Industrial Applications of Synchrotron Radiation

J. Homeyer, U. Krell, J. Wienold and T. Wroblewski

Introduction

Synchrotron radiation and the variety of experiments installed at HASYLAB provide inmany cases the key to problems arising from technological challenges in industrialresearch or development. It is the aim of DESY-HASYLAB, to support applications ofsynchrotron radiation in collaboration with industrial partners. To facilitate access to thelaboratory and the wide range of techniques available, an industrial service group co-ordinates these activities. The group provides contact to the companies, defines thetechnique to solve the problem under question and helps in carrying through themeasurements. To organise industrial collaborations DESY has created the HASYLAB co-operation model.

In the co-operation model fast access to beam time can be provided and a publication ofthe results, which is otherwise mandatory for all experiments at HASYLAB, may bedelayed or fully omitted. The service group co-ordinates the preparation of themeasurements, it can provide help during the experiment and does in many cases the dataanalysis. To offer highest flexibility and best service HASYLAB promotes the idea oflong-term engagement of the industrial partners. Within the three-years contracts moreknowledge is gathered about the specific problems under investigation on the one handand about synchrotron radiation techniques and their possibilities and limitations on theother hand. This way the collaboration becomes more effective. Furthermore, we canprovide full service and fast access to beam time only for long-term co-operationprojects.

The HASYLAB co-operation model distinguishes between industrial basic research,applied research and propriety research.

For basic research companies can apply for beam time, just as universities or researchinstitutes. The proposal will undergo peer reviewing, beam time will be distributed on along-term planning and the results have to be published. For basic research no fees for theusage of the facility will be charged. The service group provides help in selection of thetechnique and preparation of the proposal.

For applied research projects companies may request fast access to beam time. Theproposal is not peer reviewed, only safety issues must be declared in advance. Results orreports of these measurements have to be published. In a long-term co-operation contractthe publication can be delayed. For applied research projects the use of the facility and itsinstruments is charged on an hourly basis.

In propriety research projects results may not be published at all. Approval and fastaccess to beam time are handled as for applied projects. Here the charges for beam timeare higher than for applied projects.

Current projects

Industrial research using X-ray absorption spectroscopy comprise a short term projectand the continuation of two long term projects. The latter are both dealing with the in situcharacterization of catalyst and were carried out at the beam line X1. To provide

experiments which allow the simultaneously detection of diffraction pattern and X-rayabsorption spectra, either in transmission or in fluorescence mode, the development of anin situ cell is under way. The cell is planned to be suitable for the use of corrosive gasesand temperatures up to ~770K. The required detector and the cell will be available for thebeam lines E4 and X1 to complete the present capabilities. This technique is alreadysuccessfully applied by one of the industrial user groups at beam line X1 [1] (The usersutilize their own equipment.). A long term project with the Institute Français de Pétrol(IFP) to start in 2004 was established.

Several different applications with industrial background were performed at the highenergy wiggler beam line BW5 and at the energy dispersive beam line F3 in the field ofmaterials science and engineering to study the properties of bulk material non-destructively.

In the third year within the cooperation between the Hamburg synchrotron radiationlaboratory and the Materials Science Research Department of Risø, Denmark, the texturestudies of BSCCO/Ag superconductor tapes were successfully continued by Niels HesselAndersen, Jean-Claude Grivel and co-workers. The investigations were performed atroom temperature as well as at elevated temperatures up to 1200 K and at photonenergies of 100 keV to investigate the phase assemblage and possible preferentialorientation of the tetragonal BSCCO/Ag material. The effects of different sinteringtreatments under inert nitrogen atmosphere were studied after annealing and in-situ atbeam line BW5.

Two additional short-term projects were carried out at BW5 and in parts at F3 onindustrial products. After the first successful feasibility studies on spray compactedAluminum for applications in automotive industries residual stress analysis werecontinued on these materials using the high resolution three crystal axis set up of BW5 incombination with a one dimensional Germanium detector at 100 keV. The results of theresidual stress analysis of the bulk material obtained by X-ray diffraction performed withthe sin2ψ method have to be compared with those given by finite element calculationsand the drilling hole method to get a deeper insight into production processes.

First feasibility studies for texture analysis on coated and uncoated zirconia tubes werecarried out for Framatome, Germany, with photon energies of 100 keV using the areadetector set-up of BW5. State of the art investigations of zirconia tube textures with aninner diameter of approximately 8 mm are only obtainable with a laboratory X-ray tubein reflection mode. At the moment samples have to be investigated by stepwise removalof material due to the low penetration depth of X-ray tube radiation. Investigation intransmission mode, however, provides the opportunity to get the information about thetexture and the physical properties of the polycrystalline material around and within thetube walls non-destructively in spite of the small tube diameter.Further investigation on zirconia tubes were performed at beam line F3 in energydispersive mode. This enables the detection of the full X-ray spectrum in the energyrange between 30 up to 75 keV simultaneously to study the texture modification withinthe tube wall with a higher spatial resolution comparable to the one achieved in angledispersive mode yet. This project triggered the development of a novel technique for theinvestigation of inner surfaces, which is also of relevance for non-industrial users (see‘Novel techniques for energy dispersive diffraction’ in this annual report).

For the first time ultra small angle scattering investigations were performed on polymermaterials for an industrial user at beam line BW4. Studies using the stretching device

were made at room temperature and at elevated temperatures up to 400 K under vacuumconditions to get a better understanding of polymer behavior.

A slight decrease in the number of projects in industrial application of proteincrystallography was observed at the EMBL beamlines, which was partially compensatedby increased activities at the MPG/ASMB beamline.

Fig. 1: Julia Wienold and three colleagues from GKSS at their booth on the Materialica 2003

Further activities

The service group industry had several presentations on national (‘XXXVII. JahrestreffenDeutscher Katalytiker’, DGK-Jahrestagung) and European (_-MRS Fall Meeting)conferences and workshops. In the framework of the ‘International Workshop on HardSynchrotron X-rays for Texture and Strain Analysis’ (April 2003, Hamburg) and theMECASENS conference (September 2003, Manchester) the service group participated intwo VAMAS(Versailles Project of Advanced Materials and Standards) meetings. Thescope of the collaboration embraces all agreed aspects of science and technologyconcerned with advanced materials, including materials technology, test methods, designmethods and materials databases that are required as a precursor to the drafting ofstandards. One scope of VAMAS is the standardization of measuring procedures (in thiscase the standardization of strain determination with high energy X-rays). Additional tothis, members of the ‘Service Group Industry’ visited exhibitions and conferences withand without own presentations to acquaint the possibilities of synchrotron radiation to thepublic. In this course, the service group Industry participated on a booth of the ‘GKSS

Forschungszentrum’ Geesthacht, at the ‘Materialica 2003’ in München. ‘Materialica’ is atrade fair for materials and materials design as well as processing. Additionally the‘Hannover Messe 2003’ and the ‘ACHEMA 2003’ were visited to contact possiblecustomers.

Several organizations of potential industrial users (FA Eigenspannung derArbeitgemeinschaft Wärmebehandlung und Werkstofftechnik, Deutsche Gesellschaft fürZerstörungsfreie Prüfung) could be encouraged to organize their meetings at HASYLABincluding a presentation of the service group and a guided tour to the relevant facilities.

The ‘Service Group Industry’ of HASYLAB has organized in collaboration with ANKAGmbH and BESSY GmbH a workshop about in situ XAS applications in catalysistargeted for industry, which was carried out on the 19th of November 2003 at the DESYsite (see separate report). This one is planned to be the first one in a series of followingevents on different topics.

Further information about industrial applications of synchrotron radiation at HASYLAB,its conditions and selected examples can be found in the leaflet “Service Group Industry– Your Partner for Research” or on our web presentation : www-hasylab.desy.de/industry_cooperation/main.htm.

References

[1] J.-D. Grunwaldt and B.S. Clausen, “Combining XRD and EXAFS with on-Line CatalyticStudies for in situ Characterization of Catalysts”, Topics in Catalysis 18 (1-2) (2002) 37-43.

[2] A. Puig-Molina, L.P. Nielsen, A.M. Molenbroek, K. Herbst, "In situ EXAFS study on thechemical state of arsenic deposited on a NiMoP/AL2O3 catalyst", To be published in Cat.Let. (2003)

[3] J. W. Andreasen, O. Rasmussen, R. Feidenhans'l, F. Berg Rasmussen, R. Christensen,A.M. Molenbroek and G. Goerigk, "An in situ cell for small-angle scattering experimenton nano-structured catalysts", J. Appl. Cryst. (2003). 36, 812-813

[4] Frank B. Rasmussen, Herman T. Teunissen, Alfons M. Molenbroek, Jens Sehested, RobinChristensen, Anne-Mette H. Kjær and Bjerne S. Clausen, "Particle Size Distribution ofSupported Ni Catalysts Prepared by Impregnation and Deposition-Precipitation",Approved for publication in Kinetics and Catalysis, May 2003.