The research focuses on the characterization of solid catalysts by means of powder diffraction techniques and surface sensitive spectroscopic methods. Particular interest is put on the relationship between crystal structures and the properties of functional materials. Intensive research activities lay on diffraction studies of catalysts under reaction conditions. For this purpose, several sample environments have been developed which allow diffraction experiments, e.g. under high gas pressures. Another centre of activity is on the evaluation of microstructure properties of inorganic compounds. Microstructure details are elucidated from powder diffraction data by modern methods such as WPPM which refine diffraction profiles based on physical sound models. Aim of the research is the correlation of catalytic properties and microstructure characteristics of inorganic nanosized materials.

Untersuchungsmethoden von Materialien unter „non ambient“ Bedingungen, Universität Bochum, WS2010/2011
Informations and documents can be found on the lecture website of Ruhr-Universität Bochum.
Pommerin, A., Wosylus, A., Felderhoff, M., Schüth, F., Weidenthaler, C.*
Synthesis, crystal structures, and hydrogen storage properties of Eu(AlH4)2 and Sr(AlH4)2, and of their decomposition intermediates, EuAlH5 and SrAlH5.
Inorg. Chem. Accepted
Tüysüz,H., Weidenthaler,C.,Schüth, F.
A novel strategy to create mesostructured metal oxides with lower oxidation state.
Chemistry - A Euopean Journal, Accepted
Kaper,H., Grandjean,A., Weidenthaler,C., Schüth,F., Goettmann, F.
Surface Diels–Alder Reactions as an Effective Method to Synthesize
Functional Carbon Materials.
Chemistry - A European Journal, DOI: 10.1002/chem.201102718
Jia, C.J., Schwickardi, M., Weidenthaler, C., Schmidt, W., Korhonen, S., Weckhuysen, B.M., Schüth, F.
Small sized Co3O4-SiO2 composite: A very active catalyst for CO oxidation with unusual catalytic behavior, JACS, accepted
Shao, H., Felderhoff, M. Schüth, F., Weidenthaler C.
Ti-catalysed nanostructured MgH2 of hydrogen storage;
Nanotechnology, Vol 22, 235401 (2011)
DOI: 10.1088/0957-4484/22/23/235401
Weidenthaler C., Felderhoff M.
Hydrogen Storage for Mobile Applications – Quo Vadis?
Energy Environ. Sci., in press 2011
Weidenthaler, C:
Pitfalls in the characterization of nanoporous and nanosized materials.
Nanoscale 3 (2011) 792 - 810
DOI:10.1039/c0nr00561d
Feyen, M., Weidenthaler, C., Güttel, R., Schlichte, K., Holle, U. Lu, A.H., Schüth, F.
High-Temperature Stable, Iron-Based Core-Shell Catalysts for Ammonia Decomposition
Chemistry –A European Journal 17 (2011) 598-605
Dangwal Pandey, A., R. Güttel, M. Leoni, F. Schüth, C. Weidenthaler*
Influence of the microstructure of gold-zirkonia yolk-shell catalysts on the CO oxidation activity.
J. Phys. Chem. C. 114 (45), 19386–19394 (2010)
Lu, A.H., J.J. Nitz, M. Comotti, C. Weidenthaler, K. Schlichte, C. W. Lehmann, O. Terasaki, F. Schüth
Spatially and Size Selective Synthesis of Fe-Based Nanoparticles on Ordered Mesoporous Supports as Highly Active and Stable Catalysts for Ammonia Decomposition.
J. Am. Chem. Soc. DOI: 10.1021/ja105308e (2010).
Jia, C.J., Y. Liu, M. Schwickardi, C. Weidenthaler, B. Spliethoff, W. Schmidt, F. Schüth
Small gold particles supported on MgFe2O4 nanocrystals as novel catalyst for CO oxidation. Appl. Catal. A General 386, 94-100 (2010).
Pommerin, A., M. Felderhoff, F. Schüth, C. Weidenthaler*
Influence of the ball milling conditions on the preparation of rare earth aluminum hydrides.
Scr. Mater. 63, 1128-1131 (2010).
Feyen,M., Weidenthaler,C., Schüth,F., Lu, A.H.
Synthesis of Structurally Stable Colloidal Composites as Magnetically Recyclable Acid Catalysts Chem. Mater. 22 (2010) 2955-2961.
Feyen,M., Weidenthaler,C., Schüth,F., Lu, A.H.
Regioselectively Controlled Synthesis of Colloidal Mushroom Nanostructures and Their Hollow Derivatives
J. Amer. Chem. Soc. 32 (2010), 6791-6799.
Huang, A., Weidenthaler, C., Caro, J. Facile and reproducible synthesis of ITQ-29 zeolite by using Kryptofix 222 as the structure directing agent.
Micropor. Mesopor. Mater. 130 (2010) 352-356.
Pommerin, A., Weidenthaler, C., Schüth, F., Felderhoff, M.
Direct Synthesis of Pure Complex Aluminium Hydrides by Cryomilling.
Scripta Mater. 62 (2010) 576-578
Weidenthaler, C., Felderhoff M.
Complex Metal Hydrides: Handbook of Hydrogen Storage, New Materials for Future Energy Storage, Ed. Hirscher M.; Wiley-VCH (2010)
Weidenthaler, C., Pommerin, A., Felderhoff, M., Sun, W.S., Wolverton C., Bogdanovic, B., Schüth, F. Complex Rare-Earth Aluminum Hydrides: Mechanochemical Preparation, Crystal Structure and Potential for Hydrogen Storage.
J. Amer. Chem. Soc. 131 (2009) 16735
Pawelke, R.H., Felderhoff, M., Weidenthaler, C., Bogdanovic, B., Schüth, F.
Mechanochemical synthesis of ternary potassium transition metal chlorides.
Z. Anorg. Allg. Chem. 635 (2009) 265-270.
Zukerman, R., Vradman, L., Weidenthaler, C., Landau, M.V., Herskowitz, M.
Effect of silica wall microporosity on the state and performance of TiO2 nanocrystals in SBA-15 matrix Micropo.
Mesopor. Mater. 116 (2008) 237-245.
Hou, Z., Theyssen, N. Brinkmann, A., Klementiev, K.V., Grünert, W., Bühl, M.., Schmidt, W. Spliethoff, B., Tesche, B., Weidenthaler, C., Leitner, W.
Supported palladium nanoparticles on hybrid mesoporous silica: Structure/activity-relationship in the aerobic alcohol oxidation using supercritical carbon dioxide
J. Catal. 258 (2008) 315-323.
Pawelke, R., Felderhoff, M., Weidenthaler, C., Schüth, F.
Convenient synthesis of deuterated aluminium hydrides
Script. Mater. 59 (2008) 515-517.
Tüysüz, H., Lyon, L., Weidenthaler, C., Schüth, F.
Pseudomorphic Transformation of Highly Ordered Mesoporous Co3O4 to CoO via Reduction with Glycerol
J. Am. Chem. Soc. 130 (2008) 14108-14110
Pommerin, A., Felderhoff, M., Goddard, R., Weidenthaler, C.
Crystal structure of bis(diglyme-O,O ',O '')bis((mu(2)-deutero)trideuteroaluminato-D)calcium, Ca(AlD4)(2)(C6H14O3)(2)
Z. Krist.- New Crystal Structures 223 (2008) 67-68.
Tüysüz, H., Salabaş, E.L., Weidenthaler, C., Schüth, F.
Synthesis and magnetic investigation of ordered mesoporous 2-line ferrihydrite.
J. Am. Chem. Soc. 130 (2008) 280-287
Schmidt, W., Wilczok, U., Weidenthaler, C., Medenbach, O., Goddard, R., Buth, G., Cepak, A.
Preparation and Morphology of Pyramidal MFI Single-Crystal Fragments.
J. Phys. Chem. B 111 (2007) 13538-13543
Ritterskamp, P., Kuklya, A., Wüstkamp, M., Kerpen, K., Weidenthaler, C., Demuth, M.
A Titanium Disilicide Derived Semiconducting Catalyst for Water Splitting under Solar Radiation—Reversible Storage of Oxygen and Hydrogen
Angew. Chem., Int. Ed. 46 (2007) 41, 7770-7774.
Felderhoff, M., Weidenthaler, C. von Helmolt, R., Eberle, U.
Hydrogen storage: the remaining scientific and technological challenges.
Phys. Chem. Chem. Phys. 9 (2007) 2643-2653.
Comotti, M., Weidenthaler, C., Li, W.C., Schüth, F.
Comparison of gold supported catalysts obtained by using different allotropic forms of titanium dioxide
Topics in Catalysis 44 (2007) 275-284.
Rufinska, A., Goddard, R., Weidenthaler, C., Buehl, M., Poerschke, K.-R.
Structural Properties and Dynamics of Five-Coordinate Nickel(II)-II-Allyl Complexes Containing Monodentate Phosphorus Ligands.
Organometallics 25 (2006) 2308-2330
Weidenthaler, C., Frankcombe, T., Felderhoff, M.
First crystal structure studies of CaAlH5.
Inorg. Chem. 45 (2006) 3849-3851
Arnal, P.M., Weidenthaler, C., Schüth, F.
Monodisperse zirconia hollow spheres with remarkable textural properties.
Chem.Mater. 18 (2006) 2733-2739
Ritzkopf, I., Vukojević, S. Weidenthaler, C., Grunwaldt, J.D. Schüth, F.
Decreased CO production in methanol steam reforming over Cu/ZrO2 catalysts prepared by the microemulsion technique
Applied Catalysis A, 302(2) (2006) 215-223.
Khelashvili, G., Behrens, S., Weidenthaler, C., Vetter, C., Hinsch, A.
Kern, R. Skupien, K., Dinjus, E., Bönnemann, H.
Catalytic platinum layers for dye solar cells. A comparative study.
Thin Solid Films 511 (2006) 342-348
Mamatha, M., Weidenthaler, C.*, Pommerin, A., Felderhoff, M. Schüth, F.
Comparative studies of the decomposition of alanates followed by in situ XRD and DSC methods.
J. Alloys Compd. 416 ( 2006) 303-314.
Nagabhushana, K.S., Weidenthaler, C., Bönnemann, H., Hočevar, S., Strmčnik, D., Gaberšček, M., Antozzi, L.A., Martelli G. N.
Preparation, Characterization and Properties of Pt-Cu Co-reduced and Pt @ Cu Onion-Type Bimetallic Supported Electrocatalysts.
J.New Mater. Electrochem. Sys. 9 (2006) 73-81
Smått, J.H., Weidenthaler, C., Rosenholm, J.B., Lindén, M.
Hierachically Porous Metal Oxide Monoliths Prepared by the Nanocasting Route.
Chem.Mater. 18(6) (2006) 1443-1450.
Krawiec, P. De Cola, P.L., Gläser, R., Weitkamp, J., Weidenthaler, C., Kaskel, S.
Oxide Foams for the Synthesis of High Surface Area Vanadium Nitride Catalysts
Adv. Mater. 18(4) (2006) 505-508.
Mamatha, M., Bogdanović, B., Felderhoff, M., Pommerin, P., Schmidt, W., Schüth, F. Weidenthaler, C.
Mechanochemical preparation and investigation of properties of magnesium, calcium and lithium magnesium alanates
J. Alloys Comp. 407(1-2) (2006) 78-86.
Weidenthaler, C., Lu, A.H., Schmidt, W., Schüth, F.
X-ray Photoelectron Spectroscopic Studies Of PAN-Based Ordered Mesoporous Carbons (OMC)
Micropo. Mesopor. Mater. 88 (2006) 238-243.
Weidenthaler, C., Mao, Y., Schmidt, W.
Mixed CoNiAl spinels synthesized from ion-exchanged zeolites A and X
Studies in Surface Science and Catalysis, 158 (2005) 415-422.
Li, W.C., Lu, A.H, Weidenthaler, C., Goddard, R., Bongard, H.J., Schüth, F.
Growth of single crystal α-Al2O3 nanofibers on a carbon aerogel substrate
J. Mat. Chem. 15(29) (2005) 2993-2996
Bellosta v. Colbe, J.M., Felderhoff, M., Bogdanovic, B., Schüth, F., Weidenthaler, C.
One-step direct synthesis of Ti-doped sodium alanate hydrogen storage material.
Chem. Comm. 37 (2005) 4732-4734.
Ould-Ely, T., Thurston, J.H., Kumar, A. Respaud, M. Guo, W. H., Weidenthaler, C., Whitmire, K. H.
Wet-chemistry synthesis of nickel-bismuth bimetallic nanoparticles and nanowires. Chem. Mater. 17 (2005) 4750-4454.
Weidenthaler, C., Zibrowius, B., Schimanke, J., Mao, Y., Mienert, B., Bill, E., Schmidt, W.
Oxidation Behavior of Ferrous Cations During Ion Exchange under Atmospheric Conditions in A, X, and Y Zeolites
Micropor. Mesopor. Mat. 84(1-3) (2005) 302-317.
Wen, F., Bönnemann, H., Mynott, R.J., Spliethoff, B., Weidenthaler, C., Palina, N., Zinoveva, S., Modrow, H.
Preparation of Pt13 clusters in the presence of trialkyl aluminium
Appl. Organometal. Chem. 19 (2005) 827-829
Weidenthaler, C.*, Pommerin, A., Felderhoff, M., Schmidt, W. Bogdanović, B., Schüth, F.
Evidence for the existence of -Na3AlH6: Monitoring the phase transformation from -Na3AlH6 by in-situ methods.
J. Alloys Comp. 398 (2005), 228-234
Yang, C.M., Weidenthaler, C., Spliethoff, B., Mayanna, M., Schüth, F.
Facile Template Synthesis of Ordereed Mesoporous Carbon with Polypyrrole as Carbon Precursor.
Chem. Mater. 17 (2005), 355-358
Li, W.C., Lu, A.H., Weidenthaler, C., Schüth, F.
Hard-Templating Pathway To Create Mesoporous Magnesium Oxide.
Chem. Mater. 16 (2004) 5676-5681.
Felderhoff, M., Klementiev, K., Grünert, G., Spliethoff, B., Tesche, B., Bellosta von Colbe, JM, Bogdanović, B., Härtel, M., Pommerin, A., Schüth, F., Weidenthaler, C.
Combined TEM-EDX and XAFS studies of Ti-doped sodium alanate
Phys. Chem. Chem. Phys.6(17) 2004, 4369-4374.
Krawiec, P., Weidenthaler, C., Kaskel, S.
SiC/MCM-48 and SiC/SBA-15 Nanocomposite Materials
Chem. Mater. 16 (2004) 2869-2880.
Schüth, C., Kummer, N.A., Weidenthaler, C., Schad, H.
Field application of a tailored catalyst for hydrodechlorinating chlorinated hydrocarbon contaminants in groundwater”,
Applied Catalysis B: Environmental 52 (2004) 197-203.
Karafilidis, C., Hermann, H.; Rufinska, A.; Gabor, B.; Mynott, R. J.; Breitenbruch, G.; Weidenthaler, C.; Rust, J.; Joppek, W.; Brookhart, M. S.; Thiel, W.; Fink, G.
Metallocene-catalyzed C7-linkage in the hydrooligomerization of norbornene by s-bond metathesis: Insight into the microstructure of polynorbornene.
Angew. Chem. International Edition, Vol. 43(18) (2004) 2444-2446.
Reetz, M.T., Schulenburg, H., Weidenthaler, C., Spliethoff, B., Dreier, A., Bongard, H., Lopez, M.
PtOx/C based catalysts with high metal loading for oxygen reduction in PEM fuel cell.
VDI-Berichte (2003), 1803(Nanofair 2003: New Ideas for Industry, 2003), 243-246.
Weidenthaler, C., Pommerin, A., Felderhoff, M., Bogdanovic, B., Schüth, F.
On the state of the titanium and zirconium in Ti- or Zr-doped NaAlH4 hydrogen storage material.
Phys. Chem. Chem. Phys. 5 (2003) 5149-5153.
Weidenthaler C., Brijoux, W., Ould-Ely, T., Spliethoff, B., Bönnemann, H.
Synthesis and characterization of a new modification of PtAl.
Appl. Organometal. Chem. 17 (2003) 701-705.
Kahlenberg, V., Rakic, S., Weidenthaler, C.
Room - and high - temperature single crystal diffraction studies on g - Na2Si2O5: an interrupted framework with exclusively Q3 - units.
Z. Krist. 218(6) (2003) 421-431.
Zibrowius, B., Weidenthaler, C., Schmidt, W.
Sorbate-inuced changes in the framework of ETS-10 as detected by 29Si MAS NMR spectroscopy and X-ray powder diffraction
Phys. Chem. Chem. Phys. 5 (2003) 773-777.
Bogdanovic, B., Felderhoff, M. Germann, M., Härtel, M., Pommerin, A., Schüth, F., Weidenthaler, C., Zibrowius, B.
Investigation of hydrogen discharging and recharging process of Ti-doped NaAlH4 by X-ray diffraction analysis (XRD) and solid state NMR spectroscopy
J. Alloys Comp.350 (2003) 246-255.
Weidenthaler, C., Mao, Y., Schmidt, W.
Competitive ion exchange of transition metals in low silica zeolites.
Stud. Surf. Sci. Catal. Vol. 142 (2002) 1857-1864.
Rakic, S., Kahlenberg, V., Weidenthaler, C., Zibrowius, B.
Structural characterization of high pressure c-Na2Si2O5 by single crystal diffraction and 29SiMAS NMR
Physics and Chemistry of Minerals 29 (2002) 477-484.
Kahlenberg, V., Weidenthaler, C.
High temperature single crystal diffraction study on monobarium gallate - the crystal structure of b-BaGa2O4
Solid State Science 4 (2002) 963-968.
Bönnemann, H., Brijoux, W., Hofstadt, W., Ould-Ely, T., Schmidt, W., Waßmuth, B., Weidenthaler, C.
Wet chemistry synthesis of b-nickel aluminide NiAl
Angew. Chem.Int. Ed. 41(4) (2002) 599-603.
Schmidt, W., Weidenthaler, C.
A novel synthesis route for high surface area spinels using ion exchanged zeolites as precursors
Micropor. Mesopor. Mater. 48 (2001) 89-94.
Schmidt, W., Weidenthaler, C.
Heavy metal exchanged zeolites as precursors for high temperature stable phases
Stud. Surf. Sci. Catal. 135 (2001) 1569-1576
or CD version: Stud. Surf. Sci. Catal. 135 (2001) 206, full text CD A10p07.
Marlow, F.; Leike, I.; Weidenthaler, C.; Lehmann, C.W., Wilczok, U.
Mesostructured silica fibres: Ring structures in reciprocal space
Adv. Mater., 13(5) (2001) 307-310.
Schmidt, W., Weidenthaler, C.
Nanosized transition metal spinels with high surface areas from zeolite precursors
Chem. Mater. 13 (2001) 607-612.
Weidenthaler, C., Schmidt, W.
Thermal induced transformations on completely Zn2+ exchanged zeolites A and Y
Z. Kristallogr. 216 (2001) 105-111.
Weidenthaler, C., Schmidt, W.
Thermal stability and thermal transformation of Co2+ and Ni2+ exchanged zeolites A, X, and Y
Chem. Mater. 12 (2000) 3811-3820
Schmidt, W., Weidenthaler, C.
Ion-exchange behavior and stability of heavy metal exchanged zeolites
Applied Mineralogy, Eds: D. Rammlmair, J. Mederer, Th. Oberthür, R.B. Heimann, H.Pentinghaus, Balkema, Rotterdam (2000) 241-244
Weidenthaler, C., Fischer, R.X., Shannon, R.D., Abrams, L., Hewat, A.
Zeolite rho loaded with methylamines. Part III: Trimethylamine loadings
Acta Cryst, B53 (1997) 444-450.
Weidenthaler, C., Fischer, R.X., Shannon, R.D., Abrams, L., Hewat, A.
Zeolite rho loaded with methylamines. Part II: Dimethylamine loadings
Acta Cryst, B53 (1997) 440-443.
Weidenthaler, C., Fischer, R.X., Shannon, R.D., Abrams, L., Hewat, A.
Zeolite rho loaded with methylamines. Part I: Monomethylamine loadings
Acta Cryst, B53 (1997) 429-439.
Weidenthaler, C., Fischer, R.X., Shannon, R.D., Medenbach, O.
Optical investigations of intergrowth effects in the zeolite catalysts ZSM-5 and ZSM-8
J. Phys. Chem. 98 (1994) 12687-12694.
Weidenthaler, C., Fischer, R.X., Shannon, R.D.
The essential identity of the framework structures of ZSM-8 and ZSM-5
Stud.Surf.Sci.Catal, Vol. 84. Zeolites and Related Microporous Materials:State of the Art 1994. J. Weitkamp, H.G. Karge, H. Pfeifer and W. Hölderich (Eds.) (1994)
551-558.
Weidenthaler, C., Fischer, R.X., Shannon, R.D.
Pitfalls in the powder diffraction analysis of zeolites ZSM-5 and ZSM-8
Powder Diffraction 9(3) (1994) 204-212
Weidenthaler, C., Tillmanns, E., Hentschel, G.
Orschallite, Ca3(SO3)2SO4 * 12H2O, a new Calcium-Sulfite-Sulfate-Hydrate Mineral
Mineralogy and Petrology 48 (1993) 167-177.
In situ diffraction experimentation is a powerful tool to obtain deeper insight in the behavior of functional materials, such as porous compounds, nanosized catalysts or metal hydrides. Catalysts may undergo not only changes of the crystal structure or of the microstructure, but also decomposition or segregation reactions may take place. Investigations at non-ambient temperatures are reasonable when growth effects strongly influence the performance of a catalyst, or phase transformation or phase separation start. We have developed sample holders which also enable the investigation of compounds under high hydrogen pressures up to 300 bar. The ammonia decomposition reaction has been chosen as model reaction to investigate catalysts systematically under reaction conditions in a reaction chamber. The analysis of different iron oxide catalysts shows the stepwise reduction of the metal oxides combined with several phase changes and variation of microstructure parameters during reaction. These observations can be directly correlated to variation of the catalytic activity and especially the catalyst stability. (With V. Tagliazzuca, K. Schlichte, U. Holle)
Figure: In situ powder diffraction studies of iron oxides as catalysts for ammonia decomposition
Complex metal hydrides gained much interest as potential solid-state hydrogen storage materials. The preparation of new complex hydrides as potential storage materials, the influence of the preparation strategies on the products formed, as well as structural characterization of these new compounds is in the center of interest. The crystal structures of several new complex aluminum hydrides have been solved directly from powder diffraction data by simulated annealing methods or by the combination of DFT calculations and simulation studies in collaboration with theoretical chemists. Key issue is also to understand all processes involved in the dehydrogenation and rehydrogenation of complex hydrides. Theses steps are monitored by means of in situ X-ray diffraction experiments under non ambient conditions. (With A. Pommerin and M. Felderhoff)
Figure: Crystal structure of NdAlH6 and in situ powder patterns collected during the dehydrogenation.
One important property of solid catalysts and catalysts supports with respect to their catalytic performance is their high specific surface area. However, the morphology of crystals, the coordination number of active sites, the size of the crystalline domains or the presence of distortions, such as stacking faults or dislocations, may also influence the catalytic behavior. The analysis of X-ray powder diffraction profiles allows the evaluation of size domains, size distribution, and the quantification of dislocations or faults present. Whole powder pattern fitting methods have been implemented to investigate the microstructure of nanosized catalysts, such as Au or Co3O4. This allows the correlation of different distortion types with the catalytic properties. (With V. Tagliazucca, R. Güttel, CJ. Jia)
Figure: Microstructure studies of encapsulated gold catalysts for CO oxidation.
For solid catalysts, heterogeneous catalysis mainly takes place on the surface of the catalysts. For this reason, knowledge about the surface chemistry is one of the major keys to understand catalytic reactions. Modification of our high resolution spectrometer allows the investigation of samples during cooling or heating between 100 K and 800 K. Simultaneously, XP spectra can be recorded at non ambient temperatures without further transportation of the sample to the analysis chamber. The instrument is combined with a mass spectrometer for the analysis of reaction gases. As one example the stability of modified zeolite surfaces has been analyzed. (with U. Wilczok, W. Schmidt)