Structure solution and refinement of stacking-faulted NiCl(OH)

被引:22
作者
Bette, Sebastian [1 ]
Dinnebier, Robert E. [2 ]
Freyer, Daniela [1 ]
机构
[1] TU Bergakad Freiberg, Inst Inorgan Chem, D-09599 Freiberg, Saxony, Germany
[2] Max Planck Inst Solid State Res, D-70569 Stuttgart, Germany
关键词
alkaline nickel(II) chlorides; X-ray powder diffraction; stacking faults; microstructure of layered compounds; X-RAY-DIFFRACTION; LATTICE VIBRATION-SPECTRA; CRYSTAL-STRUCTURE; LAYER STRUCTURES; POWDER-PATTERN; BASIC SALTS; HYDROXIDES; RIETVELD; PHASES; FE;
D O I
10.1107/S1600576715017719
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
Two samples of pure NiCl(OH) were produced by hydrothermal synthesis and characterized by chemical analysis, IR spectroscopy, high-resolution laboratory X-ray powder diffraction and scanning electron microscopy. Layers composed of edge-sharing distorted NiCl6x(OH)(6-6x) octahedra were identified as the main building blocks of the crystal structure. NiCl(OH) is isostructural to CoOOH and crystallizes in space group R (3) over barm [a = 3.2606 (1), c = 17.0062 (9) angstrom]. Each sample exhibits faults in the stacking pattern of the layers. Crystal intergrowth of (A gamma B)(B alpha C)(C beta A) and (A gamma B)(A gamma B) [C6 like, beta-Ni(OH)(2) related] stacked layers was identified as the main feature of the microstructure of NiCl(OH) by DIFFaX simulations. A recursion routine for creating distinct stacking patterns of rigid-body-like layers in real space with distinct faults (global optimization) and a Rietveld-compatible approach (local optimization) was realized and implemented in a macro for the program TOPAS for the first time. This routine enables a recursive creation of supercells containing (A gamma B)(B alpha C)(C beta A), (A gamma B)(A gamma B) and (C beta A)(B alpha C)(A gamma B) stacking patterns, according to user-defined transition probabilities. Hence it is an enhancement of the few previously published Rietveld-compatible approaches. This routine was applied successfully to create and adapt a detailed microstructure model to the measured data of two stacking-faulted NiCl(OH) samples. The obtained microstructure models were supported by high-resolution scanning electron microscopy images.
引用
收藏
页码:1706 / 1718
页数:13
相关论文
共 47 条
[1]  
Andre G., 1888, CR HEBD ACAD SCI, V106, P936
[2]   Layer-stacking irregularities in C36-type Nb-Cr and Ti-Cr Laves phases and their relation with polytypic phase transformations [J].
Aufrecht, J. ;
Baumann, W. ;
Leineweber, A. ;
Duppel, V. ;
Mittemeijer, E. J. .
PHILOSOPHICAL MAGAZINE, 2010, 90 (23) :3149-3175
[3]   LATTICE VIBRATION-SPECTRA .72. OH STRETCHING FREQUENCIES OF SOLID HYDROXIDES - CORRELATION WITH STRUCTURAL AND BONDING DATA [J].
BECKENKAMP, K ;
LUTZ, HD .
JOURNAL OF MOLECULAR STRUCTURE, 1992, 270 :393-405
[4]   A solid solution series of atacamite type Ni2xMg2-2xCl(OH)3 [J].
Bette, Sebastian ;
Dinnebier, Robert E. ;
Roeder, Christian ;
Freyer, Daniela .
JOURNAL OF SOLID STATE CHEMISTRY, 2015, 228 :131-140
[5]   Ni3Cl2.1(OH)3.9•4H2O, the Ni Analogue to Mg3Cl2(OH)4•4H2O [J].
Bette, Sebastian ;
Dinnebier, Robert E. ;
Freyer, Daniela .
INORGANIC CHEMISTRY, 2014, 53 (09) :4316-4324
[6]  
Bruker AXS, 2009, TOP VERS 4 2
[7]   Fundamental parameters line profile fitting in laboratory diffractometers [J].
Cheary, RW ;
Coelho, AA ;
Cline, JP .
JOURNAL OF RESEARCH OF THE NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, 2004, 109 (01) :1-25
[8]   Whole-profile structure solution from powder diffraction data using simulated annealing [J].
Coelho, AA .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2000, 33 (02) :899-908
[9]   Indexing of powder diffraction patterns by iterative use of singular value decomposition [J].
Coelho, AA .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2003, 36 :86-95
[10]   Synthesis and crystal structures of Cd(OH)Cl and Cu(OH)Cl and relationship to brucite type [J].
Cudennec, Y ;
Riou, A ;
Gérault, Y ;
Lecerf, A .
JOURNAL OF SOLID STATE CHEMISTRY, 2000, 151 (02) :308-312