Powder Diffraction最新文献_第4页

Bimodal microstructural characterization of Si powder using X-ray diffraction: the role of peak shape 利用 X 射线衍射表征硅粉的双峰微结构：峰形的作用

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-06-04 DOI: 10.1017/s0885715624000216

Ashok Bhakar, Himanshu Srivastava, Pragya Tiwari, S. K. Rai

{"title":"Bimodal microstructural characterization of Si powder using X-ray diffraction: the role of peak shape","authors":"Ashok Bhakar, Himanshu Srivastava, Pragya Tiwari, S. K. Rai","doi":"10.1017/s0885715624000216","DOIUrl":"https://doi.org/10.1017/s0885715624000216","url":null,"abstract":"X-ray diffraction (XRD) characterization of Si powder was carried out using synchrotron and laboratory sources. Microstructural (size-strain) analyses of XRD patterns were carried out using the Rietveld refinement method. Experimentally observed super-Lorentzian shapes of the XRD peaks of Si powder were examined using multimodal profile fitting and bimodal model was found to be adequate. The two components obtained using a bimodal approach are referred as narrow and broad profiles based on their estimated relative peak widths. Peak shapes of crystallite size-dependent parts of narrow and broad profiles were found to be almost Gaussian and Lorentzian in nature, respectively. The simultaneous presence of such peak shapes corresponding to a bimodal microstructure is uncommon in literature. Therefore, in order to explore the role of different natures of XRD peak shapes (size dependent) of the bimodal profiles of Si, detailed microstructural analysis was carried out using the complementary method of whole powder pattern modeling (WPPM) and found to be related to the variance of crystallites' size distribution. Additionally, the effect of instrument resolution (laboratory and synchrotron sources) on the microstructural parameters was also studied. Scanning and transmission electron microscopy were used to characterize the morphology of Si powder and correlate with the microstructural findings of XRD methods.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"28 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141257818","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal chemistry and ionic conductivity of garnet-type solid-state electrolyte, Li5-xLa3(NbTa)O12-y 石榴石型固态电解质 Li5-xLa3(NbTa)O12-y 的晶体化学和离子电导率

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-06-03 DOI: 10.1017/s0885715624000290

Amrit P. Kafle, Winnie Wong-Ng, Vladimir Oleshko, Gery R. Stafford, James A. Kaduk, Andreza Eufrasio, Ian L. Pegg, Biprodas Dutta

{"title":"Crystal chemistry and ionic conductivity of garnet-type solid-state electrolyte, Li5-xLa3(NbTa)O12-y","authors":"Amrit P. Kafle, Winnie Wong-Ng, Vladimir Oleshko, Gery R. Stafford, James A. Kaduk, Andreza Eufrasio, Ian L. Pegg, Biprodas Dutta","doi":"10.1017/s0885715624000290","DOIUrl":"https://doi.org/10.1017/s0885715624000290","url":null,"abstract":"Crystal structures, microtopography, morphologies, elemental compositions, and ionic conductivity have been investigated for Li5-xLa3(Nb,Ta)O12-y using X-ray diffraction (XRD), field-emission analytical scanning and transmission electron microscopies (S/TEM), and electrochemical impedance spectroscopy. Using Rietveld refinements with powder XRD patterns, we determined that the number of Li atoms in the formula is less than 5 and that Li5-xLa3(NbTa)O12-y crystallizes in the cubic garnet structure with a space group Ia-3d. Sintering at varying temperatures (750–1000 °C) for 5 h in an ambient atmosphere produced distinct outcomes. Rietveld refinements disclosed that the sample sintered at 1000 °C (Li3.43(2)La3Nb1.07(2)Ta0.93(2)O12-y, a = 12.8361(7) Å, V = 2114.96(3) Å3) exhibited the highest ionic conductivity, while the 850 °C sample had the lowest conductivity, characterized by lower Li concentration and impurity phases (Li(Nb,Ta)3O88, Li2CO3). Analyses, including XRD and electron microscopy, confirmed the 1000 °C sample as a relatively phase pure with enhanced Li content (Li/La = 1.2), larger grains (15 μm), and uniform crystallinity. The 1000 °C sample introduced additional partially filled Li3 (96h) sites, promoting Li migration, and enhancing ionic conductivity. The resulting XRD pattern at 1000 °C has been submitted to the Powder Diffraction File as a reference.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"30 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141257810","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal structure of ribociclib hydrogen succinate, (C23H31N8O)(HC4H4O4) 琥珀酸利福昔布氢(C23H31N8O)(HC4H4O4)的晶体结构

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-27 DOI: 10.1017/s0885715624000277

James A. Kaduk, Anja Dosen, Thomas N. Blanton

{"title":"Crystal structure of ribociclib hydrogen succinate, (C23H31N8O)(HC4H4O4)","authors":"James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000277","DOIUrl":"https://doi.org/10.1017/s0885715624000277","url":null,"abstract":"The crystal structure of ribociclib hydrogen succinate (commonly referred to as ribociclib succinate) has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Ribociclib hydrogen succinate crystallizes in space group P-1 (#2) with a = 6.52215(4), b = 12.67120(16), c = 18.16978(33) Å, α = 74.0855(8), β = 82.0814(4), γ = 88.6943(1)°, V = 1430.112(6) Å3, and Z = 2 at 295 K. The crystal structure consists of alternating layers of cations and anions parallel to the ab-plane. The protonated N in each ribociclib cation acts as a donor in two strong N–H⋯O hydrogen bonds to two different succinate anions. Strong O–H⋯O hydrogen bonds link the hydrogen succinate anions into chains parallel to the a-axis. N–H⋯N hydrogen bonds link the cations into dimers, with a graph set R2,2(8). The result is a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"35 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141171977","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Powder X-ray diffraction of acalabrutinib dihydrate Form III, C26H23N7O2(H2O)2 阿卡布替尼二水物 Form III（C26H23N7O2(H2O)2）的粉末 X 射线衍射

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-27 DOI: 10.1017/s0885715624000265

James A. Kaduk, Megan M. Rost, Anja Dosen, Thomas N. Blanton

引用次数: 0

Crystal structures and X-ray powder diffraction data for AAlGe2O6 synthetic leucite analogs (A = K, Rb, Cs) AAlGe2O6 合成白铁矿类似物（A = K、Rb、Cs）的晶体结构和 X 射线粉末衍射数据

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-16 DOI: 10.1017/s088571562400023x

Anthony M. T. Bell

{"title":"Crystal structures and X-ray powder diffraction data for AAlGe2O6 synthetic leucite analogs (A = K, Rb, Cs)","authors":"Anthony M. T. Bell","doi":"10.1017/s088571562400023x","DOIUrl":"https://doi.org/10.1017/s088571562400023x","url":null,"abstract":"Leucites are tetrahedrally coordinated silicate framework structures with some of the silicon framework cations that are partially replaced by divalent or trivalent cations. These structures have general formulae A2BSi5O12 and ACSi2O6, where A is a monovalent alkali metal cation, B is a divalent cation, and C is a trivalent cation. There are also leucite analogs with analogous tetrahedrally coordinated germanate framework structures. These have general formulae A2BGe5O12 and ACGe2O6. In this paper, the Rietveld refinements of three synthetic Ge-leucite analogs with stoichiometries of AAlGe2O6 (A = K, Rb, Cs) are discussed. KAlGe2O6 is I41/a tetragonal and is isostructural with KAlSi2O6. RbAlGe2O6 and CsAlGe2O6 are $Ibar{4}3d$ cubic and are isostructural with KBSi2O6.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141060512","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal structure of brimonidine hydrogen tartrate, (C11H11BrN5)(HC4H4O6) 酒石酸溴莫尼定晶体结构，(C11H11BrN5)(HC4H4O6)

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-06 DOI: 10.1017/s0885715624000174

James A. Kaduk, Anja Dosen, Thomas N. Blanton

{"title":"Crystal structure of brimonidine hydrogen tartrate, (C11H11BrN5)(HC4H4O6)","authors":"James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000174","DOIUrl":"https://doi.org/10.1017/s0885715624000174","url":null,"abstract":"The crystal structure of brimonidine hydrogen tartrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Brimonidine hydrogen tartrate crystallizes in space group P21 (#4) with a = 7.56032(2), b = 7.35278(2), c = 30.10149(9) Å, β = 90.1992(2)°, V = 1673.312(10) Å3, and Z = 4 at 295 K. The crystal structure consists of alternating layers of cations and anions parallel to the ab-plane. Each of the hydrogen tartrate anions is linked to itself by very strong charge-assisted O–H⋯O hydrogen bonds into chains along the a-axis. Each hydroxyl group of each tartrate acts as a donor in an O–H⋯O or O–H⋯N hydrogen bond. One of these is intramolecular, but the other three are intermolecular. These hydrogen bonds link the hydrogen tartrate anions into layers parallel to the ab-plane and also link the anion–cation layers. The protonated N atoms act as donors in N–H⋯O or N–H⋯N hydrogen bonds to the carboxyl groups of the tartrates and to a ring nitrogen atom. These link the cations and anions, as well as providing cation–cation links. The amino N atoms of the cations form N–H⋯O hydrogen bonds to hydroxyl groups of the anions. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"46 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140883157","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal structure of valbenazine, C24H38N2O4 缬苯嗪（C24H38N2O4）的晶体结构

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-06 DOI: 10.1017/s0885715624000198

Tawnee M. Ens, James A. Kaduk, Megan M. Rost, Anja Dosen, Thomas N. Blanton

引用次数: 0

Powder X-ray diffraction of nintedanib esylate hemihydrate, (C31H33N5O4)(C2H5O3S)(H2O)0.5 宁替尼酯半水合物(C31H33N5O4)(C2H5O3S)(H2O)0.5的粉末 X 射线衍射

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-05-03 DOI: 10.1017/s0885715624000186

Tawnee M. Ens, James A. Kaduk, Anja Dosen, Thomas N. Blanton

{"title":"Powder X-ray diffraction of nintedanib esylate hemihydrate, (C31H33N5O4)(C2H5O3S)(H2O)0.5","authors":"Tawnee M. Ens, James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000186","DOIUrl":"https://doi.org/10.1017/s0885715624000186","url":null,"abstract":"The crystal structure of nintedanib esylate hemihydrate was refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Nintedanib esylate hemihydrate crystallizes in space group P-1 (#2) with a = 11.5137(1), b = 16.3208(4), c = 19.1780(5) Å, α = 69.0259(12), β = 84.4955(8), γ = 89.8319(6)°, V = 3347.57(3) Å3, and Z = 4 at 295 K. Hydrogen bonds are prominent in the crystal structure. The water molecule forms two medium-strength O–H⋯O hydrogen bonds to one of the esylate anions. The protonated nitrogen atom in each cation forms a N–H⋯O hydrogen bond to an esylate anion. The ring N–H groups form strong intramolecular N–H⋯O hydrogen bonds to carbonyl groups. The ring N–H groups form intramolecular N–H⋯O hydrogen bonds to esylate anions. Many C–H⋅⋅⋅O hydrogen bonds (and one C–H⋯N hydrogen bond), with aromatic C–H, methylene groups and methyl groups as donors, are present. The hydrogen bonding patterns of the two cations differ considerably. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"30 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140826711","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

PDF-5+: a comprehensive powder diffraction file™ for materials characterization PDF-5+：用于材料表征的综合粉末衍射文件

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-04-15 DOI: 10.1017/s0885715624000150

Soorya N. Kabekkodu, Anja Dosen, Thomas N. Blanton

{"title":"PDF-5+: a comprehensive powder diffraction file™ for materials characterization","authors":"Soorya N. Kabekkodu, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000150","DOIUrl":"https://doi.org/10.1017/s0885715624000150","url":null,"abstract":"For more than 80 years, the scientific community has extensively used International Centre for Diffraction Data's (ICDD®) Powder Diffraction File (PDF®) for material characterization, including powder X-ray diffraction analysis. Historically, PDF was made available for two major material types: one for inorganic analysis and the other for organic analysis. In the early years of the PDF, this two-material approach was implemented due to limited computer capabilities. With Release 2024, ICDD provides a comprehensive database consisting of the entire PDF in one database called PDF-5+, comprised of more than one million entries (1,061,898). The PDF-5+ with a relational database (RDB) construct houses extensive chemical, physical, bibliographic, and crystallographic data, including atomic coordinates and raw data, enabling qualitative and quantitative phase analysis. This wealth of information in one database is advantageous for phase identification, materials characterization, and several data mining applications in materials science. A database of this size needs rigorous data curation and structural and chemical classifications to optimize pattern search/match and characterization methods. Each entry in the PDF has an editorially assigned quality mark. An editorial comment will describe the reason if an entry does not meet the top-quality mark. The editorial processes of ICDD's quality management system are unique in that they are ISO 9001:2015 certified. Among several classifications implemented in PDF-5+, subfiles (such as Bioactive, Pharmaceuticals, Minerals, etc.) directly impact the search/match in minimizing false positives. Scientists with specific field expertise continuously review these subfiles to maintain their quality. This paper describes the features of PDF with an emphasis on the newly released PDF-5+.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"300 1","pages":""},"PeriodicalIF":0.5,"publicationDate":"2024-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140601681","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal structure of nicarbazin, (C13H10N4O5)(C6H8N2O) 尼卡巴嗪（C13H10N4O5）（C6H8N2O）的晶体结构

IF 0.5 4区材料科学

Powder Diffraction Pub Date : 2024-03-18 DOI: 10.1017/s0885715624000125

James A. Kaduk, A. Dosen, Thomas N. Blanton

引用次数: 0