, anionic exchange and reconstruction

Iglesias, L.; Walther, C.; Medina, F.; Holzer, A.; Neumann, A.; Lozano-Rodriguez, M. J.; Alvarez, M. G.; Torapava, N.

We explored the use of selected layered double hydroxides (LDHs) of different compositions and obtained by means of different routes (i.e., coprecipitation, anionic exchange and reconstruction) as iodine/iodate adsorbents. The influence of speciation (iodide vs. iodate) on iodine uptake was rather strong, resulting in much lower iodide incorporation. The Fourier transform of iodine K X-ray absorption edge data (EXAFS) of all iodate-LDHs showed a single I–O scattering path of 1.8 A ° . Thermal stability and leaching experiments showed that the incorporated iodate and iodide were rather loosely bound in the interlayer space and were easily released under heating to 180 C and leaching with Milli-Q water and brine solution.

Keywords: Iodine; Layered double hydroxide; Immobilization; Nuclear waste; Aqueous systems

Publ.-Id: 22248

Coffinite, USiO4, Is Abundant in Nature: So Why Is It So Difficult To Synthesize?

Mesbah, A.; Szenknect, S.; Clavier, N.; Lozano-Rodriguez, J.; Poinssot, C.; Den Auwer, C.; Ewing, R. C.; Dacheux, N.

Coffinite, USIO4, is the second most abundant U4+ mineral on Earth, and its formation by the alteration of the UO2 in spent nuclear fuel in a geologic repository may control the release of radionuclides to the environment. Despite its abundance in nature, the synthesis and characterization of coffinite have eluded researchers for decades. On the basis of the recent synthesis of USiO4, we can now define the experimental conditions under which coffinite is most efficiently formed. Optimal formation conditions are defined for four parameters: pH, T, heating time and U/Si molar ratio. The adjustment pf pH between 10 and 12 leads probably to the formation of a uranium (IV) hydroxo-silicate complex that acts as a precursor of uranium (IV) silicate colloids and then of coffinite. Moreover, in this pH range, the largest yield of coffinite formation (as compared with those of the two competing byproduct phases, nanometer-scale UO2 and amorphous SiO2) is obtained for 250 C, 7 days and 100% excess silica.

Keywords: coffinite; PXRD; EXAFS; XANES; Raman spectra

Publ.-Id: 22247

High Conversion Th–U233 fuel for current generation of PWRs: Part III – Fuel availability and utilization considerations

Baldova, D.; Fridman, E.; Shwageraus, E.

In the previous studies, reported in Parts I and II of the paper, the high conversion (HC) Th-U233 fuel design for current generation of PWRs was proposed and investigated in details on single fuel assembly and 3D full core levels. One of the important limitations of the previous studies was the reliance on the availability of pure U233 as a fissile driver. In reality, however, U233 will always be accompanied by other U isotopes. Part III of the paper deals with a number of fuel cycle aspects associated with the use of HC Th-U fuel in PWRs including: (1) more realistic estimation of neutronic properties and conversion performance of HC Th-U fuel by accounting for the evolution of U isotopic composition with a number of recycle stages; (2) reassessment of the HC Th-U PWR core performance through 3D full core coupled neutronic and T-H analysis; (3) demonstration of a feasible way of generating U233; and finally (4) evaluation of potential savings in available resources that can be achieved by using HC Th-U fuel cycle as compared to the current fuel cycle practices.

Keywords: High conversion; PWR; Th-U233 fuel; seed-blanket; DYN3D

Publ.-Id: 22246

Liquid Metal Alloy Ion Sources - an Alternative for Focused Ion Beam Technology

Bischoff, L.; Mazarov, P.; Bruchhaus, L.; Gierak, J.

Today Focused Ion Beam (FIB) processing is nearly exclusively based on gallium Liquid Metal Ion Sources (LMIS). But, many applications in the µm- or nm range could benefit from ion species other than gallium: local ion implantation, ion beam mixing, ion beam synthesis or Focused Ion Beam Lithography (IBL). Therefore Liquid Metal Alloy Ion Sources (LMAIS) represent a promising alternative to expand remarkable the application fields for FIB. Especially the IBL process shows potential advantages over e.g. electron beam (EBL) or other lithography techniques: direct, resistless, and three-dimensional patterning, enabling a simultaneous in-situ process control by cross sectioning and inspection. Taking additionally into account that the used ion species influence significantly the physical and chemical nature of the resulting nanostructures -in particular the electrical, optical, magnetic and mechanic properties- leading to a large potential application area which can be tuned by choosing a well suited LMAIS. Nearly half of the elements of the Periodic Table are recently available in FIB technology as a result of continuous research in this area during the last forty years. Key features of a LMAIS are long life-time, high brightness and stable ion current. Recent developments could make these sources feasible for nano patterning issues as an alternative technology more in research than in industry. The authors will review existing LMAIS, working with pure elements (LMIS) other than Ga or binary or ternary alloys, their physical properties as well as the fabrication technology and prospective domains for modern FIB applications. Other emerging ion sources will be also presented and their performances discussed.

Keywords: Liquid Metal Alloy Ion Sources; Focused Ion Beam; Mass Separation

Publ.-Id: 22245

Relationship Between Kolmogorov Entropy and Characteristic Mixing Length in Narrow Bubble Columns Operated in the Transition Flow Regime

Nedeltchev, S.; Schubert, M.; Donath, T.; Rabha, S.; Hampel, U.

The mixing performance of bubble column reactors depends strongly on the prevailing flow regime. Kawase and Tokunaga (Can. J. Chem. Eng. 69, 1228-1231, 1991) introduced the characteristic mixing length L as an important mixing parameter. In the homogeneous regime the liquid mixing is at the scale of the bubble diameter, whereas in the heterogeneous regime it is at the scale of the column diameter. Our research is aimed at determining the scale of liquid mixing in the transition flow regime by using some advanced methods.
The Kolmogorov entropies (KE) were extracted from gas holdup time series measured (at 2000 Hz) by a new type of wire mesh sensor. It was found that in a relatively narrow bubble column (0.15 m in ID, clear liquid height = 2 m) operated with an air-water system in the transition flow regime the KE values could be correlated to L. The KE in the transition flow regime decreases monotonously and can be correlated to the superficial gas velocity (KE=1.5Ug^-0.38). The same exponent (-0.38) for UG was reported by Kawase and Tokunaga (1991) in their correlation for prediction of L. Therefore, the KE and L values (in a narrow bubble column) are correlated as follows: KE=222.222L.
A new parameter called maximum number of visits per region Nv-max was also introduced and in the same way was related to L in the transition flow regime.

Keywords: Narrow bubble column; Transition flow regime; Kolmogorov entropy; Mixing length; New statistical parameter

  • Lecture (Conference)
    Jahrestreffen der Fachgruppen Mehrphasenströmungen und Wärme- und Stoffübertragung, 24.-26.03.2014, Fulda, Deutschland

Publ.-Id: 22244

18F-FDG PET/MRI for therapy response assessment in sarcoma: Comparison of PET and MR imaging results

Schuler, M. K.; Platzek, I.; Beuthien-Baumann, B.; Fenchel, M.; Ehninger, G. E.; van den Hoff, J.

Background: 18F-Fluorodeoxyglucose (FDG) positron emission tomography (PET) has proven to be of substantial benefit in imaging of sarcoma patients. We therefore investigated the feasibility and benefit of combined PET/magnetic resonance imaging (MRI). Methods: Twelve patients with sarcoma who underwent FDG PET/MRI for staging and response assessment after chemotherapy were included. Results: Based on contrast-enhanced MRI and application of Choi criteria, therapy response was classified as stable disease in 6/12 patients (50%) and as partial remission in 6/12 patients (50%). Conclusion: In sarcoma patients, response assessment using Choi criteria based on contrast-enhanced MRI in comparison to FDG PET imaging only demonstrates slight correlation.

Keywords: Cancer imaging; Choi criteria; FDG PET/MRI; Sarcoma

Publ.-Id: 22243

2-[18F]Fluoroethyl tosylate - a versatile tool for building 18F-based radiotracers for positron emission tomography

Knieß, T.; Laube, M.; Brust, P.; Steinbach, J.

Positron emission tomography (PET) is a modern in vivo imaging technique and an important diagnostic modality for clinical and pre-clinical research. The incorporation of a radionuclide like fluorine-18 into a target molecule to form PET radiopharmaceuticals is a repeated challenge for radiochemists. 18F-Fluoroethylation is a well acknowledged method for 18F-radiolabeling and 2-[ 18F]fluoroethyltosylate ([ 18 F]FEts) is a preferred reagent because of its high reactivity to phenolic, thiophenolic, carboxylic and amide functions. The review will highlight the role of [ 18F]FEts in PET-chemistry, and summarize its applicability in radiotracer design. The radiolabeling conditions and pros and cons of direct and indirect radiolabeling as well the aspects of reactivity of [ 18F]FEts compared with other [ 18F]fluoroalkylating reagents will be discussed comprehensively.

Publ.-Id: 22242

New Methods for Flow Regime Identification in Bubble Columns and Fluidized Beds

Nedeltchev, S.

New methods for flow regime identification were developed and applied to photon count time series measured in a bubble column (0.162 m in ID) and fluidized bed (0.438 m in ID). The signals in the bubble column (operated with an air-therminol system) were measured by means of Computed Tomography (CT), whereas the data in the fluidized bed (operated with an air-polyethylene system) were recorded by means of Nuclear Gauge Densitometry (NGD). The hidden information in the time series was extracted by means of two new parameters: entropy (bit/s) and information entropy (bit). Both of them were calculated on the basis of multiple reconstructions of the time series. In the case of the bubble column, the well-pronounced local minima were used for identification of three transition velocities (0.04, 0.08 and 0.13 m/s). They distinguished the boundaries of the bubbly flow, transition and churn-turbulent flow regimes. In the case of the fluidized bed, the minimum fluidization velocity (0.086 m/s) and minimum bubbling velocity (0.12 m/s) were also identified on the basis of the well-pronounced local minima in the profiles of the new parameters. They distinguished the boundaries of both the transition and bubbling fluidization regimes.

Keywords: Flow regime identification; Bubble column; Fluidized bed; Transition velocities; Entropy; Information entropy

Publ.-Id: 22241

Terahertz emission based on large-area photoconductive emitters illuminated via beam interference

Krauß, N.; Haas, M.; Niemeyer, L.; Winnerl, S.; Helm, M.; Dekorsy, T.

The use of beam interference in combination with large-area photoconductive emitters for the generation of pulsed terahertz radiation is presented. An interference pattern with a periode twice that of the terahertz emitter is generated with a transmission phase grating, placed directly in front of the photoconductive emitter. This way, efficient terahertz generation is achieved with a single metallization layer and a single lithography step in the fabrication technology of the THz emitter.

Keywords: THz photoconductive emitter; large-area THz emitter

Publ.-Id: 22240

Characterization of microbiological community in natural REE-containing matrixes

Kutschke, S.; Raff, J.; Pollmann, K.

Biochemistry of REE is very poorly understood. As microbes drive biogeochemistry in many ecosystems it can be expected with various yet unknown organisms that play a role in REE biogeochemistry. Thus these environments are a promising source for the recovery of microbes that are suitable candidates for their application in REE extraction and recycling.
The microbial community is a close metabolic network, where some of the organisms actively contribute to the carbon, nitrogen, sulfur, and phosphorus cycle and other microorganisms interact with minerals, metals, and pollutants. On the one hand such a microbial community is well adapted to environment and on other hand it is influenced by the geochemical parameters. Investigation of microbial community of REE containing matrixes has to be accompanied by (geo)-chemical analyses. Geochemical and structural soil parameters like organic compounds, ion exchange or waterholding capacity and porosity influence the microbial population. Moreover daily or seasonal changes of physical matrix properties force the microbial community to adapt. Reflection of environmental circumstances is one challenge describing natural microbial community (Xu 2006). The most sensitive describing tools are culture independent genomic methods. These genomic methods describe and characterize the majority of microorganisms including even the uncultivated microorganisms. Generated metagenomic data will be matched with already existing genomic databases. Up to now genetic methods like PCR fingerprinting techniques and fluorescence in situ hybridization used to identify and quantify microorganisms interacted with REE containing ore. Nevertheless genomic information of energetic metabolism, phosphate, sulfur and iron metabolism, quorum sensing, and genes involved in metal resistance and amino acid biosynthesis pathways were identified (Jerez 2008). As already mentioned the data base for comparative genomic is small. To extent this fundament it is necessary to extract single strains, to cultivate them and to analyze their genomes.
Jerez, C. A. (2008). "The use of genomics, proteomics and other OMICS technologies for the global understanding of biomining microorganisms." Hydrometallurgy 94(1–4): 162-169.
Xu, J. (2006). "Microbial ecology in the age of genomics and metagenomics: Concepts, tools, and recent advances." Molecular Ecology 15(7): 1713-1731.

  • Poster
    World Congress and Expo on Applied Microbiology 2015, 18.-20.08.2015, Frankfurt, Deutschland

Publ.-Id: 22239

Efficient Auger scattering in Landau-quantized graphene

Wendler, F. H. F.; Mittendorff, M.; Winnerl, S.; Helm, M.; Knorr, A.; Malic, E.

We present an analytical expression for the differential transmission of a delta-shaped light field in Landauquantized graphene. This enables a direct comparison of experimental spectra to theoretical calculations reflecting the carrier dynamics including all relevant scattering channels. In particular, the relation is used to provide evidence for strong Auger scattering in Landau-quantized graphene.

Keywords: Graphene; ultrafast spectroscopy; Landau quantization; Auger scattering

  • Lecture (Conference)
    Photonics West Conference, 07.-12.02.2015, San Francisco, USA
  • Contribution to proceedings
    Photonics West Conference, 07.-12.02.2015, San Francisco, USA
    Proceedings of SPIE, 936105
    DOI: 10.1117/12.2075458

Publ.-Id: 22238

Theoretical Prediction of Mass Transfer Coefficients in Two-Phase and Slurry Bubble Columns

Nedeltchev, S.

Two-phase and slurry bubble columns are characterized with high volumetric mass transfer coefficients kLa at low energy input. The design, modelling, optimization and scale-up of these reactors require precise knowledge of the mass transfer parameters. The mass transfer coefficients determine the efficiency and dimensions of (slurry) bubble columns. Nedeltchev et al. (2007) developed a correlation for prediction of mass transfer coefficients in gas-liquid bubble columns operated in the homogeneous flow regime. It was based on experimental gas holdups. On the other hand, Nedeltchev and Schumpe (2008) developed a correlation for prediction of gas holdups in gas-liquid bubble columns operated in the homogeneous regime. In this work, the theoretically calculated gas holdups were substituted in the mass transfer model (in the correlation for the interfacial area) of Nedeltchev et al. (2007) and the mass transfer coefficients were recalculated by means of a purely theoretical approach. The same gases and liquids (18 pure organic liquids, 14 adjusted liquid mixtures and tap water) were used and 263 kLa values (only in the homogeneous regime) were successfully predicted at ambient and high pressures (up to 1 MPa).
The same approach was tested in a slurry bubble column. Nedeltchev et al. (2014) predicted successfully the experimental mass transfer coefficients in a slurry bubble column based on bubble sizes which depended on the experimental gas holdups. On the other hand, Nedeltchev (2014) established a new approach for predicting the gas holdups in a slurry bubble column. When these theoretical gas holdups were substituted in the mass transfer model (in the correlations for prediction of bubble size and interfacial area), a purely theoretical kLa values in a slurry bubble column were obtained. The predictions were good not only in the homogeneous regime but also in the heterogeneous regime. The theoretical approach was applicable up to relatively high (18 %) solids concentrations. Six different liquid-solid systems were used and 66 kLa values were successfully predicted. In both mass transfer models, correction factors (a function of Eӧtvӧs numbers) were introduced due to the non-spherical (ellipsoidal) shape of the bubbles.

Keywords: Mass transfer coefficients; Penetration theory; New contact time; Gas-liquid bubble columns; Slurry bubble columns

  • Lecture (Conference)
    12th International Conference on Gas-Liquid and Gas-Liquid-Solid Reactor Engineering (GLS12), 28.06.-01.07.2015, New York, USA

Publ.-Id: 22237

Hydrothermal Alteration of Trachyte Satellite Intrusions in the Cripple Creek District

Rahfeld, A.; Kelly, N.; Monecke, T.

The Cripple Creek deposit located in southwestern Colorado represents one of the largest epithermal gold deposits hosted by alkaline volcanic rocks. A petrographic study of the mostly barren satellite intrusions surrounding the deposit was undertaken to investigate and identify regional alteration patterns. Transmitted light, optical cathodoluminescence, and scanning electron microscopy, integrated with whole-rock geochemical data, revealed a complex history of fluid-rock interaction.
Early albitization of trachyte is preserved within weakly potassic-altered rocks. In more intensely altered rocks, potassium feldspar pervasively replaced the sanidine-dominated groundmass. Late alteration of the trachyte involved the formation of white mica and later kaolinite. The mineralogical changes imply a change in the physiochemical conditions of alteration from early sodic to later potassic alteration, followed by alteration caused at progressively decreasing temperatures and increasing acidity.
Tephrite intrusions within the trachyte satellite bodies have not been influenced by these styles of alteration. The tephrite has been altered to Fe-hydroxide minerals and biotite, most likely caused by influx of Fe-rich fluids. Within the mineralized trachyte of the main diatreme, Au-Te mineralization is at least locally associated with this style of Fe-rich alteration.

Keywords: Alkaline rocks; epithermal deposits; Cripple Creek; hydrothermal Alteration

  • Poster
    13th SGA Biennial Meeting (SGA2015), 24.-27.08.2015, Nancy, Frankreich
  • Contribution to proceedings
    13th SGA Biennial Meeting (SGA2015), 24.-27.08.2015, Nancy, Frankreich
    Mineral resources in a sustainable world. 13th SGA Biennial Meeting (SGA2015)

Publ.-Id: 22236

Geochemical and Mineralogical Analysis of Kupferschiefer

Rahfeld, A.; Möckel, R.; Gutzmer, J.

Kupferschiefer, i.e. very fine-grained and disseminated polymetallic Cu-Ag ores of the extensive stratabound deposits of the Central European Copperbelt is well known for its mineralogical complexity and the challenges surrounding its characterization. It is marked by a combination of high metal sulfide contents (up to 25 wt%) and organic matter (up to 30 wt%) within a matrix predominantly composed of fine-grained clay and carbonate minerals. Conventional analytical procedures often yield unreliable results of this very complex raw material. Regardless, recent research into the hydrometallurgical and microbiological beneficiation of Kupferschiefer has raised the demand for supplying reliable quantitative data of the mineralogy and the geochemistry for both the raw material and process samples. A research project was thus initiative to establish a robust analytical procedure to quantify both mineralogical as well as geochemical attributes of Kupferschiefer-type ores. A combination of analytical techniques is employed for this purpose, including quantitative X-ray diffraction (QXRD), image analysis based on scanning electron microscopy/mineral liberation analysis (MLA), XRF, ICP-AES, and INAA. Method development was based on selected Kupferschiefer samples obtained from Sangerhausen (Germany) and Polkowice-Sieroszowice (Poland) deposits.

QXRD by Rietveld refinement is particularly well-suited to determine the modal mineralogy of fine-grained samples. Five types of layer silicates were identified in Kupferschiefer samples. These are being characterized in detail in order to build crystal structure files needed to enable a full quantification of the minerals present. The necessary characterization of this set of layer silicates has been inhibited by the presence of organic matter, requiring chemical pre-treatment of the raw material that is specifically developed for this purpose.
SEM-based mineral liberation analysis (MLA) on grain mounts of crushed aliquots of the powder samples used for QXRD is used to verify mineral identification and to determine the amounts, liberation, and types of sulphide minerals contained in the samples. This technique is not suited to determine the abundance of the silicate minerals due to their fine-grained and intimately intergrown texture. Further obstacles, such as misidentification of disordered carbonate minerals by XRD or copper sulfides by MLA, are encountered often and can only be recognized and minimized by verifying results using multiple analytical methods. Independent observations from microscopy or bulk geochemistry by fusion XRF are useful in ensuring a high data quality and to test for consistency.
Whole rock trace element data are acquired using INAA, XRF, and ICP-OES. While INAA can guarantee a full analysis without requiring a problematic digestion treatment, the procedure itself is not available for routine measurements. XRF analysis of pressed pellets has been inhibited by the variable content of organic material and matrix effects caused by high sulfide concentrations. ICP-AES/MS analysis is considered to be the most appropriate technique in this case. Different combinations of hydrogen peroxide, nitric acid, and perchloric acid digestion techniques are tested to identify an optimal procedure for the acid digestion of the diverse sulfide compounds as well as the organic matter contained in Kupferschiefer.

Keywords: Kupferschiefer; Analysis; XRD; MLA; XRF; TXRF; ICP-OES; INAA

  • Poster
    The 9th International Conference on the Analysis of Geological and Environmental Materials - Geoanalysis 2015, 10.-13.08.2015, Leoben, Östereich

Publ.-Id: 22235

Multiscale structural characterizations of mixed U(IV)-An(III) oxalates (An(III) = Pu or Am) combining XAS and XRD measurements

Arab-Chapelet, B.; Martin, P.; Costenoble, S.; Delahaye, T.; Scheinost, A. C.; Grandjean, S.; Abraham, F.

Mixed actinides(III,IV) oxalates of general formula M2.2UIV1.8AnIII0.2(C2O4)5·nH2O (An = Pu or Am and M = H3O+ and N2H5+) have been quantitatively precipitated by oxalic precipitation in nitric medium (yield> 99%). Thorough multiscale structural characterizations by XRD and XAS measurements evidenced the existence of oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium are kept during the precipitation step. The local environments around U+IV, Pu+III and Am+III determined by EXAFS measurements are similar and show that cations are surrounded by five oxalate ligands. The mean metal-oxygen distances by XAS measurements are in agreement with those calculated from XRD lattice parameters. Finally, these An(III)-An(IV) oxalate solid solutions can be used to synthetize mixed actinide oxides characterized by a high homogeneity at molecular scale.

Keywords: Plutonium; Americium; XAFS; XRD; nuclear fuel; transmutation

Publ.-Id: 22234

Extremely large magnetoresistance and ultrahigh mobility in the topological Weyl semimetal candidate NbP

Shekhar, C.; Nayak, A. K.; Sun, Y.; Schmidt, M.; Nicklas, M.; Leermakers, I.; Zeitler, U.; Skourski, Y.; Wosnitza, J.; Liu, Z.; Chen, Y.; Schnelle, W.; Borrmann, H.; Grin, Y.; Felser, C.; Yan, B.

Recent experiments have revealed spectacular transport properties in semimetals, such as the large, non-saturating magnetoresistance exhibited by WTe2. Topological semimetals with massless relativistic electrons have also been predicted as three-dimensional analogues of graphene. These systems are known as Weyl semimetals, and are predicted to have a range of exotic transport properties and surface states, distinct from those of topological insulators. Here we examine the magneto-transport properties of NbP, a material the band structure of which has been predicted to combine the hallmarks of a Weyl semimetal with those of a normal semimetal. We observe an extremely large magnetoresistance of 850,000% at 1.85 K (250% at room temperature) in a magnetic field of up to 9 T, without any signs of saturation, and an ultrahigh carrier mobility of 5x106 cm2 V-1 s-1 that is accompanied by strong Shubnikov–de Haas (SdH) oscillations. NbP therefore presents a unique example of a material combining topological and conventional electronic phases, with intriguing physical properties resulting from their interplay.

Publ.-Id: 22233

Controllable Broadband Absorption in the Mixed Phase of Metamagnets

Pregelj, M.; Zaharko, O.; Zorko, A.; Gomilsek, M.; Sendetskyi, O.; Günther, A.; Ozerov, M.; Zvyagin, S. A.; Luetkens, H.; Baines, C.; Tsurkan, V.; Loidl, A.

Materials with broad absorption bands are highly desirable for electromagnetic filtering and processing applications, especially if the absorption can be externally controlled. Here, a new class of broadband-absorption materials is introduced. Namely, layered metamagnets exhibit an electromagnetic excitation continuum in the magnetic-field-induced mixed ferro-and anti-ferromagnetic phase. Employing a series of complementary experimental techniques involving neutron scattering, muon spin relaxation, specific heat, ac and dc magnetization measurements, and electron magnetic resonance, a detailed magnetic phase diagram of Cu3Bi(SeO3)2O2Br is determined and it is found that the excitations in the mixed phase extend over at least ten decades of frequency. The results, which reveal a new dynamical aspect of the mixed phase in metamagnets, open up a novel approach to controllable microwave filtering.

Publ.-Id: 22232

Depth Resolved Structural and Compositional Characterization of Ion-Implanted Polystyrene that Enables Direct Covalent Immobilization of Biomolecules

Bilek, M. M. M.; Kondyurin, A.; Dekker, S. A.; Steel, B. C.; Wilhelm, R. A.; Heller, R.; Mckenzie, D. R.; Weiss, A. S.; James, M.; Möller, W.

A polystyrene film spun onto polished silicon substrates was implanted with argon ions using plasma immersion ion implantation (PIII) in order to activate its surface for single step immobilization of biological molecules. The film was subsequently investigated by X-ray and neutron reflectometry, ultraviolet (UV)-visible (VIS) and Fourier transform infrared (FTIR) ellipsometry, FTIR and Raman spectroscopy, as well as nuclear reaction analysis to determine the structural and compositional transformations associated with the surface activation. The ion irradiation resulted in a significant densification of the carbon structure, which was accompanied by hydrogen loss. The density and hydrogen profiles in the modified surface layers were found to agree with the expected depths of ion implantation as calculated by the Stopping and Range of Ions in Matter (SRIM) software. The data demonstrate that the reduction in film thickness is due to ion-induced densification rather than the removal of material by etching. Characterization by FTIR, atomic force microscopy (AFM), ellipsometry and X-ray reflectometry shows that polystyrene films modified in this way immobilize dense layers of protein (tropoelastin) directly from solution. A substantial fraction of the immobilized protein layer remains after rigorous washing with sodium dodecyl sulfate solution, indicating that its immobilization is by covalent bonding.

Keywords: Plasma immersion ion implantation; polystyrene; protein immobilization; nuclear reaction analysis; X-ray reflectometry; neutron reflectometry; spectroscopic ellipsometry; Raman and FTIR spectroscopy

Publ.-Id: 22230

An investigation of the interactions of Eu3+ and Am3+ with uranyl minerals: implications for the storage of spent nuclear fuel

Biswas, S.; Steudtner, R.; Schmidt, M.; Mckenna, C.; Vintró, L. L.; Twamley, B.; Baker, R. J.

The reaction of a number of uranyl minerals of the (oxy)hydroxide, phosphate and carbonate types with Eu(III), as a surrogate for Am(III), have been investigated. A photoluminescence study shows that Eu(III) can interact with the uranyl minerals Ca[(UO2)6(O)4(OH)6]·8H2O (becquerelite) and A[UO2(CO3)3]·xH2O (A/x = K3Na/1, grimselite; CaNa2/6, andersonite; and Ca2/11, liebigite). For the minerals [(UO2)8(O)2(OH)12]·12H2O (schoepite), K2[(UO2)6(O)4(OH)6]·7H2O (compreignacite), A[(UO2)2(PO4)2]·8H2O (A = Ca, meta-autunite; Cu, meta-torbernite) and Cu[(UO2)2(SiO3OH)2]·6H2O (cuprosklodowskite) no Eu(III) emission was observed, indicating no incorporation into, or sorption onto the structure. In the examples with Eu3+ incorporation, sensitized emission is seen and the lifetimes, hydration numbers and quantum yields have been determined. Time Resolved Laser Induced Fluorescence Spectroscopy (TRLFS) at 10 K have also been measured and the resolution enhancements at these temperatures allow further information to be derived on the sites of Eu(III) incorporation. Infrared and Raman spectra are recorded, and SEM analysis show significant morphology changes and the substitution of particularly Ca2+ by Eu3+ ions. Therefore, Eu3+ can substitute Ca2+ in the interlayers of becquerelite and liebigite and in the structure of andersonite, whilst in grimselite only sodium is exchanged. These results have guided an investigation into the reactions with 241Am on a tracer scale and results from gamma-spectrometry show that becquerelite, andersonite, grimselite, liebigite and compreignacite can include americium in the structure. Shifts in the U=O and C-O Raman active bands are similar to that observed in the Eu(III) analogues and Am(III) photoluminescence measurements are also reported on these phases; the Am3+ ion quenches the emission from the uranyl ion. An unusual structure of a 3D uranyl framework is also reported.

Keywords: uranium; europium; emission spectroscopy

Publ.-Id: 22229

Polymer and cluster chemistry of tetravalent cerium in aqueous solutions - Comparison with tetravalent actinides

Ikeda-Ohno, A.; Weiss, S.; Hennig, C.

Cerium (Ce) is known to be the only lanthanide (Ln) which can be stabilized in the tetravalent state (i.e., Ce(IV)) in aqueous solutions. Owing to this chemical specificity, the aqueous chemistry of Ce(IV) shows unique characters as compared to that for the other Ln. For instance, due to its high charge density, the aqueous chemistry of Ce(IV) is predominantly characterised by strong hydrolysis. This strong hydrolysis results in the formation of a variety of hydroxide species even under acidic conditions.1 Moreover, the hydrolysis of Ce(IV) is often a primary step of many wet syntheses to yield nano-sized CeO2 particles which have many technological applications. Despite these chemical uniqueness and importance in applications, the aqueous chemistry of Ce(IV) is poorly understood even to date. Based on this background, this study aims to comprehensively understand the chemical behaviour of Ce(IV) in aqueous solutions by combining several spectroscopic (XAS, HEXS, DLS) and microscopic (TEM) techniques.

Keywords: f-elements; lanthanides; actinides; tetravalent; hydrolysis; aqueous solution; X-ray spectroscopy; TEM

  • Lecture (Conference)
    The 9th International Conference on f-Elements (ICfE 9), 08.09.2015, Oxford, United Kingdom

Publ.-Id: 22228

Bimodal grain size distribution of nanostructured ferritic ODS Fe-Cr alloys

Hilger, I.; Bergner, F.; Weißgärber, T.

Oxide dispersion strengthened Fe-Cr alloys produced by mechanical alloying and spark plasma sintering were found to form different heterogeneous hardness distribution and microstructures depending on the milling parameters. Microstructure investigations by means of electron diffraction techniques and atom probe tomography revealed the presence of large particle-free zones in one material, which is, together with the inhomogeneous deformation at short milling times, considered the main reason for the formation of a heterogeneous microstructure. The inhomogeneous temperature distribution in the sample volume during the sintering process is also expected to contribute to the formation of a heterogeneous grain size distribution in the final material.

Keywords: Spark plasma sintering; bimodal grain size; EBSD; Atom probe tomography; Nanoindentation; microstructure

Publ.-Id: 22227

Response of GaN to energetic ion irradiation: conditions for ion track formation

Karlušić, M.; Kozubek, R.; Lebius, H.; Ban-D’Etat, B.; Wilhelm, R. A.; Buljan, M.; Siketić, Z.; Scholz, F.; Meisch, T.; Jakšić, M.; Bernstorff, S.; Schleberger, M.; Šantić, B.

We investigated the response of wurzite GaN thin films to energetic ion irradiation. Both swift heavy ions (92 MeV Xe23+, 23 MeV I6+) and highly charged ions (100 keV Xe40+) were used. After irradiation, the samples were investigated using atomic force microscopy, grazing incidence small angle x-ray scattering, Rutherford backscattering spectroscopy in channelling orientation and time of flight elastic recoil detection analysis. Only grazing incidence swift heavy ion irradiation induced changes on the surface of the GaN, when the appearance of nanoholes is accompanied by a notable loss of nitrogen. The results are discussed in the framework of the thermal spike model.

Keywords: GaN; swift heavy ion; highly charged ion; ion track; thermal spike

Publ.-Id: 22226

Formation of shallow boron emitters in crystalline silicon using flash lamp annealing: Role of excess silicon interstitials

Riise, H. N.; Schumann, T.; Azarov, A.; Hübner, R.; Skorupa, W.; Svensson, B. G.; Monakhov, E.

Shallow, Boron (B)-doped p+ emitters have been realized using spin-on deposition and Flash Lamp Annealing (FLA) to diffuse B into monocrystalline float zone Silicon (Si). The emitters extend between 50 and 140 nm in depth below the surface, have peak concentrations between 9x1019 cm-3 and 3x1020 cm-3, and exhibit sheet resistances between 70 and 3000 Ohm/Square. An exceptionally large increase in B diffusion occurs for FLA energy densities exceeding approximately 93 J/cm2 irrespective of 10 or 20 ms pulse duration. The effect is attributed to enhanced diffusion of B caused by Si interstitial injection following a thermally activated reaction between the spin-on diffusant film and the silicon wafer.

Publ.-Id: 22225

Indium als Beiprodukt – Bedeutung von Geometallurgie und Rohstoffcharakterisierung

Frenzel, M.; Krause, J.; Bachmann, K.; Gutzmer, J.

Anhand des Beispiels von Indium wird gezeigt wie geometallurgische Denkweisen und Methoden auf typische Beiprodukte angewendet werden können. Besonders für Elemente wie Gallium, Germanium, Selen und Tellur fehlen bisher leider ähnliche Arbeiten völlig. Es wäre daher wünschenswert, dass solche an ausgewählten Lagerstätten durchgeführt werden. Auch für typische Strafelemente wie Cadmium oder Arsen könnte dies sinnvoll sein. Allerdings würde der Fokus bei letzteren eher auf der Vermeidung ihrer Anreicherung in den Konzentraten liegen. Die hier vorgestellte Arbeit könnte für solche Studien als Muster dienen.

  • ACAMONTA - Zeitschrift des Vereins der Freunde und Förderer der TU Bergakademie Freiberg 22(2015), 25-28

Publ.-Id: 22224

Petrographic characterization of REE-Nb-Zr mineralization at the Dubbo trachyte, NSW Australia

Müller, C.; Mentoren: Schulz, B.; Atanasova, P.; Gutzmer, J.

This thesis was the first study which intensively investigated the mineralisation and described the mineral transition between the supergene alterated and the main Toongi trachyte. Compared to other works on this trachyte the identified ore minerals differ. The works of Ramsden [1990, 1992] as well as the actually published mineral lists of Alkane resources Ltd. primarily deal with minerals of the supergene alterated zone. Within all three mineral lists there are major differences (cf. Table 5).
Due to the fact that this thesis, as well as the works of Ramsden, only used EDS measurements, a final evaluation is not possible.
The observed ore minerals often occur as small grains and as impregnation-like patches within the alterated matrix. Within the supergene alterated trachyte LREE are primary hosted by REEphosphates (monazite (Ce)) and zircon minerals, REE-fluorites (bastnaesite (Ce)) are not so important. HREE are primarily hosted by a Nb-Ta mineral. Major Nb hosting minerals are columbite and a Nb-Ta mineral. Zr is hosted by various Zr silicates, especially zircon. Within the main trachyte, LREE are hosted by REE-fluorites (bastnaesite (Ce)) and Zr-silicates (especially poikiloblastic zircon), REE-phosphates are not so important. HREE are primarily hosted by HREEY-(As) minerals. Major Zr hosting minerals are zircon and poikiloblastic zircon. Nb is primarily hosted by a Nb-Na mineral (natroniobite/lueshite) and less by a Nb-REE mineral. Most of the valuable minerals have a hydrothermal origin or they are products of alterated ores, respectively.
Only poikiloblastic zircon and Nb-Na-mineral have a magmatic origin.
Further investigations should confirm the mineral names by using more accurate measurements like X-Ray microanalysis. To determine the composition and temperature of the hydrothermal fluids the fluid inclusions should be investigated. Further investigations of samples out of the depths between 12 and 25 m (between sample DUB 5 and 6) could show the process of supergene mineral transformation more detailed.

Keywords: rare earth elements; metal deportment; trachyte

  • Master thesis
    TU Bergakademie Freiberg, 2015
    Mentor: Bernhard Schulz, Petya Atanasova, Jens Gutzmer
    116 Seiten

Publ.-Id: 22223

Distinguishing magmatic and metamorphic processes in the Norra Kärr alkaline complex, Southern Sweden

Atanasova, P.; Marks, M.; Krause, J.; Markl, G.; Gutzmer, J.

The Norra Kärr rare metal deposit in Southern Sweden represents one of the largest resources of rare earth elements (REE) in Europe. The mineralization is hosted by deformed agpaitic nepheline syenites covering an area 350 by 1100 m in size. REE-bearing minerals include eudialyte-group minerals (EGM) and minor mosandrite and britholite-group minerals. Zr is hosted by catapleiite and EGM.
The intrusion was emplaced between 1.55-1.40 Ga within the Transscandinavian Igneous Belt in an anorogenic (post Svecofennian) environment and deformed and metamorphosed during the Sveconorwegian (Grenvillian) orogeny between 1.25-0.85 Ga (e.g. Andersson et al., 2007). Microtextures and compositional variations in clinopyroxene and EGM are used to distinguish magmatic and metamorphic processes during the evolution of this rare metal mineralization.
Clinopyroxenes are invariably sodic and are characterized by early magmatic Zr-rich cores, euhedrally overgrown by presumably late magmatic aegirine, anhedrally overgrown by metamorphic Al-rich aegirine (jadeite). Similarly, EGM show complex distribution patterns of major and minor elements suggesting multiphase influence of fractional crystallization, recrystallization, fluid-induced re-mobilization and late alteration.

  • Open Access Logo Contribution to proceedings
    Goldschmidt 2015, 17.-21.08.2015, Prag, Tschechische Republik
    Goldschmidt2015 Abstracts: Cambridge Publications, 138-138
  • Poster
    Goldschmidt 2015, 20.08.2015, Prag, Tschechische Republik

Publ.-Id: 22222

Mass of GaAsN in Pulsed Magnetic Fields up to 60 T with Free-Electron Laser IR Radiation

Eßer, F.; Schneider, H.; Winnerl, S.; Drachenko, O.; Patanè, A.; Helm, M.

We use the unique combination of the widely tunable (4 μm – 250 μm) Free-Electron laser (FEL) FELBE and pulsed magnetic fields up to 60T of the High Magnetic Field Laboratory HLD to perform spectroscopic investigations on the dilute nitride system GaAsN. We carry out systematic cyclotron resonance (CR) spectroscopy and analyze the dependence of the electron effective mass on the nitrogen content. The red triangles in Figure 1 illustrate our findings for the illumination wavelength 46 μm at 100 K. We observe a slight increase of the effective mass with nitrogen content, which is in very good agreement with the Band Anti-Crossing (BAC) model [1], the empirical Tight Binding (TB) calculations [2] and the Two band BAC model [3], which are represented in Figure 1 by dashed, dotted and dash-dotted black lines, respectively. We compare our results with magneto-photoluminescence (PL) investigations performed by Alberi et al. [4] and Masia et al. [5], which are presented with blue circles and stars respectively. Magneto-PL investigations reveal a very fast increase of the effective mass with nitrogen content, well above the mentioned models [1-3], but consistent with the modified k·p calculations by Lindsay and O’Reilly [6]. Our magneto-PL study (not shown) exhibits a very similar behavior as shown by Alberi et al. and Masia et al., which allows us to exclude the different samples as a source for the deviation.
It is well known that nitrogen tends to form pairs and clusters during the growth, which is only considered in the modified k·p calculations [4]. Magneto-PL is a method which is very sensitive to localization of the neighboring atoms and thus to clusters. For this reason the magneto-PL results are consistent with [4], but cannot be described by [1-3], which do not take clusters into account. On the other hand, CR spectroscopy is only sensitive to delocalized states and this is why our results are in such good agreement with [1-3].

[1] J. Wu et al. Phys. Rev. B 64, 085320 (2000).
[2] N. Shtinkov et al. Phys. Rev. B 67, 081202(R) (2003).
[3] Tomic et al. Phys. Rev. B 69, 245305 (2004).
[4] Alberi et al. Phys. Rev. Lett. 110, 156405 (2013).
[5] Masia et al. Phys. Rev. B 73, 073201, (2006).
[6] A. Lindsay and E. P. O’Reilly Phys. Rev. Lett. 93, 196402 (2004).

Keywords: GaAsN; effective mass; cyclotron resonance spectroscopy; THz spectroscopy in pulsed magnetic fields

  • Lecture (Conference)
    RHMF 2015; International Conference on Research in High Magnetic Fields 2015, 01.-04.07.2015, Grenoble, France

Publ.-Id: 22221

Constraining big bang lithium production with recent solar neutrino data

Takács, M. P.; Bemmerer, D.; Szücs, T.; Zuber, K.

The 3He(α, γ)7Be reaction affects not only the production of 7Li in Big Bang nucleosynthesis, but also the fluxes of 7Be and 8B neutrinos from the Sun. This double role is exploited here to constrain the former by the latter. A number of recent experiments on 3He(α,γ)7Be provide precise cross section data at E = 0.5-1.0 MeV center-of-mass energy. However, there is a scarcity of precise data at Big Bang energies, 0.1-0.5 MeV, and below. This problem can be alleviated, based on precisely calibrated 7Be and 8B neutrino fluxes from the Sun that are now available, assuming the neutrino flavour oscillation framework to be correct. These fluxes and the standard solar model are used here to determine the 3He(α,γ)7Be astrophysical S-factor at the solar Gamow peak, Sν (23+6 keV) 34 −5 = 0.548±0.054 keVb. This new data point is then included in a re-evaluation of the 3He(α,γ)7Be S-factor at Big Bang energies, following an approach recently developed for this reaction in the context of solar fusion studies. The re-evaluated S-factor curve is then used to re-determine the 3He(α,γ)7Be thermonuclear reaction rate at Big Bang energies. The predicted primordial lithium abundance is 7Li/H = 5.0 ×10−10, far higher than the Spite plateau.

Keywords: solar neutrinos; S34; Big Bang; Standard Solar Model

Publ.-Id: 22220

Cyclotron Resonance Spectroscopy of GaAsN in Pulsed Magnetic Fields up to 60 T with Free-Electron Laser IR Radiation

Eßer, F.; Schneider, H.; Winnerl, S.; Drachenko, O.; Patanè, A.; Pettinari, G.; Helm, M.

The unique combination of the high magnetic field laboratory Dresden (HLD) and the free-electron laser facility FELBE allow us to perform cyclotron resonance spectroscopy experiments with tunable, intense, coherent infrared radiation of high brilliance in the range of 4 - 250 µm in pulsed magnetic fields up to 60 T. The material system of interest is the dilute nitride GaAsN, a promising candidate for electro-optical applications, because of its band gap tunability. The incorporation of a few percent of nitrogen into GaAs enables the gradual decrease of the band gap, which is proportional to the nitrogen content. The description of the band structure and in particular of the effective mass are still challenging despite the number of experimental works (e.g. [1, 2]) that have been performed on this system. In order to contribute to a clarification of this problem, we apply different investigation methods on one sample series of GaAsN with different nitrogen contents (0%; 0.1%; 0.2%).
Probably the most direct and reliable method for the investigation of the effective mass is cyclotron resonance spectroscopy, which has never been applied to bulk GaAsN layers before, according to our best knowledge. Figure 1 illustrates our CR spectroscopy investigation of three samples with different nitrogen contents illuminated with the FEL at wavelengths of 30 µm and 70 µm. These wavelengths have been chosen intentionally to investigate the effective mass behavior below and above the Reststrahlenband of GaAs. We discuss the significance of these CR studies, which were conducted using a range of temperatures, illumination wavelengths and n-type doping of the GaAsN layers. Using a simple Drude-like absorption model we deduce the electron CR mass, the electron mobility, the density of free carriers and the electron relaxation time.

[1] F. Masia et al., Phys. Rev. B 73, 07320 (2006).
[2] K. Alberi et al., Phys. Rev. Lett. 110, 156405 (2013).

Keywords: GaAsN; effective mass; cyclotron resonance spectroscopy; THz spectroscopy in pulsed magnetic fields

  • Lecture (Conference)
    EDiSON'19 19th International Conference on Electron Dynamics in Semiconductors, Optoelectronics and Nanostructures, 29.06.-02.07.2015, Salamanca, España

Publ.-Id: 22219

THz free-electron laser investigation of GaAsN in pulsed magnetic fields up to 60 T

Eßer, F.; Schneider, H.; Winnerl, S.; Drachenko, O.; Patanè, A.; Helm, M.

We use the unique combination of the free-electron laser FELBE and the High Magnetic Field Laboratory Dresden to perform cyclotron resonance (CR) spectroscopy on the dilute nitride alloy GaAsN. FELBE is a tunable (4 – 250 µm) laser source of high brilliance, which can be used in pulsed magnetic fields up to 60 T. Our CR studies enable us to measure fundamental electronic properties of GaAsN, a very interesting candidate for optoelectronic applications because of the tunability of its band gap energy in the range of 1.4 eV – 0.9 eV by the incorporation of a small concentration of N-atoms (~ 1%). Figure 1 illustrates a typical CR spectrum and our values of the CR electron mass at 100 K and 6.5 THz. We observe a slight increase of the electron CR mass with nitrogen content. This dependence is in very good agreement with that described by the band anticrossing (BAC) model [1] and the empirical tight binding (TB) calculations [2], which are represented in Figure 1 by dashed and dotted black lines, respectively. The comparison with magneto-photoluminescence (PL) investigations performed by Alberi et al. [3] and Masia et al. [4] reveal instead a steep increase of the electron effective mass with nitrogen content, which is consistent with a modified k·p calculation by Lindsay and O’Reilly [5]. This model assumes that nitrogen can form pairs and clusters, not considered in [1,2]. Since PL is very sensitive to carrier localization effects, the results in [3,4] can be well described by [5]. In contrast, CR spectroscopy is only sensitive to delocalized states, which explains the good agreement of the present results with [1,2].

[1] J. Wu et al. Phys. Rev. B 64, 085320 (2000).
[2] N. Shtinkov et al. Phys. Rev. B 67, 081202(R) (2003).
[3] Alberi et al. Phys. Rev. Lett. 110, 156405 (2013).
[4] Masia et al. Phys. Rev. B 73, 073201, (2006).
[5] A. Lindsay and E. P. O’Reilly Phys. Rev. Lett. 93, 196402 (2004).

Keywords: GaAsN; effective mass; cyclotron resonance spectroscopy; THz spectroscopy in pulsed magnetic fields

  • Poster
    German THz Conference 2015, 08.-10.06.2015, Dresden, Deutschland

Publ.-Id: 22218

Triadic resonances in nonlinear simulations of a fluid flow in a precessing cylinder

Giesecke, A.; Albrecht, T.; Gundrum, T.; Herault, J.; Stefani, F.

We present results from three-dimensional non-linear hydrodynamic simulations of a precession driven flow in cylindrical geometry. The simulations are motivated by a dynamo experiment currently under development at Helmholtz-Zentrum Dresden-Rossendorf (HZDR) in which the possibility of generating a magnetohydrodynamic dynamo will be investigated in a cylinder filled with liquid sodium and simultaneously rotating around two axes.
In this study, we focus on the emergence of non-axisymmetric time-dependent flow structures in terms of inertial waves which – in cylindrical geometry – form so-called Kelvin modes. For a precession ratio Γ = Ωp /Ωc = 0.014 considered by us, the amplitude of the forced Kelvin mode reaches up to one fourth of the rotation velocity of the cylindrical container confirming that precession provides a rather efficient flow driving mechanism even at moderate values for Γ.
More relevant for dynamo action might be free Kelvin modes with higher azimuthal wave number. These free Kelvin modes are triggered by non-linear interactions and may constitute a triadic resonance with the fundamental forced mode when the height of the container matches their axial wave lengths. Our simulations reveal triadic resonances at aspect ratios close to those predicted by the linear theory except around the primary resonance of the forced mode. In that regime we still identify various free Kelvin modes, however, all of them exhibit a retrograde drift around the symmetry axis of the cylinder and none of them can be assigned to a triadic resonance.
The amplitudes of the free Kelvin modes always remain below the forced mode but may reach up to 6% of the of the container’s angular velocity. The properties of the free Kelvin modes, namely their amplitude and their frequency, will be used in future simulations of the magnetic induction equation to investigate their ability to provide for dynamo action.

Keywords: Precession; DRESDYN; Dynamo

Publ.-Id: 22217

Design of compensated ferrimagnetic Heusler alloys for giant tunable exchange bias

Nayak, A. K.; Nicklas, M.; Chadov, S.; Khuntia, P.; Shekhar, C.; Kalache, A.; Baenitz, M.; Skourski, Y.; Guduru, V. K.; Puri, A.; Zeitler, U.; Coey, J. M. D.; Felser, C.

Rational material design can accelerate the discovery of materials with improved functionalities. This approach can be implemented in Heusler compounds with tunable magnetic sublattices to demonstrate unprecedented magnetic properties. Here, we have designed a family of Heusler alloys with a compensated ferrimagnetic state. In the vicinity of the compensation composition in Mn–Pt–Ga, a giant exchange bias (EB) of more than 3 T and a large coercivity are established.
The large exchange anisotropy originates from the Exchange interaction between the compensated host and ferrimagnetic clusters that arise from intrinsic anti-site disorder. Our design approach is also demonstrated on a second material with a magnetic transition above room temperature, Mn–Fe–Ga, exemplifying the universality of the concept and the feasibility of room-temperature applications. These findings may lead to the development of magneto-electronic devices and rareearth-free exchange-biased hard magnets, where the second quadrant magnetization can be stabilized by the exchange bias.

Publ.-Id: 22216

Preferential adsorption of Cu in a multi-metal mixture onto biogenic elemental selenium nanoparticles

Jain, R.; Dominica, D.; Jordan, N.; Rene, E. R.; Weiss, S.; van Hullebusch, E. D.; Hübner, R.; Lens, P. N. L.

Preferential adsorption of Cu contained in wastewaters is desirable as the Cu can then be reprocessed and reused more easily. In this study, biogenic elemental selenium nanoparticles (BioSeNPs) were assessed for their ability to preferentially adsorb Cu from an equimolar mixture containing Cu, Cd and Zn. Both metal to BioSeNPs ratio and initial metal solution pH have been shown to affect the preferential adsorption capacity of BioSeNPs towards Cu. BioSeNPs adsorbed 2.3 times more Cu from an equimolar mixture of Cu, Zn and Cd at an initial metal solution pH of 5.2 and metal to BioSeNPs ratio of 0.21 mg mg−1, while adsorbing more than 78% of added Cu. Infrared spectroscopy revealed that the Cu, Cd and Zn were interacting with hydroxyl and carboxyl surface functional groups of the BioSeNPs. The modeling of BioSeNPs' acid-base titration revealed the presence of high concentrations of carboxylic groups (C = 60.26 mol Kg−1) with a pKa of 3.9 providing, further evidence of their interaction with Cu. The adsorption of Cu resulted in a lower colloidal stability of the BioSeNPs as indicated by less negative ζ-potential values. BioSeNPs showed good preferential adsorption capacity towards Cu when compared to oxidized carbon nanotubes. This study provides proof-of-concept for preferential adsorption of Cu onto BioSeNPs which are present in the effluent of a bioreactor treating selenium oxyanions containing wastewater.

Keywords: preferential adsorption; biogenic; selenium nanoparticles; heavy metals; FT-IR

Publ.-Id: 22215

Ga, Ge, In and other trace elements in sphalerite from different geological deposit types, with reference to mineralisation events at Freiberg.

Frenzel, M.

Sphalerite (ZnS) is an important source of a number of high-tech metals. However, while a large amount of analytical data on trace and minor element concentrations in sphalerite has been collected over the last decades, our understanding of the geological controls on their enrichment or depletion remains limited. No comprehensive meta-analysis of this data has ever been conducted. This talk presents the results of such a meta-analysis, based on an extensive collection of data from the scientific literature. Nine elements (Ag, Cd, Co, Cu, Fe, Ga, Ge, In and Mn) were considered. For five of these elements (Fe, Ga, Ge, In, Mn) significant differences were found between different geological types of deposits. The regularity of these differences suggests the operation of a single underlying control parameter – possibly formation temperature – with obvious implications for the identification of future sources of these elements.

  • Lecture (others)
    BHMZ Seminar, 06.05.2015, Freiberg, Deutschland

Publ.-Id: 22214

The role of geoscientists in securing the future supply of high technology minerals and metals

Gutzmer, J.; Birtel, S.; Frenzel, M.

The availability of minerals and metals required for high technology applications has in recent years been widely recognized as being of strategic importance for future development - especially for highly industrialized economies. Because the absolute tonnage of such high technology minerals and metals in industrial products is typically small, inventories in the technosphere will remain limited and widely disseminated. This will significantly hamper recycling efforts. As a direct consequence, primary resources will need to be utilized to secure supply into the foreseeable future. Tapping primary resources appears as a reasonable approach, as these are readily available for most high technology metals. Geoscientists will have to make an important contribution – not only towards exploration and discovery, but also to the implementation of technological concepts for comprehensive resource utilization, i.e., mining operations that are not only economic, but also resource-efficient and environmentally benign.

Keywords: High technology metals; criticality; exploration; mineral systems analysis; geometallurgy

  • Lecture (Conference)
    12th Biennial SGA Conference, 12.-15.08.2013, Uppsala, Sverige

Publ.-Id: 22213

Pages: [1] [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] [12] [13] [14] [15] [16] [17] [18] [19] [20] [21] [22] [23] [24] [25] [26] [27] [28] [29] [30] [31] [32] [33] [34] [35] [36] [37] [38] [39] [40] [41] [42] [43] [44] [45] [46] [47] [48] [49] [50] [51] [52] [53] [54] [55] [56] [57] [58] [59] [60] [61] [62] [63] [64] [65] [66] [67] [68] [69] [70] [71] [72] [73] [74] [75] [76] [77] [78] [79] [80] [81] [82] [83] [84] [85] [86] [87] [88] [89] [90] [91] [92] [93] [94] [95] [96] [97] [98] [99] [100] [101] [102] [103] [104] [105] [106] [107] [108] [109] [110] [111] [112] [113] [114] [115] [116] [117] [118] [119] [120] [121] [122] [123] [124] [125] [126] [127] [128] [129] [130] [131] [132] [133] [134] [135] [136] [137] [138] [139] [140] [141] [142] [143] [144] [145] [146] [147] [148] [149] [150] [151] [152] [153] [154] [155] [156] [157] [158] [159] [160] [161] [162] [163] [164] [165] [166] [167] [168] [169] [170] [171] [172] [173] [174] [175] [176] [177] [178] [179] [180] [181] [182] [183] [184] [185] [186] [187] [188] [189] [190] [191] [192] [193] [194] [195] [196] [197] [198] [199] [200] [201] [202] [203] [204] [205] [206] [207] [208] [209] [210] [211] [212] [213] [214] [215] [216] [217] [218] [219] [220] [221] [222] [223] [224] [225] [226] [227] [228] [229] [230] [231] [232] [233] [234] [235] [236] [237] [238] [239] [240] [241] [242] [243] [244] [245] [246] [247] [248] [249] [250] [251] [252] [253] [254] [255] [256] [257] [258] [259] [260] [261] [262] [263] [264] [265] [266] [267] [268] [269] [270] [271] [272] [273] [274] [275] [276] [277] [278] [279] [280] [281] [282] [283] [284]