Rotational Polymorphism of Methyl-Substituted Ammonium Perchlorates

1965 ◽  
Vol 9 ◽  
pp. 170-189 ◽  
Author(s):  
M. Stammler ◽  
R. Bruenner ◽  
W. Schmidt ◽  
D. Orcutt
Keyword(s):  
Phase Transition ◽  
Ammonium Perchlorate ◽  
Room Temperature ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Analysis Techniques ◽  
Cell Dimensions ◽  
Thermal Analysis Techniques ◽  
Space Requirements

AbstractThe thermal transformations which take place in solid methyl-substituted ammonium perchlorates have been studied using high-temperature X-ray diffraction and differential thermal analysis techniques. In the temperature range from 20°C to their decomposition temperature (above 300°C), ammonium perchlorate and tetramethyl ammonium perchlorate undergo only one enantiomorphic phase transition, namely at 240 and 340°C (with decomposition), respectively. This I—II transition is ascribed to the beginning of the free rotation of the ClO4− ions. The rotation of the cations, however, begins below room temperature. If the symmetry of the cation is lowered by having both methyl groups and hydrogens arranged around the nitrogen (as in monomethyl, dimethyl, and trimethyl ammonium perchlorates), there is an additional enantiomorphic phase transition. This I—II transformation is ascribed to the rotation of the cations which have, in the partially substituted ions, two sets of non-equivalent symmetry axes (different moments of inertia). The temperatures of transformation are discussed in terms of the space requirements for rotation. Symmetries and cell dimensions of some modifications were determined.

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.

scholarly journals Structural Formation of UHMWPE Film Tracked by Real-Time Retardation Measurements during Uniaxial/Biaxial Stretching

Materials ◽  
2018 ◽  
Vol 11 (11) ◽  
pp. 2292 ◽  
Author(s):  
Yoshinori Hashimoto ◽  
Shotaro Nishitsuji ◽  
Takashi Kurose ◽  
Hiroshi Ito
Keyword(s):  
Tensile Testing ◽  
X Ray Diffraction ◽  
Structural Formation ◽  
X Ray ◽  
Amorphous Phases ◽  
Analysis Techniques ◽  
Biaxial Stretching ◽  
Thermal Analysis Techniques ◽  
Ultra High Molecular Weight ◽  
Order Structures

This work reports on an experimental study of the stretching of ultra-high molecular weight polyethylene (UHMWPE) film in various uniaxial/biaxial stretching modes at various temperatures and stretching speeds. We examined the stress-birefringence relationship as a stress-optical rule (SOR) under uniaxial stretching and evaluated the stress-optical coefficient (SOC). Wide-angle X-ray diffraction (WAXD) measurements were applied to evaluate the contribution to birefringence of the crystalline and amorphous phases and to characterize stretching modes. In simultaneous biaxial stretching, the melting temperature (Tm) proved critical to structural formation. We applied thermal analysis techniques and tensile testing to evaluate higher order structures after each stretching mode.

Synthesis, Crystal Structure and Magnetic Properties of a Copper(II) p-Formylbenzoate Complex

2012 ◽  
Vol 67 (11) ◽  
pp. 1185-1190 ◽  
Author(s):  
Jin-Li Qi ◽  
Wei Xu ◽  
Yue-Qing Zheng
Keyword(s):  
Room Temperature ◽  
Magnetic Measurements ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Ferromagnetic Interactions ◽  
Aqueous Conditions ◽  
Discrete Complex

A new Cu(II) complex was prepared at room temperature from the reaction of p-formylbenzoic acid, phenanthroline, CuCl2⋅2H2O, and NaOH under ethanolic aqueous conditions. The complex has been characterized by X-ray diffraction, IR spectroscopy, TG-DTA analyses, and magnetic measurements. Single-crystal X-ray diffraction analysis indicated that the complex crystallizes in the triclinic space group P1̄ with the cell dimensions a=7.875(2), b=10.724(2), c=15.317(3) Å , α =102.65(3), β =93.71(3), γ =107:64(3)°. The Cu atoms are in the environment of distorted CuN2O3 tetragonal pyramids. These discrete complex molecules are packed through intermolecular π...π-stacking interactions and C-H...O hydrogen bonds forming a supramolecular structure. The title complex obeys the Curie-Weiss law with a Curie constant C=0:53 cm3 K mol-1 and a Weiss constant θ = -0:27 K. The shape of the xmT curve is characteristic of weak ferromagnetic interactions between the Cu(II) centers from 300 to 7 K, while there are weak antiferromagnetic interactions below 7 K.

Laser Ablation Synthesis of Ceramic Powders

1990 ◽  
Vol 201 ◽  
Author(s):  
W. G. Fahrenholtz ◽  
S. R. Foltyn ◽  
K. C. Ott ◽  
M. Chadwick ◽  
D. M. Smith
Keyword(s):  
Thermal Analysis ◽  
Laser Ablation ◽  
Aluminum Oxide ◽  
Fine Powder ◽  
X Ray Diffraction ◽  
Ceramic Powders ◽  
X Ray ◽  
Analysis Techniques ◽  
Aluminum Metal ◽  
Thermal Analysis Techniques

AbstractA pulsed excimer laser was used to ablate aluminum metal into an oxygen-containing atmosphere. The resulting fine powder was collected on a 0.1 μm filter and analyzed to determine structure and composition. Using a combination of TEM, EELS, and thermal analysis techniques, the product was found to be amorphous aluminum oxide, Al2O3. The morphology of the powders was investigated using SEM, TEM, and surface area measurements. The resulting powder was crystallized and examined by x-ray diffraction.

Structure and phase transition of the Se-rich variety of antimonpearceite, [(Ag,Cu)6(Sb,As)2(S,Se)7][Ag9Cu(S,Se)2Se2]

2006 ◽  
Vol 62 (5) ◽  
pp. 768-774 ◽  
Author(s):  
Michel Evain ◽  
Luca Bindi ◽  
Silvio Menchetti
Keyword(s):  
Phase Transition ◽  
Room Temperature ◽  
Atomic Displacement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Diffusion ◽  
Ionic Conducting ◽  
Local Arrangement ◽  
Diffusion Paths ◽  
Linear Coordination

The crystal structure of a Se-rich antimonpearceite has been solved and refined by means of X-ray diffraction data collected at temperatures above (room temperature) and below (120 K) an ionic conductivity-induced phase transition. Both structure arrangements consist of the stacking of [(Ag,Cu)6(Sb,As)2(S,Se)7]2− A (A′) and [Ag9Cu(S,Se)2Se2]2+ B (B′) module layers in which Sb forms isolated SbS3 pyramids typically occurring in sulfosalts; copper links two S atoms in a linear coordination, and silver occupies sites with coordination ranging from quasi-linear to almost tetrahedral. In the ionic-conducting form, at room temperature, the silver d 10 ions are found in the B (B′) module layer along two-dimensional diffusion paths and their electron densities described by means of a combination of a Gram–Charlier development of the atomic displacement factors and a split-atom model. The structure resembles that of pearceite, except for the presence of both specific (Se) and mixed (S, Se) sites. In the low-temperature `ordered' phase at 120 K the silver d 10 ions of the B (B′) module layer are located in well defined sites with mixed S—Se coordination ranging from quasi-linear to almost tetrahedral. The structure is then similar to that of 222-pearceite but with major differences, specifically its cell metric, symmetry and local arrangement in the B (B′) module layer.

Kinetic Study on the Formation of the Aragonite-Like Phase Ba(CuOx)1-Y(CO3)y

1995 ◽  
Vol 398 ◽  
Author(s):  
A. Tomasi ◽  
E. Galvanetto ◽  
F.C. Matacotta ◽  
P. Nozar ◽  
P. Scardi ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
High Resolution Electron Microscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Analysis Techniques ◽  
Formation Kinetics ◽  
Resolution Electron ◽  
Thermal Analysis Techniques ◽  
Kinetics Of

ABSTRACTA systematic study on phase formation and stabilisation in the Ba-Cu-C-O system in the temperature range 20-500°C, under various atmospheres, by traditional thermal analysis techniques, high temperature X-ray diffraction and high resolution electron microscopy, has permitted to identify and characterise the formation kinetics of a new copper containing phase isomorphic to γ-BaCO3.

Effect of pressure on phase transitions in K1−xNaxMnF3(x = 0.04)

1999 ◽  
Vol 32 (2) ◽  
pp. 174-177 ◽  
Author(s):  
S. Åsbrink ◽  
A. Waśkowska ◽  
H. G. Krane ◽  
L. Gerward ◽  
J. Staun Olsen
Keyword(s):  
Phase Transition ◽  
Parent Compound ◽  
X Ray Diffraction ◽  
X Ray ◽  
Effect Of Pressure ◽  
Cell Dimensions ◽  
Main Effect ◽  
Diamond Anvil ◽  
Na Ions ◽  
Unit Cell Dimensions

The pressure-induced phase transition sequence in the title compound, potassium sodium fluoromanganate, has been investigated by single-crystal X-ray diffraction using synchrotron radiation and a diamond anvil pressure cell. Na^+ ions at 4% of the K^+ sites shift the ferrodistortive phase transition to the lower pressure P_{c1} of 2.75 (5) GPa compared to 3.12 GPa in the parent compound KMnF3. The transition is illustrated by the critical behaviour of the unit-cell dimensions, the pressure-dependent evolution of the MnF_6 ^- octahedral rotation and related macroscopic spontaneous strain. As far as precision of the present experiment allows, the observations show that the 4% of Na^+ admixture at the K^+ sites does not substantially change the nature of the transition at P_{c1}. The main effect of pressure is to stabilize the tetragonal phase II. The expected further evolution of the MnF_6 ^- octahedral tiltings, leading to the orthorhombic and monoclinic phases, has not been observed up to 8.33 GPa.

scholarly journals Stable Organic-Inorganic Hybrid Bismuth-Halide Monocrystalline Compounds With Adjustable Optoelectronic Properties

2021 ◽  
Author(s):  
Xinru Hu ◽  
Jilin Wang ◽  
Jian He ◽  
Guoyuan Zheng ◽  
Disheng Yao ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Room Temperature ◽  
Diffuse Reflectance ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
Good Thermal Stability ◽  
Chemical Groups ◽  
Thermal Stability Of

Abstract Two kinds of novel organic-inorganic bismuth-halide hybrid monocrystalline compounds (C6H5CH2NH3)2BiCl5 and (C6H5CH2NH3)BiI4 were synthesized and characterized. The crystal structure, intermolecular interaction, morphology, chemical groups and bonds, optical and thermal stability of the samples were systematically investigated through single crystal X-ray diffraction, Hirshfeld surface analysis, SEM, FTIR, TG and UV-vis diffuse reflectance spectra. The results indicated that (C6H5CH2NH3)2BiCl5 and (C6H5CH2NH3)BiI4 crystals displayed a monoclinic system with the space group P21/c and P21/n at room temperature, respectively. These materials showed strong absorption in the ultraviolet and visible light regions, resulting in very low Eg, which could be continuously adjustable from 1.67 eV to 3.21 eV by changing the halogen ratio. In addition, these hybrid materials also exhibited good thermal stability. The decomposition temperature of (C6H5CH2NH3)2BiCl5 and (C6H5CH2NH3)BiI4 were 260℃ and 300℃ respectively. Therefore, these organic-inorganic bismuth-halide hybrid compounds have excellent development potential in the field of solar cell research.

scholarly journals Structural Study of δ-AlOOH Up to 29 GPa

Minerals ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1055
Author(s):  
Dariia Simonova ◽  
Elena Bykova ◽  
Maxim Bykov ◽  
Takaaki Kawazoe ◽  
Arkadiy Simonov ◽  
...  
Keyword(s):  
Phase Transition ◽  
Synchrotron Radiation ◽  
Equation Of State ◽  
Room Temperature ◽  
Diamond Anvil Cell ◽  
Volume Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diamond Anvil ◽  
Murnaghan Equation

A structure and equation of the state of δ-AlOOH has been studied at room temperature, up to 29.35 GPa, by means of single crystal X-ray diffraction in a diamond anvil cell using synchrotron radiation. Above ~10 GPa, we observed a phase transition with symmetry changes from P21nm to Pnnm. Pressure-volume data were fitted with the second order Birch-Murnaghan equation of state and showed that, at the phase transition, the bulk modulus (K0) of the calculated wrt 0 pressure increases from 142(5) to 216(5) GPa.

Temperature Dependent Structural Studies of K- and RB- Doped C60

1992 ◽  
Vol 270 ◽  
Author(s):  
Otto Zhou ◽  
Qing Zhu ◽  
Gavin B.M. Vaughan ◽  
John E. Fischer ◽  
Paul A. Heiney ◽  
...  
Keyword(s):  
Room Temperature ◽  
The Body ◽  
Face Centered Cubic ◽  
Temperature Dependent ◽  
X Ray ◽  
Analysis Techniques ◽  
Temperature Range ◽  
Face Centered ◽  
Thermal Analysis Techniques ◽  
Bcc Phase

ABSTRACTThe temperature dependent structural evolutions of RbxC60 (x = 3, 5, 6) and K4C60 were studied using both in-house andsynchrotron x-ray powder diffraction and thermal analysis techniques over a temperature range of 10K - 673K. The superconducting face centered-cubic (fcc) Rb3C60 and the body centered-tetragonal (bct) M4C60(M = K, Rb) phases are found to be line compounds in this temperature range, while the body centered-cubic (bcc) phase forms a solid solution in which the solubility of vacant M sites increases with temperature. The orientation of the C60 molecules in the K4C60 phase was analyzed. A crystalline fcc Rb1C60 phase is stable only above room temperature.

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