Pub Date : 2007-11-01DOI: 10.1524/ZKSU.2007.2007.SUPPL_26.125
L. Lutterotti, M. Bortolotti, G. Ischia, I. Lonardelli, H. Wenk
The procedure to perform Rietveld texture analysis from diffraction images collected with CCDs or image plates is shown. In some cases only one transmission image may be sufficient to obtain an Orientation Distribution Function (ODF) if a sufficient number of peaks are included. The images are transformed in spectra and analyzed using the Maud Rietveld program containing some recently developed texture model well suited for this kind of analysis. In this work we will present the results obtained using a custom laboratory image plate camera developed for texture analysis. The instrument may work with a curve image plate detector in reflection condition or with a flat detector in transmission. The reflection condition is used mainly for ceramics and metal-alloys and the transmission mode for polymers and fibres. We will show how with the combination of such camera and the Rietveld Texture Analysis method we were able to analyze the ODF of the martensitic phase of Shape Memory Alloy (monoclinic NiTi SMA) as well as to obtain the quantitative texture of low symmetry polymers in fibre form.
{"title":"Rietveld texture analysis from diffraction images","authors":"L. Lutterotti, M. Bortolotti, G. Ischia, I. Lonardelli, H. Wenk","doi":"10.1524/ZKSU.2007.2007.SUPPL_26.125","DOIUrl":"https://doi.org/10.1524/ZKSU.2007.2007.SUPPL_26.125","url":null,"abstract":"The procedure to perform Rietveld texture analysis from diffraction images collected with CCDs or image plates is shown. In some cases only one transmission image may be sufficient to obtain an Orientation Distribution Function (ODF) if a sufficient number of peaks are included. The images are transformed in spectra and analyzed using the Maud Rietveld program containing some recently developed texture model well suited for this kind of analysis. In this work we will present the results obtained using a custom laboratory image plate camera developed for texture analysis. The instrument may work with a curve image plate detector in reflection condition or with a flat detector in transmission. The reflection condition is used mainly for ceramics and metal-alloys and the transmission mode for polymers and fibres. We will show how with the combination of such camera and the Rietveld Texture Analysis method we were able to analyze the ODF of the martensitic phase of Shape Memory Alloy (monoclinic NiTi SMA) as well as to obtain the quantitative texture of low symmetry polymers in fibre form.","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81802434","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKRI.2007.2007.SUPPL_26.261
K. Pantleon, M. Somers
. The microstructure evolution in copper electrodeposits at room temperature (self-annealing) was investigated by means of X-ray diffraction analysis and simultaneous measurement of the electrical resistivity as a function of time. In-situ studies were started immediately after electrodeposition and continued with an unprecedented time resolution until sta-tionary values of the recorded data were obtained. Independent of the copper layer thickness, the as-deposited microstructure consisted of nanocrystalline grains with orientation dependent crystallite sizes. Orientation dependent grain growth, crystallographic texture changes by multiple twinning and a decrease of the electrical resistivity occurred as a function of time at room temperature. The kinetics of self-annealing is strongly affected by the layer thickness: the thinner the layer the slower is the microstructure evolution and self-annealing is sup-pressed completely for a thin layer of 0.4 μm.
{"title":"Evolution of the microstructure in nanocrystalline copper electrodeposits during room temperature storage","authors":"K. Pantleon, M. Somers","doi":"10.1524/ZKRI.2007.2007.SUPPL_26.261","DOIUrl":"https://doi.org/10.1524/ZKRI.2007.2007.SUPPL_26.261","url":null,"abstract":". The microstructure evolution in copper electrodeposits at room temperature (self-annealing) was investigated by means of X-ray diffraction analysis and simultaneous measurement of the electrical resistivity as a function of time. In-situ studies were started immediately after electrodeposition and continued with an unprecedented time resolution until sta-tionary values of the recorded data were obtained. Independent of the copper layer thickness, the as-deposited microstructure consisted of nanocrystalline grains with orientation dependent crystallite sizes. Orientation dependent grain growth, crystallographic texture changes by multiple twinning and a decrease of the electrical resistivity occurred as a function of time at room temperature. The kinetics of self-annealing is strongly affected by the layer thickness: the thinner the layer the slower is the microstructure evolution and self-annealing is sup-pressed completely for a thin layer of 0.4 μm.","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90343058","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKSU.2007.2007.SUPPL_26.247
R. Kužel, L. Nichtová, Z. Matěj, D. Herman, J. Sícha, J. Musil
{"title":"Study of crystallization of magnetron sputtered TiO2thin films by X-ray scattering","authors":"R. Kužel, L. Nichtová, Z. Matěj, D. Herman, J. Sícha, J. Musil","doi":"10.1524/ZKSU.2007.2007.SUPPL_26.247","DOIUrl":"https://doi.org/10.1524/ZKSU.2007.2007.SUPPL_26.247","url":null,"abstract":"","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77581807","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKRI.2007.2007.SUPPL_26.581
Anne Carton, A. Mesbah, M. François, P. Rabu
{"title":"Structures of transition metal hydroxyterephthalates","authors":"Anne Carton, A. Mesbah, M. François, P. Rabu","doi":"10.1524/ZKRI.2007.2007.SUPPL_26.581","DOIUrl":"https://doi.org/10.1524/ZKRI.2007.2007.SUPPL_26.581","url":null,"abstract":"","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84425303","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKSU.2007.2007.SUPPL_26.537
J. G. Carrió, S. B. Faldini, L. Miranda, P. K. Kiyohara, L. G. Silva, A. H. Munhoz
{"title":"Structural analysis by the Rietveld method and SEM of irradiated pseudoboehmite and Al2O3","authors":"J. G. Carrió, S. B. Faldini, L. Miranda, P. K. Kiyohara, L. G. Silva, A. H. Munhoz","doi":"10.1524/ZKSU.2007.2007.SUPPL_26.537","DOIUrl":"https://doi.org/10.1524/ZKSU.2007.2007.SUPPL_26.537","url":null,"abstract":"","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86896709","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKRI.2007.2007.SUPPL_26.549
P. Pardo, J. Bastida, M. Kojdecki, R. Ibáñez, M. Zbik
The influence of dry milling on the crystalline microstructure of two kaolinites of different origins is studied by X-ray diffraction (XRD) and by analysing field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) images. Two methods of XRD microstructural analysis are used: the Voigt function and the Warren- Averbach methods; good linear correlation between average apparent crystallite size estimated by both methods is found.
{"title":"X-ray diffraction line broadening in dry grinding of kaolinite","authors":"P. Pardo, J. Bastida, M. Kojdecki, R. Ibáñez, M. Zbik","doi":"10.1524/ZKRI.2007.2007.SUPPL_26.549","DOIUrl":"https://doi.org/10.1524/ZKRI.2007.2007.SUPPL_26.549","url":null,"abstract":"The influence of dry milling on the crystalline microstructure of two kaolinites of different origins is studied by X-ray diffraction (XRD) and by analysing field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) images. Two methods of XRD microstructural analysis are used: the Voigt function and the Warren- Averbach methods; good linear correlation between average apparent crystallite size estimated by both methods is found.","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89449429","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKRI.2007.2007.SUPPL_26.525
E. Neubauer, P. Angerer
{"title":"Phase composition and thermal expansion behaviour of zirconium tungstate prepared by rapid sintering","authors":"E. Neubauer, P. Angerer","doi":"10.1524/ZKRI.2007.2007.SUPPL_26.525","DOIUrl":"https://doi.org/10.1524/ZKRI.2007.2007.SUPPL_26.525","url":null,"abstract":"","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75759025","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKSU.2007.2007.SUPPL_26.45
K. Harris
Techniques for structure determination of organic materials from powder X-ray diffraction data are now applied widely in many different fields of scientific research. Nevertheless, structure determination from powder diffraction data is far from an automatic, "black-box" process, and it is essential that the results obtained from such analysis are subjected to adequate scrutiny before they are assigned to be valid and correct. Here we consider two aspects of validation relevant to this field: (i) validation of the structural model used in direct-space structure solution calculations, and (ii) validation of the final structure obtained from Rietveld refinement. The advantages of exploiting information obtained from other experimental and computational techniques are emphasized.
{"title":"Aspects of validation in the structure determination of organic materials from powder X-ray diffraction data","authors":"K. Harris","doi":"10.1524/ZKSU.2007.2007.SUPPL_26.45","DOIUrl":"https://doi.org/10.1524/ZKSU.2007.2007.SUPPL_26.45","url":null,"abstract":"Techniques for structure determination of organic materials from powder X-ray \u0000diffraction data are now applied widely in many different fields of scientific research. Nevertheless, \u0000structure determination from powder diffraction data is far from an automatic, \u0000\"black-box\" process, and it is essential that the results obtained from such analysis are subjected \u0000to adequate scrutiny before they are assigned to be valid and correct. Here we consider \u0000two aspects of validation relevant to this field: (i) validation of the structural model used in \u0000direct-space structure solution calculations, and (ii) validation of the final structure obtained \u0000from Rietveld refinement. The advantages of exploiting information obtained from other \u0000experimental and computational techniques are emphasized.","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74882089","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2007-11-01DOI: 10.1524/ZKRI.2007.2007.SUPPL_26.147
M. Wohlschlögel, T. Schülli, G. Maier, U. Welzel, E. Mittemeijer
{"title":"Characterization of a high-performance laboratory parallel-beam diffractometer-bridging the gap to the synchrotron","authors":"M. Wohlschlögel, T. Schülli, G. Maier, U. Welzel, E. Mittemeijer","doi":"10.1524/ZKRI.2007.2007.SUPPL_26.147","DOIUrl":"https://doi.org/10.1524/ZKRI.2007.2007.SUPPL_26.147","url":null,"abstract":"","PeriodicalId":23897,"journal":{"name":"Zeitschrift Fur Kristallographie","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2007-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77747970","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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