Publications Repository - Helmholtz-Zentrum Dresden-Rossendorf

Radiometals play an important role in nuclear medicine^1-3 for the diagnosis or therapy of various diseases. Beside technetium-99m, the most frequently used radionuclide for in-vivo- diagnosis because its optimal nuclide properties, economically supply by the ⁹⁹Mo/^99mTc generator and easy preparation of the ^99mTc-radiopharmaceutical in the clinic, current search for metalloradiopharmaceuticals focuses on both unconventional positron emitting metals (e.g. Cu-64, Ga-66, Y-86, Tc-94m) as potential agents for positron emission tomography (PET) and of radiometal agents labeled with particle emitters for radionuclide therapy³. Since the basic requirement for therapeutic radiopharmaceuticals, namely to induce high effective dose for the target but practically no interference with healthy tissue is not fulfilled yet, the number of therapeutic radiopharmaceuticals for routine use is limited.
Besides the availability of suitable nuclides, the design of chelate systems for stable binding of the radiometal is a crucial point in the development of new metalloradiopharmaceuticals. The chemistry of respective chelates designed in recent years for binding technetium and rhenium at various oxidation states will be discussed. Such chelates involve mixed-ligand complexes containing the metalnitrido core at oxidation state V, Tc(III)/Re(III) and organometallic Tc(I)/Re(I) complexes.
Finally, the application of these chelates for labeling peptides and receptor-affine coordination compounds will be demonstrated.

Visualisation of primary prostate cancer and its metastases remains a clinical important problem, state-of-the-art methods like CT, MRI, TRUS (transrectal ultrasound) and ¹⁸F-FDG PET notwithstanding. The difficulties are even more pronounced in case of local recurrence as ¹⁸F-FDG PET, while useful in the detection of metastases, is not considered helpful in the investigation of relapse. The aim of this study was to evaluate the efficacy of ¹¹C-acetate and ¹⁸F-FDG-PET in the detection of prostate cancer and its metastases in patients treated with or without hormonal ablation.
25 patients (age: 54 to 82 years) were investigated during follow-up of a primary prostate cancer, suspected relapse, or metastatic disease using ¹¹C-acetate PET and 15 with ¹⁸F-FDG PET additionally. 14 Patients had antiandrogen treatment at the time of the investigation, the other 11 patients were drug-naive.
Primary tumours were detected in 20/24 (83%) patients using ¹¹C-acetate PET and in 10/15 (75%) patients using ¹⁸F-FDG PET. Based on the results of both PET scans, one patient was diagnosed with a lung cancer as second malignancy. Median ¹⁸F-FDG uptake exceeded that ¹¹C-acetate in distant metastases (SUV=3.2 vs. 2.3, respectively). ¹¹C-acetate uptake, however, was higher in local recurrence and in local lymph node metastases (median SUVs = 2.9 and 3.8) compared to ¹¹C-acetate (median SUVs = 1.0 and 1.1, respectively). ¹¹C-acetate and ¹⁸F-FDG uptake was lower in patients on antiandrogen therapy compared with the drug-naïve patients but ¹¹C-acetate uptake was not significantly impaired. A close correlation of serum PSA level and Gleason score on the one hand and both ¹¹C-acetate uptake and ¹⁸F-FDG uptake on the other hand was observed.
These data confirm that ¹¹C-acetate is more useful than ¹⁸F-FDG in the detection of local recurrences and localised lymph node metastases. ¹⁸F-FDG, however, appears to be more accurate in visualising distant metastases. Antiandrogen therapy reduces tumour metabolic activity and therefore overall PET accuracy but detection of local recurrences by ¹¹C-acetate is not severly compromised. Ultimately, there may be a role for combined ¹¹C-acetate/¹⁸F-FDG PET in the follow-up of patients with prostate cancer and persisting or increasing PSA.

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The influence of the formation of secondary iron phases on the sorption behavior of U(VI) on chlorite was investigated in batch sorption experiments with two different types of chlorites: an unaltered chlorite from Flagstaff Hill (CCa-2) and a hydrothermally altered chlorite from Grimsel/Switzerland. The easily extractable ions have not been removed in the CCa-2 chlorite and it therefore tends to form secondary phases. In contrast, the hydrothermally altered chlorite is relative resitant to weathering as discussed in Arnold et. al. [1] and therefore does not tend to form secondary phases. The batch sorption experiments were carried out under ambient temperature and pressure using a solid concentration of 0,5 g chlorite in 40 mL 0,1 M NaClO4 solution. The higher sorption capacity of the unaltered CCa-2 chlorite of more than 20 % of the initially added 1´10-6 M U(VI) compared to the hydrothermally altered chlorite is especially striking in the pH region from 6,5 to 8,5 and was attributed to the generation of secondary Fe and Al phases forming during the two months period of the batch sorption experiments. As a consequence of the formation of a new phase additional mineral surface area is generated [2] which serves as a substrate for further uranium sorption. It is well known that Fe-oxyhydroxide particles show a very high affinity for sorbing U(VI) [3]. Our results clearly show that newly-forming secondary phases may increase the sorption capacity of primary minerals. The Diffuse Double Layer Model (DDLM) was applied to model the U(VI) sorption on the two chlorites including the newly-formed secondary phases.

This class of flows is characterized by the feeding of strong electrical currents into a volume of liquid metal. A prominent example of industrial interest is the electrode-welding where the current is supplied via a locally restricted area, leading to high current densities. The interaction of these currents with their own magnetic field drives flows which exhibit phenomena like formation of jets and pinch-effect. Further increasing the current may lead to disruption of the melt column accompanied with a discharge. This can be used for a liquid metal current limiter with self-healing properties.
Local measurements of the flow structures are of obvious interest for a better understanding of these phenomena. The paper will give results from a systematic study of the flow structure performed by means of our mechano-optical velocity probe. The measured flow structure of the evolving jet was found to be in a reasonable agreement with our numerical simulations.

Passing an electrical current through a volume of conducting fluid drives flow via the interaction with its own magnetic field. Among this class of electro-vortical flows the electrode-welding is a prominent example of industrial interest. In such configurations where a strong current is supplied locally, the resulting high current densities show phenomena like formation of jets and pinch-effect. The latter may disrupt the melt column in the case of very strong currents, accompanied by a discharge. Thus pinching can be used for a liquid metal current limiter with self-healing properties.
Local flow measurements are important for a better understanding of these phenomena. This paper gives results from a systematic study of the fluid motion performed with our mechano-optical velocity probe. The measured flow structure of the evolving jet was found to be in a reasonable agreement with our numerical simulations. Local pressure measurements have been consistent with the experimental and numerical results for the flow field.

Nonlinear probing of the fundamental lattice vibration of polar crystals is shown to reveal insight into higher-order cohesive lattice forces. With a free-electron laser tunable in the far infrared we experimentally investigate the dispersion of the second-order susceptibility due to the phonon resonance in GaAs. We observe a strong resonance enhancement of second harmonic light generation at half the optical phonon frequency, and in addition a minimum at a higher frequency below the phonon frequency. Measuring this frequency and comparison to a theoretical model allows the determination of competing higher-order lattice forces.

195-keV Fe+ Ionen wurden mit einer nominellen Dosis von 5x10E16 cmE-2 bei Raumtemperatur in einen GaN(0001)-Wafer implantiert.

Half-sandwich complexes of the type (RCOCp)M(CO)₃] with M ) Re and ^99(m)Tc were synthesized from [M(OH₂)_3-(CO)₃]⁺ in water. The R group can be an organic residue or a receptor binding biomolecule with a spacer to cyclopentadienyl (Cp). This provides a general route to Cp complexes of technetium without the need for starting from [TcBr(CO)₅].
The X-ray structure of [{C_6H5CH₂COC₅H₄}Tc(CO)₃] has been elucidated. The compound crystallizes in the monoclinic space group P2₁/c with a = 16.1454(9), b = 7.6300(6), and c = 12.3922(7) Å and beta = 107.792(6)°. We have chosen a serotonergic receptor ligand (WAY) as an example for the derivatization of Cp with a bioactive molecule. WAY is linked to Cp by an aliphatic chain of variable length. The half-sandwich complexes were prepared from water and organic solvents. The structure of [(WAY4-Cp)Re(CO)₃] could be elucidated. The compound crystallizes in the monoclinic space group P2₁/c with a = 15.7112(6), b = 6.8775(3), and c = 25.5217(12) Å and beta = 103.778(5)°. Quantification of inhibition constants gave a clear structure-activity relationship. A single methylene group between the receptor binding site and the half-sandwich complex gave an IC₅₀ of 217 nM for T_1A, whereas a butylene linker resulted in retention of the inhibition constant with an IC₅₀ of 6 nM with respect to underivatized WAY. For use as radiopharmaceuticals, the compounds have also been prepared with ^99mTc in quantitative yield.

The [¹⁸F]fluoromethyl analogue of (+)-McN5652 ([¹⁸F]FMe-McN) has recently been developed as a radioligand for imaging the neuronal serotonin transporter (SERT) with positron emission tomography (PET). We describe here the autoradiographic evaluation of [¹⁸F]FMe-McN in the brain of rats and pigs. Autoradiographic studies of [¹⁸F]FMe-McN performed on rat and pig brain in vitro showed a high accumulation of radioactivity in the regions rich in SERT, such as amygdala, hypothalamus, superficial gray layer of the superior colliculus, various nuclei of thalamus and substantia nigra. The binding of [¹⁸F]FMe-McN was reduced by citalopram, a highly selective inhibitor for SERT. Similar regional specific binding densities of [¹⁸F]FMe-McN were observed in both species. The regional distribution and specific binding of this radiotracer correlates well with the distribution and regional brain binding of [³H]citalopram. Region-to-cerebellum ratios of [¹⁸F]FMe-McN in vitro reached a maximum value of 20.6 in the rat and 14.5 in the pig. In addition, ex vivo autoradiography of the rat brain was performed 90 min after i.v. administration of [¹⁸F]FMe-McN. The highest regional uptake of [¹⁸F]FMe-McN was observed in the hypothalamic area, substantia nigra and amygdaloid area. There is a high correlation between the in vitro and in vivo binding. The region-to cerebellum ratio in vivo reached a maximum value of 5.1 in the substantia nigra, the highest yet reported for a ¹⁸F-labelled SERT tracer in vivo in this region. Furthermore, the distribution volume of [¹⁸F]FMe-McN calculated from the PET data in various regions of the porcine brain is highly correlated with the SERT density as determined by in vitro autoradiography with [³H]citalopram. Thus, [¹⁸F]FMe-McN has a clear potential as a radiotracer for studies of the SERT distribution in man with PET.

Das vorliegende Projekt hatte die Ermittlung der räumlichen und zeitlichen Verteilung der Kühlmittelparameter am Spaltzoneneintritt bei transienten Prozessen zum Ziel, bei denen an den einzelnen Kühlmitteleintrittsstutzen des Reaktors Unterschiede in der Borkonzentration bzw. in der Kühlmittel-temperatur auftreten. Die Sicherheitsrelevanz ist durch die Auswirkungen von Deborierungs- und Kaltwassertransienten auf die Leistungsfreisetzung im Reaktorkern gegeben.Mit Hilfe von Experimenten an einem Reaktormodell sowie durch Validierung und Nutzung eines dreidimensionalen Fluidynamikcodes (CFX-4) und durch Entwicklung eines vereinfachten Vermischungsmodells (SAPR) wurden die für die Ermittlung der reaktordynamischen Systemantwort notwendigen Tools zur Beschreibung der Verhältnisse am Kerneintritt geschaffen. Mit der Modellierung der räum-lich und zeitlich aufgelösten Bor- bzw. Temperaturverteilung im RDB wurden die Voraussetzungen für die gekoppelte neutronenkinetisch-thermohydraulische Simulation von Deborierungs- und Kaltwas-sertransienten und deren Sicherheitsbewertung entwickelt. Das Vorhaben beschränkt sich auf Vor-gänge ohne Verdampfung des Kühlmittels, die Vermischung innerhalb des Reaktorkerns bleibt aus-geklammert. Um Mehrfachzirkulationen von Temperatur- bzw. Borkonzentrationsstörungen im Pri-märkreis adäquat abbilden zu können, wurde auch die Vermischung im oberen Plenum behandelt. Zur Lösung der Aufgabe wurde die Versuchsanlage ROCOM (Rossendorf Coolant Mixing Model) aufgebaut. ROCOM ist ein 1:5-Modell eines KONVOI DWR. Durch die volle Abbildung aller vier Um-wälzschleifen, die flexible Versuchssteuerung sowie die speziell für ROCOM entwickelte Gittersen-sormesstechnik zur räumlich und zeitlich hochauflösenden Bestimmung von Konzentrationsverteilungen stellt ROCOM heute eine weltweit führende Versuchsanlage dar. Bei den Experimenten wurden transiente Konzentrationsverteilungen am Kerneintritt für alle gemäß Arbeitsplan zu betrach-tenden Szenarien ermittelt und zur Validierung von CFX-4 genutzt. Das vereinfachte Vermischungs-modell SAPR dient zur effizienten Kopplung zwischen dem thermohydraulischen Systemcode und dem dreidimensionalen neutronenkinetischen Kernmodell.

Proper characterization of tin doped indium oxide (ITO) films prepared at various deposition parameters is important to produce the layers with low resistivity and high luminous transmittance. Therefore, thin ITO films were grown on insulating substrates by means of pulsed reactive dual magnetron sputtering at different base pressure, magnetron pulse duration and Ar/O2 ratio. To characterize the layers after deposition, spectroscopic ellipsometry (SE) was applied in combination with optical transmittance and resistivity measurements. Surface roughness obtained by SE was corroborated by atomic force microscopy. A significant variation in film deposition rate was observed for experiments with different magnetron pulse duration due to SE results. It agrees with Auger depth profiling data. The latter also showed that the O/In ratio values close to 1.5 correspond to the lowest film resistivity. For ITO films produced at various deposition conditions it was observed that SE derived free electron parameters ratio demonstrates certain minimum. It corresponds to the lowest film resistivity and high transmittance. SE was also applied in situ as a non contact technique to monitor ITO film resistivity optimization during annealing.

Reactive magnetron sputtering provides possibility of high-quality tin doped indium oxide In2O3:Sn (ITO) film deposition on a large substrates at low temperature. Although resistivity and transmittance of ITO films prepared by this technique greatly depend on the deposition parameters [1], which have to be optimized. Unique combination of the ITO properties is controlled by its electronic band structure parameters [2]; the latter can be characterized by optical methods. That is why, this work is focused on application of spectroscopic ellipsometry (SE) for probing of ITO layers.

The ITO films were grown by sputtering of metallic In (90%) - Sn (10%) alloy targets in atmosphere of Ar and O2 mixture by using pulsed dual magnetron system. Base pressure, Ar/O2 ratio and magnetron pulse duration have been varied during the deposition. The films were prepared on Si (100) covered with 500 nm SiO2 and soda lime glass substrates. Spectroscopic ellipsometry was applied within the wavelength range 300-1700 nm in combination with optical transmittance measurements. The spectral dependences of ellipsometric parameters were acquired in autoretarder mode. SE data were fitted simultaneously with transmittance data by using the model of rough graded layer [3] on substrate.

Such approach yielded ITO film thickness and roughness values, which were corroborated by profilometry and atomic force microscopy respectively. A significant variation in film deposition rate was observed only for experiments with different magnetron pulse duration. This parameter is minimal at 50 µs magnetron on-time, than it reaches maximum at 125 µs followed by further decrease at longer pulse durations. Such behavior can be related to changes in plasma density with variation of pulse length that was obtained by Langmuir probe measurements. The film lowest resistivity at high transmittance was achieved at pulse length 100-150 µs. The ITO optical constants were parameterized in Drude-Lorentz approach that permitted to obtain free electron parameters (plasma, wp, and relaxation, wt, frequencies) and interband transition characteristics. Vertical grading of optical constants through the film was quantified. During variation of base pressure, Ar/O2 ratio and pulse duration the minimum values of wt/wp^2 were reached at optimal deposition parameters that provided the lowest resistivity (3.2 mOhm·cm) of the film along with the high transmittance (0.84 for 180 nm thickness). For non optimal deposition parameters the behavior of wt/wp2 ratio qualitatively resembled resistivity dependence. Only in the vicinity of optimal deposition parameters resistivity is proportional to the ratio wt/wp^2 that points on the applicability of free electron approach in this case. For non optimal deposition parameters mechanisms of electric resistivity are more complex and require more detailed investigation of the film structure.

[1] R.B.H. Tahar, T. Ban, Y. Ohya, Y. Takahashi, J. Appl. Phys., 83 (1998) 2631
[2] O.N. Mryasov, A.J. Freeman, Phys. Rev. B, 64 (2001) 233111.
[3] R.A. Synowicki, Thin Solid Films 313-314 (1998) 394.

Investigations of processes involving actinides and bacteria in environments around nuclear waste repositories are needed for improvement of the scientific basis for performance of safety assessments. Sulfate reducing bacteria (SRB) are of special interest due to their ability to reduce many metals and actinides. Motamedi and Pedersen showed that SRB are frequently distributed in the deep granitic rock aquifers at the Äspö Hard Rock Laboratory (HRL, Sweden) [1]. The presented work is focussed on interactions of curium (III) and uranium (VI) with the strain Desulfovibrio äspöensis, DSM 10631T, recovered from the deep granitic groundwater at the Äspö site [1].
The interaction of D. äspöensis with Cm (III) was investigated by time-resolved laser fluorescence spectroscopy (TRLFS) in the trace concentration range. No evidences were found for changes in the oxidation state of Cm (III). At pH 3, no interaction between Cm (III) and bacteria was detected. With increasing pH, a surface complexation of Cm (III) occurs at the cell walls. The Cm (III)/bacteria surface complex is characterized by its emission spectrum (peak maximum at 600 nm) and its fluorescence emission lifetime (160 ± 15 µs).
80 % of the U (VI), solved initially (0.02 mM) in a liquid medium supplemented with lactate (10 mM) and bacterial biomass (1.10 g/L), was removed by the cells of D. äspöensis after 72 h of incubation at pH 5. Kinetic studies showed that the main amount of U (VI) was removed from the medium during the first 24 h. The microbial activity depended on pH, initial U (VI), and biomass concentration. By using X-ray absorption spectroscopy (XAS), we demonstrated that, in contrast to the above mentioned case with Cm (III), changes of the oxidation state of U (VI) in the precipitate formed by D. äspöensis occurred. The cellular localization of uranium removed from the medium was studied by using Transmission Electron Microscopy (TEM) and Electron-Disperse X-ray (EDX) analyses.

[1] Motamedi, M., Pedersen, K., Int. Syst. Bacteriol. 1998, 48, 311-315.

This work was funded by the BMWi under contract number: 02E9491.The authors are indebted for the use of the 248Cm to the U.S.. Department of Energy, Office of Basic Energy Sciences, through the transplutonium element production facilities at Oak Ridge National Laboratory which was made available as part of a collaboration between FZR and the Lawrence Berkeley National Laboratory (LBNL).

To protect the health of the population, knowledge is necessary about the transfer of radioactive heavy metals, like uranium, via the food chain soil-water-plant-animal-human. The overall process of uptake of heavy elements into plant tissues from contaminated soils is quantified using the soil-to-plant transfer factor (TF). The transfer factor of uranium for lupine and dandelion is in the range of 10-2 to 10-3. To obtain a more mechanistic understanding of the uptake of heavy metals in plants knowledge about the individual physical-chemical processes is needed. This study focuses on the determination of uranium speciation after uptake of uranium by plants (lupine, dandelions, lamb¢s lettuce). For the first time, laser-induced fluorescence spectroscopy and X-ray absorption spectroscopy were used to determine the chemical speciation of uranium in plants. Information on the spatial distribution of uranium in the plant was achieved by scanning electron microscopy, coupled with energy-dispersive X-ray microanalysis. Differences were detected between the uranium speciation in the initial solutions (hydrophonic and pore water of soil) and inside the plants. The oxidation state of uranium remained hexavalent after the uptake. The chemical speciation of uranium was identical in the roots, shoot axis, and leaves and was independent of the various investigated plants. First results are reported concerning the speciation of uranium in cell sap and solid cell components after separation. Spectroscopic data of relevant model compounds (e.g. sugar phosphates, inorganic phosphates, carboxylic acids, proteins) are compared with the uranium complexes in the different compartments of the plants.The results indicate that the uranium is predominantly bound to phosphoryl groups but in dependence on the experimental conditions the formation of uranium carboxylate complexes cannot be excluded.

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The sheet resistance and structural properties of high-fluence Si-implanted diamond were investigated. In order to minimize the radiation damage and to facilitate SiC formation the implantation was performed at 900 °C. All samples were subsequently annealed in an rf-heated furnace at 1500 °C for 10 minutes in order to remove defects and thermally unstable phases. X-ray diffraction, infrared absorption spectrometry and high-resolution cross-sectional transmission electron microscopy revealed the formation of a buried layer inside the implanted diamond, which contains SiC nanocrystallites. These SiC nanocrystals have a cubic structure and are nearly perfectly aligned with the diamond lattice. Raman spectroscopy was applied to analyze radiation-damage-induced graphitization in dependence on the implantation conditions. The sheet resistance of the samples was measured as function of temperature by four point probe technique in van-der-Pauw geometry. The decrease of the sheet resistance with increasing ion fluence unambiguously shows the influence of implantation-induced damage. The behavior of the sheet resistance can strongly be modified by additional nitrogen implantation The resulting higher conductivity is interpreted as partial incorporation of the nitrogen donor into the SiC nanocrystals. However, when the Si fluence exceeds a critical value of 5.3×1017 Si+cm-2 at 900 °C the diamond is irreversibly damaged and defect related conductivity dominates.

The mobility of actinides in the environment is determined by their speciation which is strongly influenced by their oxidation states. Humic acids (HA) influences the speciation of actinides by complexation. However, they have also significant redox properties which can affect the oxidation states of actinides and consequently their migration in the environment. Thus, it is very important to understand both the complexation and the redox properties of HA in natural systems.
In order to study the redox behavior of HA in more detail we synthesized HA model substances with distinct redox functionalities based on the oxidation of diphenolic compounds in the absence and presence of amino acids. These humic acid-like model substances are characterized by elemental compositions and structural elements that are comparable to natural HA. However, they show phenolic/acidic OH group contents that are higher than those of natural HA. For characterization of the redox properties of these synthetic products, their Fe(III) and ferricyanide redox capacities (RC) were determined at pH 3 and pH 9.2, respectively, and compared to that of purified natural HA from Aldrich. The synthetic products show RC that are up to a factor of 11 and 4 higher than that of Aldrich HA at pH 3 and pH 9.2, respectively. Additionally, we modified, i.e., etherified the phenolic OH groups of these HA by methylation with diazomethane. Applying these modified HA we verified the dominating role of phenolic OH groups in the redox behavior of these HA.
The synthesized HA model substances with distinct redox functionalities are applied to further improve the knowledge on the impact of HA on the redox stability of actinides in the environment. We study the redox stability of uranium(VI) complexes of these HA depending on pH. Uranium(IV) that is formed due to the redox process is spectroscopically determined both directly by laser-induced photoacoustic spectroscopy and indirectly in form of the uranium(IV) arsenazo(III) complex.

a-Si:H films prepared by plasma-enhanced CVD with 10% SiH4 in hydrogen have been studied concerning the effect of film thickness on the hydrogen concentration, interconnected void network and mechanical stress. The hydrogen concentration was determined by nuclear reaction analysis. The interconnected void network was studied by the method of ion exchange in glass substrate. The films were prepared at a substrate temperature in the range of 150 - 270°C. The results show that at the substrate temperature of 150°C the film structure develops as the void network decreases with the film thickness. At the substrate temperature of 270°C the film starts to grow with a dense structure and its structural improvement is manifested by the increase of the intrinsic compressive stress with the film thickness. The hydrogen concentration does not depend on the film thickness at any substrate temperature.

The interaction of the two chemical homologues (Cm (III) and Eu(III)) with calcium silicate hydrates (CSH phases) at pH 13.3 has been investigated in batch-type sorption studies using Eu(III) and complemented with time-resolved laser fluorescence spectroscopy (TRLFS) using Cm(III). The sorption data for Eu(III) reveal fast sorption kinetics and a strong uptake by CSH phases with distribution ratios of (6±3)·105 L kg-1. Three different Cm(III) species have been identified: A non-fluorescing species, which was identified as a curium hydroxide (surface) precipitate, and two fluorescing Cm(III)/CSH sorbed species. The fluorescing sorbed species have characteristic emission spectra with main peak maxima at 618.9 nm and 620.9 nm and fluorescence emission lifetimes of 289 ± 11 µs and 1482 ± 200 µs, respectively. From the fluorescence lifetimes it was calculated that the two fluorescing Cm(III) species have one to two and no water molecules left in their first coordination sphere suggesting that these species are incorporated into the CSH structure. A structural model for Cm(III) and Eu(III) incorporation into CSH phases is proposed based on the substitution for Ca at two different types of sites in the CSH structure.
Key words : curium, europium, CSH, sorption, incorporation, TRLFS

A nuclear resonance fluorescence experiment with two highly efficient EUROBALL Cluster detectors has been performed on the Gamma-soft nucleus 194Pt. Dipole excitations were observed between 2 and 4 MeV excitation energy. They are tentatively interpreted as the main fragments of the scissors mode based on the measurec excitation strengths and a comparison to microscopic calculations in the framework of the quasiparticle random phase approximation (QRPA). The data indicate large differences to the neighbouring isotope 196Pt: a doublingof the observed dipole strength and a shift of the energy centroid by about 600 keV. None of the currently available models is able to reproduce these features consistently in both nuclei.

An investigation in the field of the crack initiation determination for Charpy size specimens was carried out. An extensive literature survey of published methods for the crack initiation was performed. Methods based on the stretch zone width measurement, blunting line, multiple gauge measurement, electric potential drop, compliance changing rate, acoustic emission, ultrasonic method and magnetic emission are discussed in the theoretical part of the report. Analytical methods for the critical J-integral evaluation were also taken into account, as well as the expressions for the J-integral calculation. On the basis of the theoretical survey suitable measurement methods were chosen and applied in the experimental programme to several different materials. Namely blunting line related methods, multiple gauge methods, electric potential drop and compliance changing rate methods were used. The initiation J-integrals were evaluated with use of wide range of evaluation procedures and compared together in order to find a reliable method for the crack initiation determination. There was not found a universal method for the crack initiation determination. The performance of the methods was varying in dependence on the investigated material, so the results enable to choose perspective method for considered case.

Low energy X-rays (Eph < 50 keV) are widely used in diagnostic radiology and radiotherapy. However, data on their relative biological effectiveness (RBE) are scarce. Of particular importance for risk estimation are the RBE value of X-rays in the range which is commonly used in mammography (10 - 30 keV). In the present study we have determined clonogenic survival after low-energy X-ray irradiation for 3 cell lines: primary human epidermal keratinocytes (HEKn), mouse fibroblasts (NIH/3T3) and Chinese hamster fibroblasts (V79). Experiments were performed with a 25 kV X-ray tube and compared to 200 kV X-rays as a reference. Compared to the effect of 200 kV X-rays, irradiation with 25 kV X-rays resulted in a decreased survival rate in the murine fibroblasts but not the human epithelial cell line. RBE value was calculated for 10 % surviving fraction. For HEKn cells, RBE was 1.33 ± 0.27, for NIH/3T3 cells 1.25 ± 0.07 and for V79 cells 1.10 ± 0.09. In conclusion, no consistently increased RBE was observed in the various cell lines. Nevertheless, a potential of increased cytogenetic changes has to be considered for risk estimation of low-energy X-rays.

Intersubband transitions in InP-based (Ga,In)As/(Al,In)As MQWs cover the wavelength range beyond 3.5 micron. Application of enhanced conduction band edge discontinuity allows for a reduced intersubband transition wavelength. This can be accomplished by replacing (Al,In)As by Al(As,Sb) barriers that can be grown lattice-matched to InP. (Ga,In)As/Al(As,Sb) MQWs were deposited by MBE and characterised using a combination of x-ray diffraction, photoluminescence and IR absorption measurements. Influence of well thickness and doping behaviour were systematically investigated. By
comparison with simplified theoretical calculations, the electronic band structure (interband and intersubband system) was deduced. Based on the corresponding results, the potential of (Ga,In)As/Al(As,Sb) MQWs for implementation in quantum cascade lasers will be discussed.

Mixed Oxide (MOX) fuel is usually considered as a solid solution formed by uranium and plutonium dioxides. Nevertheless, some physico-chemical properties of (U_1-y, Pu_y)O₂ samples manufactured under industrial conditions showed anomalies in the domain of plutonium contents ranging between 3 and 15 at.%. Cerium is commonly used as an inactive analogue of plutonium in preliminary studies on MOX fuels. Extended X-ray Absorption Fine Structure (EXAFS) measurements performed at the European Synchrotron Radiation Facility (ESRF) at the cerium and uranium edges on (U_1-y, Ce_y)O₂ samples are presented and discussed. They confirmed on an atomic scale the formation of an ideal solid solution for cerium concentrations ranging between 0 and 50 at.%.

The spatial coherence of hard X-rays provided by a bending magnet of the storage ring BESSY II was investigated performing Young's interference experiment. The interference pattern was created by the diffraction of two 2 µm pinholes drilled into a thin tantalum foil by focused ion sputtering. Using an energy-dispersive detector with an energy resolution of 200 eV the interference pattern were detected simultaneously between 5 keV < E < 16 keV scanning a 5 µm pinhole through the detector window. The set-up is suitable to characterise the coherence properties of the beamline in a simple manner, i.e. to deduce parameters as the effective source size, the coherence length and the visibility. For the present case the visibility is near 100% at 5 keV and decreases to 20% at 16 keV.

The spatial coherence of hard X-rays provided by a bending magnet of the storage ring BESSY II was investigated performing Young's interference experiment. The interference pattern was created by the diffraction of two 2 µm pinholes drilled into a thin tantalum foil by focused ion sputtering. Using an energy-dispersive detector with an energy resolution of 200 eV the interference pattern were detected simultaneously between 5 keV < E < 16 keV scanning a 5 µm pinhole through the detector window. The set-up is suitable to characterise the coherence properties of the beamline in a simple manner, i.e. to deduce parameters as the effective source size, the coherence length and the visibility. For the present case the visibility is near 100% at 5 keV and decreases to 20% at 16 keV.

Extended X-ray absorption fine structure (EXAFS) spectroscopy at the uranium L_III-edge was used for determining the structural environment of aqueous uranyl surbed onto montmorillonite. The study reveals that uranyl uptake at pH~5-~7 and at an initial uranyl concentration of 5x10^-5M takes place at amphoteric surface hydroxyl sites as inner-sphere complex. The measured bond distances sites between uranium and the equatorial oxygen atoms are in the range of 2.34 A the presence of a U-Al backscattering pair was determined. This backscattering pair indicates that the binding of the uranyl unit to amphoteric surface hydroxyl sites occurs preferred as a bidentate inner-sphere complex on aluminol groups.

Die nichtlineare Optik im THz Frequenzbereich ist weitgehend unerforscht [1], da hier keine abstimmbaren, intensiven Lichtquellen zur Verfügung stehen. Abstimmbare Freie-Elektronen Laser mit Emissionsfrequenzen im THz Bereich schließen diese Lücke. Wir haben Frequenzverdoppelung unterhalb der optischen Phononresonanz an dünnen GaAs Kristallen mit dem Freie-Elektronen Laser FELIX, Niederlande, durchfgeführt. Erstmals beobachten wir ein Maximum der nichtlinearen Suszeptibilität 2.Ordnung bei der halben Phononfrequenz (4,4 THz) und ein Minimum oberhalb dieser Frequenz (5,3 THz). Dieses Minimum basiert auf einem Vorzeichenwechsel der nichtlinearen Suszeptibilität bedingt durch konkurrierende elektronische und Gitterbeiträge. Ein Vergleich mit Berechnungen [2] zeigt, dass aus der Frequenz dieses Minimums die Beiträge höherer Ordnung des Gitterpotentials zur nichtlinearen Suszeptibilität quantitativ bestimmt werden können [3].

[1] siehe z. B. F. Keilmann, Infr. Phys. 31, 373 (1991).
[2] C. Flytzanis, Phys. Rev. B 6, 1264 (1972).
[3] T. Dekorsy et al. akzepziert zu Phys. Rev. Lett.

An overview of the research activities of the FIB group in the Research Centre
Rossendorf is given. More in detail the fabrication technology of alloy LMIS as well
as their characterization is discussed. The FIB system IMSA-100 is briefly
introduced and typical applications are presented: writing implantation of Co ions
into a heated Si target in order to create maskless sub-micron CoSi2 structures,
bombardment of semiconductor materials with different ions in a wide range of
current density, dose and temperature allows to study the damage creation and
dynamic annealing process.

Erbium silicide layers were grown epitaxially on Ge+ ion implanted Si. Epitaxy of ErSi2-x layers was achieved at temperature of 750 C.The layers are grown in the tetragonal phase.The growth of the silicide layers resulted in a drastic decrease of the dislocations in the SiGe layer accompanied by the accumulation of defects at the SiGe/ErSi2-x interface.A small redistribution of the Ge in the SiGe layer was also observed.

Solidified liquid metal ion sources (LMISs) operating with Au alloy wetted hair-pin emitters can be used as high-intensity electron point sources with nanometer dimension for electron field emission application. A nanoemitter tip on a solidified LMIS emitter can be formed by quenching during ion emission mode. I-V characteristics and the performance of the electron emitting LMIS are presented.

The study of trace-elements in archaeological metallic objects can provide important clues about the metal provenance and the involved manufacturing procedures, leading to important conclusions regarding the commercial, cultural and religious exchanges between the antique populations.
Ancient metallic materials are usually inhomogeneous on a scale of 20 microns or less: they contain remains of imperfect smelting, segregated phases in alloys, inclusions.
Due to their exceptional chemical stability, gold artefacts remain essentially unchanged during weathering and aging processes.
Several fragments of ancient gold objects coming from an Eneolithical treasury and from Pietroasa "Closca cu Puii Aur" ("The Golden Brood Hen with ITS Chickens") hoard, unearthed on Romanian territory and two Romanian native gold nuggets samples were analysed using micro-PIXE technique at the Rossendorf TANDETRON microbeam facility.
The purpose of the study was to clarify the metal provenance, establishing if the hypothesis of local gold holds. To reach this goal, trace elements (Cu, Te, Sn, Pb, Hg, As, Zr, Sb) and PEG (Platinum Group Elements) concentrations were determined.
The presence of inclusions (micrometeric size areas of compositions different from surroundings) was also checked. We found some Si, Ca, Fe ones on two Eneolithic samples, and a Ta-Cr one on sample from Pietroasa hoard. The measurements led to conclusions regarding the alluvial origin of the gold for the Eneolithical samples and gave some indications for the possible gold ore sources of Pietroasa treasury, confirming the heterogeneity of this treasury (the two analysed pieces belonged to different stylistic and compositional groups).
21 pieces of gold coins of KOSON type, considered the only kind of gold coins issued by the Daciens, were analysed using EDXRF and PAA (Proton Activation Analysis) methods at Bucharest Institute of Atomic Physics facilities. For EDXRF, three annular excitations sources - Pu 238 (30 mCi), Am 241 (50 mCi) and Am 241 (10 mCi, with nickel window for asorption of soft X-rays) and two X-ray detectors with Be window - a Si(Li) and an HPGe were used. For PAA, each coin was irradiated in vacuum for 5 hours at an incident proton energy of 11 MeV at a current of ca. 50 nA at the 8 MV FN High Voltage Bucharest Tandem and measured using a properly protected Ge(Li) gamma spectrometer. Three groups of coins of different compositions were found, corresponding to simple, complex and no monogram pieces. The gold of Koson coins is not a natural one (electrum) from present Romania's territory, but is similar to the gold of pseudo - Lysimachan staters. Some possible historical conclusions are discussed.

It is already known that the microstructure of a metallic alloy can be affected in a significant way due to the convection in the liquid phase during solidification. A time varying magnetic field can be applied to produce a flow field in the melt which influences the nucleation and growth processes. The aim of our research program is to find a strategy to refine the microstructure of castings by an optimal combination of magnetic field intensity, field frequency and cooling rate. Furthermore, the basic mechanisms controlling the solidification by magnetic fields are investigated.
A cylindrical crucible with a diameter of 50 mm was used to contain the Pb85wt%Sn alloy. A melt height of 60 mm was chosen. The container bottom is positioned on a water cooled copper chill allowing a directed solidification by a vertical heat flux. A rotating magnetic field was generated by an inductor system with 6 coils.
Local temperatures were determined during the solidification process using a set of thermocouples. Cooling curves measured at different locations inside the sample reveal the significant influence of the electromagnetic convection on the local heat transfer. Profiles of the melt velocity were obtained applying the ultrasonic Doppler method..
The Pb-85wt%Sn alloy shows a microstructure with primary tin-crystallites and eutectic. Specimens solidified without a rotating magnetic field showed a columnar dendritic microstructure which is orientated in heat flux direction. The tin crystallites and the eutectic are homogeneously distributed over the whole sample. If the alloy solidifies in a rotating magnetic field the microstructure changes. The shape of the dendrites changes from columnar to equiaxed in direction from the bottom to the top of the specimen and in the same direction the volume content of the eutectic increases.

By low dose ion implantation the magnetoresistance of LSMO is enhanced and the temperature of its maximum is shifted to lower values. At implantation of higher doses the LSMO films become semiconducting.

In the metastable solid solution Fe-15at.%Cr short range ordering (decomposition) was caused by irradiation at 723 K using Ar and Fe ions. The short range order parameter was evaluated from Moessbauer spectra. The short range order caused by the irradiation is much higher compared to the effect of only annealing at723 K for the same time without irradiation. The decomposition is not limited to the penetration depth of the ions but extends over the whole sample thickness of 30 µm. Therefore it is explained as due to radiation dynamic long range effects.

The complex formation of uranium(VI) with alpha-D-glucose 1-phosphate (C₆H₁₁O₆PO₃ ^2-, G1P) was determined by time-resolved laser-induced fluorescence spectroscopy (TRLFS) at pH 4 and potentiometric titration in the pH range from 3 to 10. Both measurements show the formation of a 1:1 complex at lower pH values. The formation constant of UO₂(C₆H₁₁O₆PO₃) was calculated from TRLFS measurements to be log beta₁₁ = 5.72 ± 0.12, and from potentiometric titration log beta₁₁ = 5.40 ± 0.25, respectively.
It was found by potentiometric titration that at higher pH values the complexation changes to a 1:2 complex. The stability constant for this complex was calculated to be log beta₁₂ = 8.96 ± 0.18.

The overall objective of the EC project "Humic Substances in Performance Assessment of Nuclear Waste Disposal: Actinide and Iodine Migration in the Far-Field" is the determination of the effect of humic substances on the actinide migration in natural systems to assess their impact on the long-term safety of radioactive waste repository sites and abandoned uranium mines. This task includes also the implementation of the present knowledge to real existing natural systems thereby verifying the correlation between important parameters, evaluating their environmental impact and finally, uncovering issues not addressed so far.
Uranium mining waste rock piles in the southern parts of the former East Germany represent a significant long-term environmental concern and liability. Although the uranium mines were decommissioned with the end of the uranium ore production in 1990, the legacy of forty-five years of uranium mining, such as abandoned mines, huge waste rock piles and mill tailings, represents a permanent reservoir and source of radioactive and non-radioactive contaminants. The discharge of radionuclides from the waste rock piles and contamination of the surrounding geosphere has to be minimized.
For the case study presented in this paper, the uranium mining waste rock pile no. 250 in Schlema/Alberoda (Saxony, Germany) was chosen. In many respects, this pile resembles other rock piles of this region. The site is characterized comprehensively with regard to composition and activity inventory of rock material and seepage water, uranium species occurring in the seepage water, TOC content and much more. Some important data of other uranium mining waste rock piles that were located in the vicinity of the rock pile no. 250 are also included in this study, especially the fulvic and humic acid content in the seepage water of rock piles and their loading with uranium. The data presented in this natural system study constitute the basis of performance assessment modeling.

Range distributions of carbon ions deposited onto tetrahedral amorphous carbon films at kinetic energies between 22 eV and 692 eV are measured utilizing high-resolution elastic recoil detection. These data are compared to range calculations based on binary collision approximation as well as to classical molecular dynamics simulations. Asymmetric range profiles, differences in mean ion ranges and increased range straggling compared to theories are attributed due to self diffusion during thermal spike as well as to intrinsic surface properties of the carbon samples which have to be considered in subplantation growth models.

The third report from the Project-Group ESRF-Beamline of the Forschungszentrum Rossendorf covers the period from January 2001 until December 2002. The Rossendorf BeamLine (ROBL) at the European Synchrotron Radiation Facility (ESRF) in Grenoble performed again well during this time - although we had major staff fluctuations, including two times a change in the project-management: Dr. W. Matz became head of the Technical Infrastructure at FZR, and Dr. T. Reich had been offered a professorship at the University of Mainz. We congratulate both of them. In the beamtime used by the FZR and collaborating institutes 77 different experiments were scheduled, while in the ESRF scheduled beamtime 21 experiments were performed by external groups. Additionally, a distinct amount of beamtime was devoted to commissioning of new equipment.

The report is organised in three main parts. The first part contains extendet contributions on results obtaines at ROBL. The second part gives an overview about the general experimental possibilities, scheduled experiments, publications, guests having visited ROBL with support of the EC, an staff information. Finally, the third part collects the experimental reports of the user groups received.

For the materials research experimental station of the Rossendorf beamline ROBL at the European Synchrotron Radiation Facility in Grenoble, France, a two magnetron sputter deposition chamber for in situ study of film growth by synchrotron X-ray diffraction and reflectivity was developed. It allows high-quality depositions of compound films and multilayers. Heteroepitaxial layer-by-layer growth of TiN on single crystal MgO(0 0 1) was observed by real-time specular X-ray reflectivity showing characteristic oscillations. The pseudomorphic growth was confirmed by high-resolution TEM micrographs. During growth on amorphous SiO2 on Si(0 0 1) substrates, the microstructural development of TiN films was studied in situ as a function of film thickness. With the deposition parameters chosen, a crossover was observed: grains with a (0 0 2) plane parallel to the film surface dominate at small thicknesses, while, at larger thicknesses, (1 1 1) grains dominate. Recrystallisation was identified as a mechanism that controls this texture development.

InGaAs/AlAs quantum wells (QWs) have the potential for the development of new devices based on intersubband transitions, such as near-infrared detectors, ultra-fast switches and light emitters that operate at the communication wavelength of 1.55 mm.However, the increased strain accommodation in the InGaAs/AlAs system considerably affects the band offsets of these QW structures and the performance of the appropriate devices. We report structural and optical characterization of InxGa1-xAs/AlAs/InyAl1-yAs (x ~ 0.7, y ~ 0.55) QW structures grown on InP substrates. In these structures, we utilize the high conduction band offset provided by AlAs. An increased In content in the wells and in the InyAl1-yAs layers helps to compensate the large AlAs tensile strain. Additionally, the smaller InGaAs band gap results in a shift of the first G-like well subband to lower energies relative to the X-minimum in the barrier layers even in very narrow wells. Intersubband absorption at wavelengths shorter than 2.0 mm is observed in thin single QWs. Also presented are spectra of asymmetric coupled QWs and short-period superlattices.

The surface hardness of the technically important alloy Ti–6Al–4V (wt.%) can be improved by nitrogen implantation. The structural mechanisms of hardening and of the stability of the improved hardness at elevated temperatures are studied. Ion implanted (II) and plasma immersion ion implanted (PII) samples were used. The formation of small TiN crystallites was detected in the as-implanted state, but only for the II samples a considerable surface hardness increase (factor 3) is observed. The in situ XRD experiments showed, that the TiN phase is stable up to temperatures of 650 °C for both types of implantation. At higher temperature Ti2N is formed which is stable up to 770 °C. ERDA results indicate a diffusion of nitrogen into the bulk material. The redistribution of N is responsible for the hardness changes: a slight decrease for II samples but an improvement by a factor of 2.5 for PII samples. The improvements/degradations of hardness and wear are discussed in correlation with the nitrogen depth distribution below the surface.

Au-ions were implanted into TiO2 single crystals with doses ranging from 2x1016Au+/cm2 to 6x1016Au+/cm2 at RT and 1000 K. At RT implanted samples were then thermally annealed at temperatures of 550 K to 1550 K. The Au-atoms precipitate to nanocrystals already during implantation at RT with an average particle size of 1.5 nm. HRTEM investigations revealed that the Au-nanocrystals, embedded in amorphous TiO2 regions, have a broad size and range distribution varying from large sizes in the near surface region to smaller sizes at larger depths. In the annealing process a reorientation of the Au-nanocrystals is observed, with the main effect of a decrease of the (111) peak and an increase of the (200)-peak in the XRD spectra. After annealing at 1000 K the particle size of the highly textured Au-implant was evaluated to ~ 6 nm; this means that during annealing the particles grow, leading to a partially coherent orientation in the disordered TiO2-matrix. Au implantation at RT performed through a metal mask with holes resulted in a narrow size distribution (2-6 nm) of the Au-nanocrystals in the near surface region.

The strong gettering of Cu atoms in single-crystal Si implanted with 3.5 MeV P+ ions was studied after thermal treatment and contamination with low amount of Cu impurity. Cu decorates the remaining damage generated by ion implantation. Three separate Cu gettering layers were detected by secondary ion mass spectrometry: at the main projected ion range, RP, below RP (RP/2 effect) and beyond RP (trans-RP effect). The defects acting as gettering centers at RP/2 and RP are implantation induced excess vacancies and excess interstitials, respectively. Cu profiles fit very well with depth distributions of excess vacancies and excess interstitials simulated by binary collision model for random and channeled ion incidence. The RP/2 and RP gettering layer are implantation induced, whereas the trans-RP gettering layer is formed by thermal treatment. The Cu accumulation in the trans-RP region increases with increasing temperature and/or with increasing annealing time. The RP/2 effect for P+ implantation was found to be significantly reduced in comparison with Si+ implantation. It completely disappears for higher P+ ion fluences. The obtained results are in agreement with the assumption that interstitials carried by P diffusion are the origin of Cu gettering in the trans-RP region.

The formation and evolution of radiation damage by ion bombardment consists of three stages: (i) atomic displacements during ballistic processes, (ii) formation of a (meta)stable defect structure after fast relaxation, and (iii) long-term thermally activated defect rearrangement, migration, recombination and reduction. The first two stages occur on very short time scales and are hardly accessible by available experimental methods. Atomistic computer simulations can contribute to a better understanding of these processes and of their microscopic mechanisms.
In this talk, a combined simulation method is employed to study a relatively simple case, the defect production by a single ion impact in silicon. Processes in the collision cascade with energy transfers above about 100 eV are treated by computer simulations based on the binary collision approximation (BCA). Classical molecular dynamics (MD) calculations are applied to consider processes in certain parts of the cascade which start with energy transfers less than about 100 eV. Detailed investigations are performed to study the temporal evolution of the defect structure until the beginning of the thermally activated phase, and to determine the damage morphology obtained after the fast relaxation. The influence of nuclear energy deposition and target temperature is discussed. The combination of BCA and MD methods allows the effective calculation of the total number and the depth distribution of different defect species (isolated vacancies and self-intersitials as well as more complex defects) formed on average per incident ion after the fast relaxation processes are finished. The procedure yields more realistic initial conditions for the simulation of post-implantation annealing than hitherto used.

In der Feinchemie- und Pharmaindustrie werden Chemikalien kleinerer Menge meistens durch diskontinuierlich geführte Batch-Prozesse hergestellt. Zur Unterstützung des Bedienungspersonals bei der schwierigen Prozessführung von Batch-Reaktoren (Rührkesselreaktoren) wurde ein Online-Monitoring-System (MoSys) entwickelt, das auf adaptiven Stoff- und Wärmebilanzen basiert. Die Industrieerprobung erfolgte im Rahmen eines entwickelten Batch-Informations-Management-Systems (BIMS), das in einem separaten Industrie-PC implementiert und über den Terminalbus in die vorhandene Automatisierungstechnik einer Mehrzweckanlage der Degussa AG eingebunden wurde. Die Betriebserfahrungen von zwei Produktionskampagnen zeigten, dass das BIMS/MoSys stabil und zuverlässig arbeitete und die Konzentrationsprofile gut mit den erwarteten Konzentrationsverläufen übereinstimmten.

Mit BIMS/MoSys sind folgende praktische Nutzanwendungen möglich:

• Einsparung einer chemischen Online-Prozessanalytik,
• Erweiterung und Archivierung des bestehenden Prozesswissens,
• Verbesserung der Produktqualität bei komplexen Batch-Prozessen,
• Optimierung der Prozessführung durch die genauere Ermittlung von Anlagen- und Prozess- Kenngrößen,
• Fehler- und Ursachenanalyse anhand der archivierten Batches,
• Rückverfolgbarkeit von Batches bei Problemen (z. B. Qualitätsbeanstandungen),
• Aufbau eines automatisierten Batch-Reports.

Darüber hinaus können unerwünschte Betriebszustände mit erhöhter Zwischenproduktakkumulation und verringerter Raum-Zeit-Ausbeute frühzeitig erkannt und dadurch rechtzeitig Gegenmaßnahmen eingeleitet werden, um größere Verluste zu vermeiden. Das auf adaptiven Stoff- und Wärmebilanzen basierende Online-Monitoring-System ist bei allen ausreichend exothermen ( oder endothermen) Semibatch-Prozessen einsetzbar, wenn geeignete Informationen in den Stoff- und Wärmebilanzen enthalten sind.

The FZR/IRC contributions are focussing on the interactions of actinides with indigenous bacteria in Äspö aquifer. We presenting the first results on interactions of the sulfate-reducing bacterium D. äspöensis (DSM 10631T) with uranium(VI). 80 % of the U(VI), solved initially in a concentration of 0.02 mM in a liquid medium supplemented with lactat (10 mM), was removed by the cells of this strain after 72 h of incubation at pH 5.

wird nachgereicht

Summary of the scientific activities of the institute in 2002 including selected highlight reports, short research contributions and an extended statistics overview.

wird nachgereicht

The grain and defect structure of submicrocrystalline and nanocrystalline nickel produced by equichannel angular pressing or by ball milling, respectively, has been studied by isochronal and isothermal annealing experiments, and Xray investigations. A detailed analysis of the thermal stability of the di.erent types of microstructures will be presented.

Bragg diffraction profiles were measured on single grains of different axial orientation in cyclically deformed Ni polycrystals. Diffraction profile parameters were determined and compared with results from profile measurements on fatigued single crystals, showing the same type of dislocation structure as the grains with corresponding axial orientation. Conclusions are drawn concerning the deformation processes in the grains taking into account the activated slip systems, the dislocation density and long-range residual strains.

Strong blue and violet photoluminescence (PL) and electroluminescence (EL) at room temperature has been achieved from thin SiO2 layers implanted with group IV elements. Thermally grown SiO2 .lms with thicknesses between 130 and 500 nm were implanted with Si, Ge or Sn ions followed by di.erent annealing procedures. Based on PL and PL excitation spectra we tentatively interpret the blue–violet PL as due to a T1- S0 transition of an oxygen deficiency center. The strong EL is well visible with the naked eye and reaches a power e.ciency of up to 5E-3 for Ge. Whereas the EL intensity shows a linear dependence on the injection current for Ge-rich layers, the shape of the EL spectrum remains unchanged. It was found that the I–V characteristics shift to lower applied electric fields with increasing implantation
fuence. Furthermore, it is assumed that the luminescence centers will be excited either by field ionization or by the scattering of hot electrons. Finally, the suitability of ion implanted silicon dioxide layers for optoelectronic applications is discussed.

Silicidation processes in nanoscale Ni and CoNi (5at.% Ni) layers on different silicon substrates were investigated using X-ray diffraction. The phase formation sequences as well as the formation and transition temperatures between 200 and 750°C were studied. The impact of different silicon substrates, i.e., polycrystalline Si and (100) oriented Si single-crystal substrates as well as the impact of different species of dopants (As, P) were analysed. The thermal range of the desired low resistance target phases NiSi and Co(0.95)Ni(0.05)Si(2) was determined. The temperatures for phase formation and phase transitions are significantly lowered on polycrystalline Silicon substrates.

Plasma immersion ion implantation of nitrogen in Si: Formation of SiO2,
Si3N4 and stressed layers under thermal and sputtering effects

Sponge-like and columnar porous silicon implanted with nitrogen by plasma immersion ion implantation (PIII)

Uranium mining waste piles are an enormous pool for heavy metal resistant bacteria. Many of these bacteria possess different mechanisms to detoxify metals, e.g. bioaccumulation, biotransformation, biomineralization or biosorption. The latter is of special interest for the development of bioremediation processes. We demonstrated that vegetative cells, spores and purified S-layer of Bacillus sphaericus JG-A12 which was recovered from a uranium mining waste pile near the town of Johanngeorgenstadt, Germany, bind selectively U, Cu, Pb, Al and Cd. In this work sol-gel techniques were used to immobilize cells, spores and stabilized S-layer of B. sphaericus JG-A12 in a porous silicate matrix. Processes of sorption and desorption of U and Cu by the produced biological ceramics (biocers) were investigated and compared with the binding properties of the single components. Localization of the bound metals was carried out using scanning electron microscopy and EDX analysis. Formed metal complexes were characterized by extended X-ray absorption fine structure spectroscopy (EXAFS). Our results demonstrate that spores followed by vegetative cells and the S-layer bind large amounts of U and Cu. The silicate matrix binds only small amounts of U and no Cu. The immobilization of the biocomponents in the bioceramics did not have any negative effect on the cells and S-layer but the metal binding capacity of the spores was strongly reduced. Binding capacity and binding kinetics of the biocers were positively influenced by adding water soluble additives as sorbitol or by freeze drying instead of air drying. The bound metals can be completely removed from the biocers by using aqueous citric acid what makes them reusable. EXAFS spectroscopy of the uranium complexes shows that uranium is bound via phosphate and carboxyl groups of the biocomponents as well as by the silicate and hydroxyl groups of the ceramic matrix. Because biocers possess high mechanical stability and metal binding capacity and are in addition reusable they are suitable for construction of intelligent filters for bioremediation.

The embrittlement of reactor pressure vessel steels is mainly effected by the neutron field. However, recently results have pointed out an additional or coupled effect of hydrogen. The aim was to investigate the influence of hydrogen on mechanical behaviour of different unirradiated reactor pressure vessel steels up to the working temperature in dependence on cathodic hydrogen charging conditions in correlation to chemical composition, microstructure, and hydrogen diffusivity and solubility. Diffusivity and solubility of hydrogen were determined by means of permeation measurements, thermodesorption measurements, and hot extraction. Small differences are mainly caused by the chemical composition of the steels. Higher copper and phosphorus contents do not yield an expected higher hydrogen uptake of the unirradiated steels. The mechanical properties were determined by slow tensile tests up to 250°C with simultaneously hydrogen charging in simulated reactor pressure water dependent on strain rate and charging conditions, and by impact tensile tests. The results of the mechanical tests and the corresponding fractographic analysis showed hardly an effect of hydrogen and no significant differences of the steels under the applied charging conditions. The loss of ductility decreases with increasing strain rate and increasing temperature. These results are the staring point for further investigations on irradiated samples.

Stationary and transient core calculations for a hypothetical boron dilution event have been carried out by the nodal code DYN3D. Two different two-group diffusion-parameter libraries, generated by the cell codes HELIOS and CASMO, have been used, in order to assess the influence of these data. Realistic core inlet boundary conditions have been applied using a validated semi-analytical coolant mixing model. The initial deborated-coolant-slug volumes, necessary for reaching recriticality in stationary calculations with both data libraries, differ by some 20 %. Differences are also observed in the height and time point of the power peak in transient calculations. The deviations between the applied data libraries are mainly due to different SCRAM reactivities and Doppler coefficients. Even when assuming a 36 m3 deborated slug, the core is brought back to subcriticality in all calculations.

AlN nanocrystalline layers and superstructures are used in the modern optoelectronic technology as reflecting mirrors in semiconductor lasers. In the present work the properties of AlN films prepared by sputtering methods from an AlN target in reactive Ar + N plasma were investigated. The characterisation was performed with HRTEM, SEM, glancing angle XRD and RBS methods. The present measurements confirmed the polycrystalline structure of AlN layers and enabled the evaluation of their grain size. The roughness and thickness of the layers were additionally determined by ellipsometric and profilometric measurements.

The structure and the elemental depth distributions of Y1Ba2Cu3O7-d (YBCO) and La0.7Sr0.3MnO3 (LSMO) were examined by q-2q XRD, and by 1.7 MeV 4He+ Rutherford Backscattering Spectrometry (RBS) in random and channeling geometry. The YBCO layers were magnetron sputtered, where the only one varying parameters were the oxygen pressure and the annealing time. The layers have high crystalline qualitiy and an almost sharp interface with the substrate as revealed by the analysis. It is shown that the oxygen content influences considerably not only the superconducting behavior, but also the lattice parameters and the cmin parameter (the minimum yield which is the ratio of aligned to random Rutherford backscattering spectra). We have found by high-precision RBS simulation, that independent on the film quality, a disordered interface region of 20 to 30 nm is present in all structures. As a complementary study we have performed also AES depth profiling.

We report here on ferromagnetic/superconductor FM/SC and SC/FM double layers deposited without a buffer layer between FM and SC. Thin films of La0.7Sr0.3MnO3 (LSMO) are used for the FM, and YBa2Cu3O7-x (YBCO) for the SC. Both films can grow crystalline on SrTiO3 (STO) or LaAlO3 (LAO) substrates in high temperature and in oxygen atmosphere conditions. Magnetic and transport measurements and X-ray diffraction analysis are used to characterise film quality and properties. It is shown that off-axis magnetron sputtering can be used for high-quality double layer deposition. A prerequisite for this is the suppression of the interdiffusion process. This is achieved by lowering the deposition temperature and shortening the deposition time for the top layer. Lattice relaxation for LSMO films deposited on LAO substrates is seen. It is demonstrated that post-deposition annealing or additional top layer deposition enlarges the relaxed part of the lower LSMO film. LSMO films are smooth and free of imperfections and the stress is partly relieved by the formation of misfit dislocations. For YBCO films, SEM, XRD, EDX and magnetisation characterisations show that film lattice relaxation starts when single-element-oxide crystals start to grow into the film. Many experiments give evidence of a critical thickness of about 30 nm of a strained layer, after which the top part of the YBCO film relaxes. Despite the small compositional deviation due to the interdiffusion, the YBCO/LSMO double films demonstrate high enough transport and magnetic properties to allow their application in the investigation of the injection of spin-polarised quasiparticles from FM to SC film. The critical current for YBCO film is Jc~0.7×106 A/cm2 if it is a bottom layer, and Jc~1.7×106 A/cm2 if YBCO is a top layer, whilst our optimal single-layer YBCO films have Jc~(2.5¯5)×106 A/cm2 at 77 K.

The OECD/NRC BWR Turbine Trip Benchmark was analysed by the codes DYN3D and the coupled code system ATHLET/DYN3D. Considering the calculations with given thermal-hydraulic boundary conditions of the core for the Exercise 2 of the benchmark the analyses were performed with the core model DYN3D. Concerning the modelling of the BWR core in the DYN3D code several simplifications and their influence on the results were investigated. The standard calculations with DYN3D were performed with 764 coolant channels (1 channel per fuel assembly), the assembly discontinuity factors (ADF) and the phase slip model of MOLOCHNIKOV. Comparisons were performed with the results obtained by calculations with 33 thermal-hydraulic channels, without the ADF and with the slip model of ZUBER-FINDLAY. It is shown that the influence on core-averaged values of the steady state and the transient is small. Considering local parameters the influence of the ADF or the reduced number of coolant channels is not negligible. For the calculations of Exercise 3 the DYN3D-model validated during the Exercise 2 calculations in combination with the ATHLET system model, developed at GRS for Exercise 1 has been used. Calculations were performed for the basic scenario as well as for all specified extreme versions. They were carried out using a modified version of the external coupling of the codes, the ?parallel? coupling. This coupling shows a stable performance at the low time step sizes, which are necessary for an appropriate description of the feedback during the transient. The influence of assumed failures of different relevant safety systems on the plant and the core behaviour was investigated in the calculations of the extreme scenarios. The calculations of Exercise 2 and 3 contribute to the validation of DYN3D and ATHLET/DYN3D for boiling water reactor systems.

With only a few exceptions, the numerical simulation of cosmic and laboratory hydromagnetic dynamos has been carried out in the framework of the differential equation method. However, the integral equation method is known to provide robust and accurate tools for the numerical solution of many problems in other fields of physics. The paper is intended to facilitate the use of integral equation solvers in dynamo theory. In concrete, the integral equation method is employed to solve the eigenvalue problem for a hydromagnetic dynamo model with a spherically symmetric, isotropic helical turbulence parameter alpha. Three examples of the function alpha(r) with steady and oscillatory solutions are considered. A convergence rate proportional to the inverse squared of the number of grid points is achieved. Based on this method, a convergence accelerating strategy is developed and the convergence rate is improved remarkably. Typically, quite accurate results can be obtained with a few tens of grid points.

At present, the GDT facility of the Budker Institute for Nuclear Physics Novosibirsk is being upgraded. The first stage of the upgrade is the Synthesised Hot Ion Plasmoid (SHIP) experiment. It aims, on the one hand, at the investigation of plasmas the parameters of which are expected to appear in the region of high neutron production in a GDT based fusion neutron source as proposed by the Budker Institute and, on the other hand, at the investigation of plasmas the parameters of which have never been achieved before in magnetic mirrors. The expected record values of plasma parameters and several peculiarities of the plasma offer a great field
for interesting investigations. In order to simulate the particle fields inside the GDT device and later in a GDT based neutron source an Integrated Transport Code System (ITCS) is being developed in collaboration between Forschungszentrum Rossendorf and Budker Institute. It consists of modules which allow the calculations of neutral gas, background plasma and of the fast ion component considering their mutual interactions. This contribution explains the concept of the SHIP experiment and presents the
results of first calculations by means of the ITCS modules.

A miniaturised ion selective electrode (ISE) for Cu2+ ions was developed, specially designed for application in a microfluidic system. The electrode was prepared on a silicon wafer substrate coated with a Cu deposit in the thickness range of 50 - 200 nm. The Cu layer was quantitatively converted into CuS by treatment in a sulphidic ambient. The chip electrode has a size of 5x5 mm2 and was mounted on a spacer chip coupled to the fluidic microcell using a chip clip technology. The coupling is liquid proof and reversible, permitting an easy exchange of the chip electrodes. The effective electrode area contacting the liquid of the microsystem flow channel amounts to about 4 mm2.

Sensitivity measurements were performed stationary and in the flow through cell. There was found a good Nernstian response of 29 mV/pCu between pCu 5 and 1 agreeing very well with reference measurements carried out with a commercial ISE.

The rapid response observed even in the dilutest solutions used, is related to the thin, non-porous structure of the CuS layer, minimizing diffusion effects during changing the test solutions. The adhesion of the sensitive CuS layer is different for the substrates Si, SiO2 and Si3N4 and depends on their history, roughness and evaporation conditions.

The first application of a Sonogashira cross-coupling reaction in ¹⁸F chemistry has been developed. The reaction was exemplified by the cross-coupling of terminal alkynes (ethynylcyclopentyl carbinol 6, 17alpha-ethynyl-3,17beta-estradiol 7 and 17alpha-ethynyl-3-methoxy-3,17beta-estradiol 8) with 4-[¹⁸F]fluoroiodobenzene. 4,4'-Diiododiaryliodonium salts were used as precursors for the synthesis of 4-[¹⁸F]fluoroiodobenzene, enabling the convenient access to 4-[¹⁸F]fluoroiodobenzene in 13-70 % yield using conventional heating or microwave activation. The Sonogashira cross-coupling of 4-[¹⁸F]fluoroiodobenzene with terminal alkynes gave the corresponding 4-[¹⁸F]fluorophenylethynyl-substituted compounds [¹⁸F]-9, [¹⁸F]-10 and [¹⁸F]-13 in yields up to 88% within 20 min starting from 4-[¹⁸F]fluoroiodobenzene.

The ¹⁸F-labelled amino acid derivative 3-O-methyl-6-[¹⁸F]fluoro-L-DOPA ([¹⁸F]OMFD) is a potential radiotracer to image tumour tissue using positron emission tomography. The precursor N-formyl-3-O-methyl-4-O-boc-6-trimethyl-stannyl-L-DOPA--ethyl ester enables the direct electrophilic radiofluorination by stereoselective destannylation. After partial hydrolysis, an optimized HPLC purification and sterile filtration the [¹⁸F]OMFD obtained with high radiochemical purity is ready for use. The total synthesis time is about 50 minutes and the radiochemical yield achieved is 20-25% (decay corrected, related to [¹⁸F]F₂). It was demonstrated that [¹⁸F]OMFD can be produced routinely and reliably for clinical use. [¹⁸F]FDOPA - preparation devices can be used with minor modifications.

On the basis of methods developed recently for square-fuel-assembly reactor cores, discontinuity factors for hexagonal VVER (Russian PWR) control absorbers and reflector nodes have been derived. Partial currents from heterogeneous multi-group transport calculations are used for the determination of the discontinuity factors. As shown by suitable benchmark calculations, the application of these quantities in the two-group nodal diffusion code DYN3D clearly improves the results of assembly-power predictions. The advantage of reflector diffusion parameters, including discontinuity factors, over conventional albedos has also been demonstrated.

In order to improve the knowledge about the interaction processes between humic acids (HA) and metal ions, e.g., actinide ions, various HA model substances with different functional properties were developed at FZR-IfR. These include synthetic HA with different functional group contents and various structural elements, chemically modified HA with blocked phenolic OH groups as well as 14C-labeled HA. Since start of the project, synthetic HA with distinct redox functionalities are developed.
The report gives an overview about the synthesis, characterization and application of HA with various functional properties. It describes the synthesis and characterization of the melanoidin-based HA type M1 and M42, which are characterized by different carboxyl group contents. In addition, the synthesis and characterization of modified HA with blocked phenolic OH groups as well as of HA with distinct redox functionalities are discussed.

Die Flüchtigkeit von Oxiden der leichten Actiniden Th, Pa, U, Np und Pu im System O₂-H₂O_(g)/SiO_2(s) wurde mittels Thermochromatographie im Temperaturbereich 300 - 1475 K untersucht. Th und Pa bilden unter den experimentellen Bedingungen keine flüchtigen Verbindungen. Bei Temperaturen > 1250 K bilden U, Np und Pu flüchtige Oxidhydroxide, deren Flüchtigkeit in der Reihenfolge Pu<Np<U zunimmt. Die Flüchtigkeit des Plutoniums belegt die Oxidation von Plutoniumdioxid durch Sauerstoff/Wasser zum Trioxid.

A crosslinked polyurethanurea (PUU) coating was synthesised from a solution on metal vascular stents. In the model system the glucocorticoid prednisolone was inserted into the film by the equilibrium swelling method; after this plasma immersion ion implantation (PIII) was applied to modify the coating for improved release kinetics. This treatment causes the formation of oxygencontaining and unsaturated carbon–carbon groups in the PUU and a destruction of the drug in the surface layer. As a consequence, the release rate of prednisolone to water becomes more stable with time than it is at the untreated coating. In this drug release system PIII treatment prevents an initial toxically high release of the drug. By this it allows the incorporation of a higher amount of the drug and an extended action.

High-dose carbon implantation (3x10e17 and 1x10e18 ions/cm2) into cubic SiC on Si was carriedout at elevated temperatures (600 to 1200 °C) and different dose rates (1x10e13 to 1.5x10e14 cm-2 s-1). Transmission electron microscopy revealed the formation of either graphite or diamond precipitates, depending on the implantation parameters. In all cases, the diamond grains were epitaxial to the SiC lattice, while the graphite was textured. The minimum temperature for diamond formation was 900 °C, while graphite formed at 600 °C. The synthesized phase depends as well on the dose rate; graphite was formed at 900 °C with a high dose rate. Obviously, a criticaltemperature for diamond formation exists and increases with increasing dose rate. This behavior is explained by the competition between the accumulation and dynamic annealing of radiation defects in the SiC lattice, which acts as a template for diamond nucleation. Diamond grains with diametersas large as 10 nm have been observed after implantation at 1200 °C.

In the fine chemical industry, complex strongly exothermic reactions are usually carried out in semibatch mode in stirred tank reactors. These reactors are characterised by nonsteady-state conditions due to the discontinuous operation. Thus, it is difficult to estimate the actual conversion and to identify undesired process states during the chemical reaction, particularly, if the reactor is not equipped with expensive measuring systems for chemical on-line analysis. Therefore, an on-line monitoring system was developed that is able to estimate the concentration profiles without the need of chemical on-line analysis.
The on-line estimation of the concentration profiles is based on calculations of the thermal and chemical conversion courses during the chemical process using heat and mass balances. In order to consider factors of influence, such as heat losses, heat bridges and systematic measuring errors, adaptive model components are included. The adaptation of the complex model to the target plant is done by software-supported calculations of the adaptive parameters using process data of at least one normal batch course in the chemical plant.
The monitoring system was developed, optimised and tested by means of experiments in a miniplant at laboratory scale. As a test process, the strongly exothermic catalytic hydrogenation of an aromatic nitro compound was chosen. For industrial testing, the monitoring system was integrated into a batch-information-management system which was implemented into the process control system of a multipurpose reactor installation in the fine chemical factory at Radebeul (Degussa, Inc.). The tests showed good agreements of the estimated concentration profiles with analytical measurements in both, the laboratory and the industrial scale. Furthermore, it was found that deviant reaction courses and undesired process states can be recognised very earlier using the on-line monitoring system than with exclusive knowledge of process variables like temperatures, pressures and volume flows.

The investigation of RPV material from decommissioned NPPs offers the unique opportunity to evaluate the real toughness response. By investigation of material from the decommissioned VVER 440-type Greifswald NPP the evaluation of a standard RPV design and the assessment of the quality of prediction rules and assessment tools will be possible. First results of the investigations are presented in the paper.

Differential production cross sections of K- and K+ mesons have been measured in Ni+Ni and Au+Au collisions at a beam energy of 1.5 A·GeV. The K-/K+ ratio is found to be nearly constant as a function of the collision centrality. The spectral slopes and the polar emission pattern differ for K- and K+ mesons. These observations indicate that K+ mesons decouple earlier from the fireball than K- mesons.

The primary structures of the S-layer proteins of the uranium mining waste pile isolate Bacillus sphaericus JG-A12 and of Bacillus sphaericus NTCC9602 were analysed. The amino acid sequences of the two proteins are almost identical but possess an abrupt homology to some of the other B. sphaericus S-layers studied up to date. This is an indication that a horizontal transfer of genetic information was involved in the evolution of the genes of the mentioned S-layers. An extensive comparative analysis of the S-layer proteins deposited to the GeneBanks demonstrated that several additional S-layers of B. sphaericus and of other Bacillus species were also subjected to late evolutionary events via lateral DNA transfer. The possible mechanism of these events in the case of B. sphaericus will be discussed.
Interestingly, the slight amino acid differences between the S-layer proteins of the strains JG-A12 and NTCC9692 lead to dramatic differences in their ability to interact with metals and also in their stability against proteases. As estimated by using EXAFS spectroscopy phosphorous residues, in addition to the carboxyl groups of the proteins, are involved in the binding of uranium (VI). ICP-MS analysis demonstrated that the two purified and recrystalized S-layer proteins contain phosphorous which indicates that they are phosphorylated. Moreover, the amount of phosphorous found in the S-layer of the strain JG-A12 was six times higher than those found in the S-layer of the reference strain NTCC 9602. This explains the higher ability of the S-layer of the uranium mining waste isolate to complex uranium and other metals. The latter seems to give an advantage to the strain JG-A12 to survive in the heavily polluted with uranium and other toxic metals environment from which it was recovered.

Uranium mining waste pile isolate Bacillus sphaericus JG-A12 and it's closest relative B. sphaericus NTCC 9602 possess S-layer proteins with a similar size of about 135 kDa and with a square lattice symmetry. The two proteins differ significantly in their ability to interact with metals and in their stability against proteases and pH changes. By using ICP-MS, the "Stain-all" dye, and colourimetric method it was demonstrated that both proteins are phosphorylated but the S-layer of the strain JG-A12 contains six times more phosphorous than those of the reference strain NTCC9602. Surprisingly, the two proteins share an extremely high homology of 98 % in the region of the N-terminal S-layer homologous domains and of 91 % in the region of the central domains. It is noticeable that the minor amino acid differences between the S-layers of the studied strains consist of threonine and serine enrichments in the case of JG-A12. Bearing in mind that the majority of the phosphoproteins are usually modified at threonine and serine residues, our observation explains the higher level of phosphorylation of the S-layer of the uranium mining isolate JG-A12. The higher amount of phosphate groups of this protein explains also it's ability to complex more effectively uranium and other metals.
In addition, there are evidences that the two Bacillus sphaericus strains studied possess an additional S-layer or an S-layer-like copy which seems to be located on large indigenous plasmids.

Sol-gel ceramics with high metal binding capacity were prepared via homogeneous dispersion and embedding of vegetative cells, spores and EDC stabilised surface proteins (S-layers) of Bacillus sphaericus JG-A12. The B. sphaericus JG-A12 strain was recovered from a uranium mining waste pile near the town of Johanngeorgen-stadt, Saxony, Germany (1). The whole cells as well as the purified S-layer protein of this strain possess an ability to bind selectively and very effectively uranium and several other metals such as Cu, Pb, Cd, Al, Pt and Pd (1, 2).
In this work the biosorption of U and Cu by the above mentioned three bacteria-based biological ceramics (biocers) was investigated. In addition, the metal binding capacity of the free SiO2 nanomatrix and of the three individual bacterial components (the vegetative cells, the spores and the S-layers) was studied as well.
Our results demonstrate that the high U and Cu binding capability of the three kinds of biocomponents is influenced by the sol-gel process in a different way. The metal binding properties of the vegetative cells and of the S-layers were not negatively influenced by the sol-gel treatments. The metal binding capacity of the embedded spores was, however, significantly lower than those of the non embedded spores. Very limited amounts of U and no Cu were bound by the silicate matrix alone.
The metal binding capacity of the biocers and also the kinetic of the biosorption were positively influenced by adding water soluble compounds such as sorbitol or by freeze drying instead of air drying. These results are connected to the higher porosity achieved by the mentioned treatments.
Both metals can be completely desorbed and washed from the biocers by using 0.5 M solution of citric acid. Afterwards the biocers can be reused for metal biosorption.
Due to their stability, high metal binding capacity and simple and complete removal of the bound metals described biocers are good candidates for construction of intelligent filters for cleaning of heavy metal contaminated liquid wastes.
The geographic origin of the source of the biocomponents, namely the strain B. sphaericus JG-A12, makes the constructed bioceramics promising for in situ bioremediation of the drain waters of the uranium mining waste piles and mill tailings.

References

1. Selenska-Pobell S., Miteva V., Boudakov I., Panak P., Bernhard G., and Nitsche H. (1999) Selective accumulation of heavy metals by three indigenous Bacillus isolates, B. cereus, B. megaterium and B. sphaericus in drain waters from a uranium waste pile.FEMS Microbiol Ecology 29, 59-67.
2. Raff J (2002) Wechselwirkungen der Hüllproteine von Bakterien aus Uran-abfallhalden mit Schwermetallen PhD Thesis, FZR-Report 358

Bacterial communities were studied in several uranium mining waste piles in Germany and in the USA by using 16S rDNA and RISA retrievals. Both approaches revealed extremely high and site-specific bacterial diversity. However, several bacterial groups including also novel lineages seem to be characteristic for the studied heavy-metal-polluted environments.
In parallel with the above mentioned direct molecular approaches, the method of enrichment culturing was applied in order to recover and study particular bacterial strains indigenous for the U wastes. Bacterial isolates belonging to different species representing diverse bacterial groups were recovered and characterized. The resistance and the interactions of these isolates with U and other heavy metals were demonstrated to be species- and even strain-specific. The atomic structures and the cellular location of the complexes formed by the isolates with U(VI) were studied using EXAFS spectroscopy, TEM, and EDX analyses. In all cases phosphate groups were predominantly implicated in the complexation of uranium but the structural parameters and the cellular location of the complexes differed between the studied bacterial groups.
Many of the studied strains possess unusual characteristics as the isolate JG-A12, for instance, which accumulates selectively U, Cu, Pb, Al, and Cd. This strain as well as it's intrinsic S-layer are forming U(VI)-complexes with identical structural parameters in which phosphorous residues in addition to the carboxyl groups are involved. ICP-MS and the "Stain-all" dye methods demonstrated that the S-layer of JG-A12 is phosphorylated. This can explain it's high ability to complex uranium and other metals. The latter seems to give an advantage to the strain to survive in the heavily polluted with uranium and other toxic metals environment from which it was recovered. Pd and Pt metallic nanoclusters were also successfully grown on the sheets of this S-layer. The latter is of interest for the nanotechnology. Interestingly, the S-layer of JG-A12 possesses unusual primary structure which indicates that lateral transfer was involved in the evolution of it's gene.
1848 words.
Keywords: bacterial diversity; S-layer, EXAFS, complexation of uranium

Boron suboxide BOx thin films have been deposited on Si (100) by reactive rf magnetron sputtering of B powders in an Ar/O2 atmosphere. Elastic recoil detection analysis and x-ray diffraction were used to study the influence of the O incorporation on the film composition and structure and relate them to mechanical properties, which were evaluated by nanoindentation. As x in BOx was increased from 0.08 to 0.18, the elastic modulus of the x-ray amorphous films decreased from 273 to 231 GPa, by 15%. This can be understood using classical molecular dynamics (MD) with a Buckingham-like interaction potential: The increase in the O concentration and corresponding formation of B–O bonds, shown to be longer than the B–B bonds, resulted in larger ionic contributions as well as a density reduction. This increased ionicity was responsible for the observed decrease in elastic modulus. As even more O was incorporated (x>0.18), the H concentration increased, exceeding 0.3 at. %. This may cause the formation of boric acid (H3BO3) as a result of the chemical reaction with H2O upon atmosphere exposure. The presence of van der Waals and hydrogen bonding, associated with H3BO3 formation, provides a reasonable explanation for the extensive decrease in elastic modulus from 231 to 15 GPa, by 94%. The parameterization for the Buckingham-like interaction potential, introduced in this study, can be used for MD simulations of amorphous BOx systems without H3BO3.

Structural materials, such as bainitic and austenitic steels and aluminium alloys as
used in the nuclear and aircraft industry are subject to external stresses in different environments. Understanding the growth of an assumed preexisting crack under these conditions is of prime importance to prevent extensive crack propagation and failure of the component. The ongoing research aims to investigate the early stages of ductile fracture, the nucleation, growth and coalescence of microvoids and the evolution of the spatial dislocation distribution. Two commercial Al-alloys, alloys 2024-T351 and 6013-T6 used in the aircraft industry were investigated. Within the above framework, a small region around the crack tip of a 2024-T351 specimen was scanned using a microfocused beam of 5 µm in diameter (Esrf, ID13-Microfocus).
The major improvement lies in the strongly diminsihed influence of grain boundary scattering. Information from fracture toughness tests, from the simulation of the distribution of stresses and strains by means of finite element analysis, from scanning and transmission electron microscopy and positron annihilation microprobe experiments, will support the small angle X-ray scattering investigations.

Der Vortrag gab ein allgemeines Bild von den Kleinwinkelstreuuntersuchungen, die am FZ Rossendorf, Abt.Material-und Komponentensicherheit durchgeführt werden, ein Bild von den Materialien (Al-Legierungen und RDB-Stähle) und Techniken/Anlagen, die dazu erforscht/angewandt werden.

Der Vortrag gab das Ziel des Untersuchungsvorhabens wieder und erteilte allgemeine Informationen über den Stand der Röntgen-Kleinwinkelstreuungsforschung zur Charakterisierung der Rissspitze in Metallen.

Aim of this report is the investigation of suitable operational conditions for the drif{}t chambers MDC III installed in the HADES setup. The simulations performed showed that operating the drif{}t chambers in a mode with nearly constant electron drif{}t velocity in a predominant part of the cell allows a more precise and fast tracking. This is particularly important for electrons and positrons; here the invariant dilepton mass must be reconstructed with high precision to get a resolution of $\Delta M/M\approx 1\%$ for the $\omega$ and $\phi$ mass peaks and thus a chance to verify also small in-medium mass shif{}ts. This helps to realize the physics program at HADES which focuses on the search for such mass shif{}ts to get insight into the in-medium behaviour of hadrons in dense strongly interacting matter.

Das Verhalten einer 3-Punkt-Biegeprobe mit Anriss unter Belastung kann mittels einem Finite-Element-Modell nachgebildet werden. Das Modell ermöglicht die Berücksichtigung von elastisch-plastischem Materialverhalten entsprechend der jeweiligen materialspezifischen nichtlinearen Spannungs-Dehnungs-Kurve, welche mit dem Modell der multilinearen kinematischen Verfestigung (MKIN) umgesetzt wird. Weiterhin gestattet das Modell die Beschreibung der Rollenkinematik beim Biegevorgang. Unter Einbeziehung eines speziellen Damage-Modells für die Beschreibung des Bruchkriteriums ist das Modell in der Lage sowohl den Beginn des Risswachstums als auch den Rissfortschritt wiederzugeben.
Mit diesem Modell lässt sich auch das Teilentlastungs-Compliance-Verfahren nachbilden. Diese Simulation ermöglicht Korrekturansätze zur experimentellen Risslängenbestimmung über die Compliance-Methode.

The A533B Cl.1-type RPV steel, designated JRQ, has been used as IAEA reference steel and shows a high sensitivity against radiation embrittlement. Specimens from this material were irradiated to three different levels of neutron fluences. Thus, the investigation allows to realize the dependence of microstructural changes on the fluence and a comparison with results on VVER-type RPV steels, which differ from the Western RPV steel design.

Durch Bestrahlung mit Neutronen entstehen in Konstruktionswerkstoffen nanoskalige Strukturdefekte, die vielfach mit den hochauflösenden, direkt abbildenden Untersuchungsverfahren nicht oder nicht ausreichend nachweisbar sind. Diese Strukturdefekte führen aber zu einer erhöhten Streuung von Neutronen- und Röntgenstrahlen im Kleinwinkelbereich. Aus der Intensitätsverteilung der Kleinwinkelstreuung lassen sich, wenn vereinfachende Annahmen getroffen werden können oder Vorinformationen vorhanden sind, Größenverteilung und Anzahldichte bestimmen. Darüber hinaus sind Hinweise zum Typ und zur Zusammensetzung der Defekte ableitbar. Das Kleinwinkelstreuverfahren ist effektiv, volumenintegrierend, sensitiv im Größenbereich von ~ 1 nm ... 10 nm und unempfindlich gegenüber Präparationsfehlern. Es ist jedoch eine indirekte Methode der Strukturanalyse und sollte deshalb nicht alternativ, son-dern komplementär angewandt werden. Prozedur und Leistungsfähigkeit des Verfahrens wird am Beispiel von Untersuchungen an bestrahlten Reaktordruckbehälterstäh-len gezeigt.

At present, the Gas Dynamic Trap (GDT) facility of the Budker Institute Novosibirsk is being upgraded. The first stage of the upgrade is the Synthesized Hot Ion Plasmoid (SHIP) experiment. It aims, on the one hand, at the investigation of plasmas which are expected to appear in the region of high neutron production in a GDT based fusion neutron source proposed by the Budker Institute and, on the other hand, at the investigation of plasmas the parameters of which have never been achieved before in magnetic mirrors. In parallel to experimental research at the GDT an Integrated Transport Code System (ITCS) is under development in collaboration with the Forschungszentrum Rossendorf. It is to calculate the relevant physical effects which are connected with neutral gas, background plasma and with the high-energetic ion component inside the central cell of the GDT and later inside the neutron source.
This contribution explains the concept of the SHIP experiment and presents the results of first calculations by means of ITCS modules.