A CBED Study of CuAgSS

1990 ◽  
Vol 48 (2) ◽  
pp. 484-485
Author(s):  
C.L. Baker ◽  
F.J. Lincoln ◽  
A.W.S. Johnson
Keyword(s):  
Room Temperature ◽  
Silver Ions ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Orthorhombic Unit Cell ◽  
X Ray ◽  
Space Groups ◽  
Hexagonal Close Packed ◽  
R Factor ◽  
Starting Model

The room temperature phase of the compound CuAgS occurs in nature as the mineral stromeyerite. Its structure is stable up to approximately 90°C, above this temperature it transforms to a cation disordered structure with copper and silver ions mobile through a hexagonal close packed sulphur lattice. The structure of stromeyerite has been investigated by single crystal X-ray diffraction and was found to have an orthorhombic unit cell with possible space groups Cmcm (63) or Cmc21 (36). The structure was refined in Cmcm but only to an R factor of 0.30. Refinement in Cmc21 was not attempted. The structure is important as a starting model for those of other phases in the system Cu-Ag-S and consequently more precise information was required.Synthetic CuAgS was prepared from the binary sulphides by solid state reaction in vacuo at 300°C for one week. It was then ground to a powder and annealed at 70°C in N2 for a month.

Electron diffraction study of the space group of Bi5Ti3FeO15 multiferroic ceramic

2020 ◽  
Vol 76 (5) ◽  
pp. 454-457
Author(s):  
Ying Zheng ◽  
Xinyan Wu ◽  
Yongcheng Zhang ◽  
Weiquan Shao ◽  
Wanneng Ye
Keyword(s):  
Electron Diffraction ◽  
Room Temperature ◽  
Electron Diffraction Study ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Space Groups ◽  
Phase Compound ◽  
First Time

Bi5Ti3FeO15 (pentabismuth trititanium iron pentadecaoxide), which is a multiferroic four-layer Aurivillius phase compound, has received much attention in recent years. However, three mutually inconsistent orthorhombic space groups, i.e. A21 am, Fmm2 and Pnn2, have been reported for the room-temperature phase of Bi5Ti3FeO15 by X-ray and neutron diffraction investigations. Here, electron diffraction results are presented and discussed for the first time to unambiguously clarify the room-temperature space group of ceramic Bi5Ti3FeO15. It has been found that all the observed reflections from the ceramic agree with those expected in A21 am, while the observed reflections 011, 013 and 015 should be forbidden in the case of Fmm2, and no 107 and 109 reflections were observed although allowed for Pnn2. The present study has demonstrated that the space group of Bi5Ti3FeO15 ceramic is A21 am rather than Fmm2 or Pnn2, an identification that proved to be a challenge for X-ray diffraction. On the basis of the space group A21 am, the lattice parameters of the Bi5Ti3FeO15 ceramic were calculated from its X-ray diffraction data.

Electron Microscope study of commensurate-incommensurate phase transition in BaZnGeO4

1990 ◽  
Vol 48 (4) ◽  
pp. 172-173
Author(s):  
Naoki Yamamoto ◽  
Makoto Kikuchi ◽  
Tooru Atake ◽  
Akihiro Hamano ◽  
Yasutoshi Saito
Keyword(s):  
Phase Transition ◽  
Electron Microscope Study ◽  
Room Temperature ◽  
Hexagonal Lattice ◽  
Ferroelectric Materials ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Periodic Arrays ◽  
Modulation Wave Vector

BaZnGeO4 undergoes many phase transitions from I to V phase. The highest temperature phase I has a BaAl2O4 type structure with a hexagonal lattice. Recent X-ray diffraction study showed that the incommensurate (IC) lattice modulation appears along the c axis in the III and IV phases with a period of about 4c, and a commensurate (C) phase with a modulated period of 4c exists between the III and IV phases in the narrow temperature region (—58°C to —47°C on cooling), called the III' phase. The modulations in the IC phases are considered displacive type, but the detailed structures have not been studied. It is also not clear whether the modulation changes into periodic arrays of discommensurations (DC’s) near the III-III' and IV-V phase transition temperature as found in the ferroelectric materials such as Rb2ZnCl4.At room temperature (III phase) satellite reflections were seen around the fundamental reflections in a diffraction pattern (Fig.1) and they aligned along a certain direction deviated from the c* direction, which indicates that the modulation wave vector q tilts from the c* axis. The tilt angle is about 2 degree at room temperature and depends on temperature.

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

Differences and similarities among hypoxanthinium nitrate hydrate structures

2019 ◽  
Vol 75 (8) ◽  
pp. 1036-1044 ◽  
Author(s):  
Małgorzata Katarzyna Cabaj ◽  
Roman Gajda ◽  
Anna Hoser ◽  
Anna Makal ◽  
Paulina Maria Dominiak
Keyword(s):  
Room Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Acta Cryst ◽  
X Ray ◽  
Nitrate Hydrate ◽  
Different Temperatures ◽  
Lower Temperature ◽  
Low Temperature Phase ◽  
Nitrate Anions

Crystals of hypoxanthinium (6-oxo-1H,7H-purin-9-ium) nitrate hydrates were investigated by means of X-ray diffraction at different temperatures. The data for hypoxanthinium nitrate monohydrate (C5H5N4O+·NO3 −·H2O, Hx1) were collected at 20, 105 and 285 K. The room-temperature phase was reported previously [Schmalle et al. (1990). Acta Cryst. C46, 340–342] and the low-temperature phase has not been investigated yet. The structure underwent a phase transition, which resulted in a change of space group from Pmnb to P21/n at lower temperature and subsequently in nonmerohedral twinning. The structure of hypoxanthinium dinitrate trihydrate (H3O+·C5H5N4O+·2NO3 −·2H2O, Hx2) was determined at 20 and 100 K, and also has not been reported previously. The Hx2 structure consists of two types of layers: the `hypoxanthinium nitrate monohydrate' layers (HX) observed in Hx1 and layers of Zundel complex H3O+·H2O interacting with nitrate anions (OX). The crystal can be considered as a solid solution of two salts, i.e. hypoxanthinium nitrate monohydrate, C5H5N4O+·NO3 −·H2O, and oxonium nitrate monohydrate, H3O+(H2O)·NO3 −.

The structure of monoclinic NaNiO2 as determined by powder X-ray and neutron scattering

1997 ◽  
Vol 12 (4) ◽  
pp. 239-241 ◽  
Author(s):  
Stefan Dick ◽  
Michaela Müller ◽  
Franziska Preissinger ◽  
Thomas Zeiske
Keyword(s):  
Neutron Scattering ◽  
Room Temperature ◽  
Scattering Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Jahn Teller ◽  
Na Ions ◽  
Starting Model

The crystal structure of low temperature NaNiO2 has been refined by Rietveld methods using powder X-ray diffraction and neutron scattering data. The starting model was based on parameters that had been obtained earlier by X-ray film methods. At room temperature NaNiO2 is monoclinic, C2/m, a=0.53192(2), b=0.28451(1), c=0.55826(4) nm, β=110.449(2)°. NaNiO2 has a layered structure. The Ni–O layer is formed by edge sharing of Jahn–Teller elonganted NiO6 octahedra with Ni–O distances of 0.1911(2) nm and 0.2144(4) nm. The Na ions between these layers also exhibit a distorted octahedral coordination with Na–O distances of 0.2328(2) nm and 0.2369(4) nm. The final R values were Rwp=0.069, RI=0.059, Rexp=0.059 for the neutron and Rwp=0.032, RI=0.034, Rexp=0.017 for the X-ray data.

On the tetragonality of the room-temperature ferroelectric phase of barium titanate, BaTiO3

2009 ◽  
Vol 42 (3) ◽  
pp. 480-484 ◽  
Author(s):  
Dean S. Keeble ◽  
Pamela A. Thomas
Keyword(s):  
Barium Titanate ◽  
Diffraction Pattern ◽  
Room Temperature ◽  
Ferroelectric Material ◽  
Tetragonal Symmetry ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Group Assignment ◽  
Growth Method

The room-temperature phase of the important ferroelectric material barium titanate, BaTiO3, was re-investigated by single-crystal X-ray diffraction on a sample grown by the top-seeded solution growth method, with the intention of demonstrating once again that the structure has tetragonal symmetry consistent with the space-group assignmentP4mmand thus resolving recent controversy in the scientific community and literature [Yoshimura, Kojima, Tokunaga, Tozaki & Koganezawa (2006).Phys. Lett. A,353, 250–254; Yoshimura, Morioka, Kojima, Tokunaga, Koganezawa & Tozaki (2007).Phys. Lett. A,367, 394–401]. To this end, the X-ray diffraction pattern of a small (341 µm3) sample of top-seeded solution-grown BaTiO3was measured using an Oxford Diffraction Gemini CCD diffractometer employing Mo Kα radiation and an extended 120 mm sample-to-detector distance. More than 104individual diffraction maxima observed out to a maximum resolution of 0.4 Å were indexed on two tetragonal lattices. These were identical to within the standard deviations on the lattice parameters and were related to each other by a single rotation of 119.7° about the [11\overline1] direction of the first tetragonal lattice (the major twin component), although the actual twinning operation that explains the observed diffraction pattern both qualitatively and quantitatively is shown to be conventional 90° twinning by them[101] operation. Importantly, it is not necessary to invoke either monoclinic symmetry or a coexistence of tetragonal and monoclinic phases to explain the observed diffraction data.

Temperature dependence of the AV3O7 (A = Ca, Sr) structure

2007 ◽  
Vol 63 (6) ◽  
pp. 836-842 ◽  
Author(s):  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth
Keyword(s):  
Single Crystal ◽  
Temperature Dependence ◽  
Crystal Structures ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Space Groups ◽  
Temperature Ranges ◽  
First Time

The V4+ (spin ½) oxovanadates AV3O7 (A = Ca, Sr) were synthesized and studied by means of single-crystal X-ray diffraction. The room-temperature structures of both compounds are orthorhombic and their respective space groups are Pnma and Pmmn. The previously assumed structure of SrV3O7 has been revised and the temperature dependence of both crystal structures in the temperature ranges 297–100 K and 315–100 K, respectively, is discussed for the first time.

Structure refinement of Cu8GeS6 using X-ray diffraction data from a multiple-twinned crystal

1999 ◽  
Vol 55 (5) ◽  
pp. 721-725 ◽  
Author(s):  
Mitsuko Onoda ◽  
Xue-An Chen ◽  
Katsuo Kato ◽  
Akira Sato ◽  
Hiroaki Wada
Keyword(s):  
Diffraction Data ◽  
Room Temperature ◽  
Structure Refinement ◽  
Unit Cell ◽  
Temperature Phase ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Germanium Sulfide ◽  
Symmetry Operations

The structure of the orthorhombic room-temperature phase of Cu8GeS6 (copper germanium sulfide), Mr = 773.27, has been refined on the basis of X-ray diffraction data from a 12-fold twinned crystal applying a six-dimensional twin refinement technique. For 1804 unique reflections measured using Mo Kα radiation, RF was 0.083 with 77 structure parameters and 12 scale factors. The symmetry operations, the unit cell and other crystal data are (0, 0, 0; ½, ½, 0) + x, y, z; y, x, z; ¼ − x, ¾ − y, ½ + z; ¾ − y, ¼ − x, ½ + z; a = b = 9.9073 (3) Å, c = 9.8703 (4) Å, α = β = 90°, γ = 90.642 (4)°; V = 968.7 (1) Å3, Z = 4, Dx  = 5.358 Mg m−3, μ = 21.70 mm−1. The standard setting of the space group and the reduced unit cell are Pmn21; a = 7.0445 (3), b = 6.9661 (3), c = 9.8699 (5) Å; Z = 2.

Crystal structure of Cr2[Ni(CN)4]3·10H2O

1996 ◽  
Vol 11 (4) ◽  
pp. 318-320 ◽  
Author(s):  
A. Ratuszna ◽  
S. Juszczyk ◽  
G. Malłecki
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Rietveld Method ◽  
Unit Cell ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carbon And Nitrogen ◽  
Disordered Structure ◽  
Starting Model

The crystal structure of Cr2[Ni(CN)4]3·10H2O has been determined on X-ray diffraction powder data by means of the Rietveld method. The starting model was based on the isomorphic, disordered structure of Mn3[Co(CN)6]2·12H2O. At room temperature the crystal is cubic, F4¯3m, a=10.097(6) Å, V=1029.4(5) Å3. The structure is disordered and contains 1.33 formula weights per unit cell. The Ni and Cr ions are coordinated by N and C atoms, respectively, forming octahedra linked by CN groups. The water molecules replace partly the chromium, carbon, and nitrogen positions in the crystal. The final R values are: Rwp=0.032 (Rexp=0.023), RB=0.088, and DW-Stat.=1.31 (DWexp=1.8).

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