Project-Group ESRF-Beamline (Robl-Erg)
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FORSCHUNGSZENTRUM RO Mitglied der Wissenschaftsgemeinschaft Gottfried Wilhelm Leibniz WISSENSCHAFTLICH-TECHNISCHE BERICHTE FZR-322 Tuni2001 ISSN 1437-322X Project-Group ESRF-Beamline (ROBl-eRG) 1500 ~ 1000~ (J) c .s:.l!! 500 go c - 2763A 2363A -- 1963A 156304 -- 1163A ....'---::-:-.::...:.----:::-=::=;<=:::::::::::::::;:=======:.:::---::;;t-..- as:r A 2.6 2.8 3.0 3 2 . th"kn Q = 41tsinelA (A"1) Je ess Bi-Annual Report 1999/2000 Cover picture: Representation of aseries of vertical Bragg-Brentano scans as a function of film thickness collected during in situ observation of TiN film desposition at ROBL-MRH. The sequence demonstates the change of texture of TiN with increasing film thickness. At the beginning of the deposition process (002) planes if the cubic lattice are parallel to the surface. For larger thicknesses the preferred orientation becomes (111), indicated by the much faster intensity increase of this reflection (see contribution on p. 5). Forschungszentrum Rossendorf P·:stfach 51 :J 1 19 Ts~e~on "'!9;3 51 2 6·J 31 22 I:e':e~ax -49 f3 51. f/2: 3';~'2 FORSCHUNGSZENTRUM ROSSENDORF Mitglied der Wissenschaftsgemeinschaft Gottfried Wilhelm Leibniz WISSENSCHAFTLICH-TECHNISCHE BERICHTE FZR-322 Juni 2001 Bi-Annual Report 1999/2000 Project - Group ESRF-Beamline (ROBL-CRG) Editor: W. Matz Preface The second report from the Project-Group ESRF-Beamline of the Forschungszentrum Rossendorf covers the period from July. 1999 until December 2000. The ROssendorf BeamLine (ROBl) at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France performed quite weil during this time. In the beamtime used by the FZR and collaborating institutes 44 scheduled experiments were performed, while in the ESRF scheduled beamtime 12 experiments. Additionally, a distinct amount of beamtime was devoted to in-house research of the FZR and methodical experiments. The main effort from the technical point of view during the reporting period was made in the improvement of equipment.. At the radiochemistry end-station a closed cycle He cryostat was commissioned and a newly developed control software XATROS for control and data acquisition in the EXAFSIXANES experiments was installed. At the materials research end station an analyser system in front of the detector and the two-dimensional CCD-detector were commissioned during the period. Additionally, a small chamber for in situ structural studies of thin films during sputter deposition was designed and commissioned. Two of the following contributions demonstrate as examples the new scientific possibilities with this equipment. Since February 2000 ROBl is part of the European Commission's programme "Access to Research Infrastructure" which supports user groups from member and associated states of the EU during experiments at ROBL. In the year 2000 ROBl hosted 6 groups for experiments. The "2nd Euroconference and NEA Workshop on Speciation, Techniques, and Facilities for Radioactive Materials at Synchrotron Light Sources" took place in Grenoble 10-12 September 2000. The FZR was main organiser of this workshop which was attended by over 70 scientist from 10 countries. The ROBl-CRG would Iike to thank all partners, research groups and organisations who supported its progress during the last 18 months. Special thanks are due to the FZR management, the CRG office and the Safety group of the ESRF. The report is organised in three main parts. The first part contains extended contributions on results obtained at ROBL. The second part gives an overview about the scheduled experiments, publications, guests having visited ROBl with support of the EC, and some other information. Finally, the third part collects the experimental reports of the user groups received. !J&ff;/7~ Dr. Wolfgang Matz 3 Contents Page Contributions A miniature sputter deposition chamber for in situ film growth studies by synchrotron radiation scattering 5 In situ study of phase transformation at elevated temperature and correlated mechanical degradation of nitrogen implanted Ti-6AI-4V alloys 12 X-ray waveguides at ROBL: New developments and applications 18 EXAFS measurements of radioactive sampies at low temperature 22 XANES and EXAFS measurements of plutonium hydrates 27 Local structure of Th complexes on montmorillonite clay mineral determined by extended X-ray absorption fine structure (EXAFS) spectroscopy 33 Statistics Overview about the beamtime distribution at ROBL 39 Support of user groups by the European Commission 40 List of EC supported users of ROBL 41 Scheduled experiments at the radiochemistry end-station 42 Scheduled experiments at the materials research end-station 45 List of publications 47 Personnel of the Project-Group ESRF-Beamline 50 Experimental reports Experimental reports from the radiochemistry end-station (No. 20_01_XXX) 51 Experimental reports from the materials research end-station (No. 20_02_xxx) 74 Experimental reports from experiments scheduled by the ESRF 98 4 A miniature sputter deposition chamber for in situ film growth studies by synchrotron radiation scattering 1 1 3 N. Schell , W. Matz ,2, W. Neumann 1 Project Group ESRF-Beamline; 2 Institute of Ion Beam Physics and Materials Research; 3 Central Department Experimental Facilities and Information Technology Forschungszentrum Rossendorf, P.O. Box 51 01 19,01314 Dresden, Germany J. B0ttiger, J. Ghevallier, P. Kringh0j Institute of Physics and Astronomy, University of Aarhus, 8000 Aarhus C, Denmark 1. Introduction The technological importance of thin films has stimulated an increasing interest in the detailed characterisation of the structure and morphology of thin films and their interfaces as weil as the underlying growth mechanisms. It is achallenge to understand, both experi mentally and theoretically, the growth mode and the micro-structural development during deposition of thin films. This development depends crucially on the deposition parameters, and such knowledge is required to tailor the film microstructure for specific applications. One widespread technique for layer deposition is sputtering. It is applied for pure elements as weil as for compounds. As its vacuum requirements are only moderate, electron diffraction as in situ characterisation method is not applicable. However, x-rays are in that case a powerful probe. In the literature some deposition chambers for in situ x-ray diffraction and reflectivity during sputtering are described [1-4]. They are, however, mostly adapted to a special dedicated instrument and use instrumental functions not commonly available. Dur approach was to develop a low cost chamber which allows to follow in situ the film growth and post deposition annealing by different modes of synchrotron radiation scattering. The chamber should fit into the standard HUBER six-circle goniometer which is used as a multi purpose instrument for many other experiments at the materials end-station of the Rossendorf Beamline ROBL in Grenoble [5]. 2. Chamber design In order to get as much information as possible on the growth process, the sputter deposition chamber allows for the following types of experiments: • symmetrie x-ray diffraction (Bragg-Brentano geometry) for measuring out-of-plane lattice constants and texture • vertical grazing incidence diffraction for enhancing the signal of very thin films and suppressing substrate scattering • reflectometry for determining the film thickness and interface roughness • in-plane grazing incidence/exit diffraction (GIXS) for the determination of lattice constants, stress and preferred orientation in the surface plane • crystal truncation rod scattering to determine the growth mode (step f1ow, layer-by- layer or island formation). To allow the preparation of either multi-component films or multi-Iayer structures, the chamber is equipped with two magnetrons and inlets for two sputter gases. To start with clean Le. defined conditions, the vacuum reaches a base pressure of less than 10'" mbar before starting the sputtering process. Furthermore, substrate heating and bias are installed. Gosts aside, the main /imitations in the design were geometrical ones. It was necessary to respect the maximum load (15 kg) and space restrietions of the existing standard HUBER goniometer in order to guarantee the high precision of the settings (0.001°) [6]. Taking those 5 limitations into account one can use afl existing instaflations/equipment at the goniometer like detectors, slits, collimators, filter units without any further modifications. The goniometer it~elf allows horizontal as weil as vertical scattering geometries, and thereby afl scattermg techniques described above. Fig. 1 shows the sputter deposition chamber inserted for experiments and Fig. 2. an interior cross-section. A detailed description can be found in Ret. [7]. The chamber conslsts of three separable parts: A central one connected to the cp-circle of the goniometer and equipped with different flanges on the circumference (for pumps, connected via throttle valves, vacuum gauges and a liquid nitrogen trap) and one bigger flange in the bottom which goes through the opening of the cp-circle and connects the demountable substrate carrier to the chamber. The hemispherical top is equipped with four radiation windows (made from 125 pm thick Kapton and sealed with Viton rings), flanges for the two unbalanced magnetrons (commercially available from AJA International [8]) - each placed at a distance of 100 mm fram the substrate and tilted 30 degrees away from the substrate normal. Fig.1: Fig.2: Photo of the deposition chamber mounted into