X-Ray Diffraction Studies of Crystallization in Elastomers

1956 ◽  
Vol 29 (2) ◽  
pp. 438-450 ◽  
Author(s):  
Leroy E. Alexander ◽  
Stanley Ohlberg ◽  
G. Russell Taylor

Abstract In general, extension of an elastomer results in a degree of preferred orientation of the molecular chains composing the amorphous phase. Therefore the amorphous fraction of a partially crystalline elastomer must be related to the integrated intensity of the amorphous diffraction halo rather than to the intensity at any one azimuth. A noteworthy exception is natural rubber, for which simple meridional measurements suffice. A Geiger-counter apparatus, with beam monitor and temperature-controlling accessories, is described for making accurate measurements of the x-ray intensities scattered at any azimuth and at small or moderate Bragg angles. Measurements of crystallinity in natural rubber are in essential agreement with the findings of previous workers. When polybutadiene is extended at room temperature, molecular orientation occurs, but little if any crystallization. Measurements at lowered temperatures show that the crystalline fraction becomes appreciable at about 0° C and that it increases with further reduction of temperature and with increasing extension ratio. Preferred orientation of the crystalline regions in extended polybutadiene has been measured quantitatively with the object of providing jointly with birefringence measurements a value of the birefringence of a single crystal of polybutadiene.

Nanomaterials ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 1023 ◽  
Author(s):  
Ashish Chhaganlal Gandhi ◽  
Chia-Liang Cheng ◽  
Sheng Yun Wu

We report the synthesis of room temperature (RT) stabilized γ–Bi2O3 nanoparticles (NPs) at the expense of metallic Bi NPs through annealing in an ambient atmosphere. RT stability of the metastable γ–Bi2O3 NPs is confirmed using synchrotron radiation powder X-ray diffraction and Raman spectroscopy. γ–Bi2O3 NPs exhibited a strong red-band emission peaking at ~701 nm, covering 81% integrated intensity of photoluminescence spectra. Our findings suggest that the RT stabilization and enhanced red-band emission of γ‒Bi2O3 is mediated by excess oxygen ion vacancies generated at the octahedral O(2) sites during the annealing process.


2013 ◽  
Vol 749 ◽  
pp. 643-647 ◽  
Author(s):  
Lei Li ◽  
Ya Feng Lu ◽  
Wen Xue Li ◽  
Li Ying Zeng ◽  
Yi Yang ◽  
...  

Ti-6Al-4V films were deposited by direct-current magnetron sputtering at different substrate temperatures. The structure and the surface morphology of the films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The hardness and elastic moduli of Ti-6Al-4V films were measured by nanoindentation test. The results showed that the phase direction of the films deposited at room temperature was (102) orientation, and turned to almost complete (002) preferred orientation at 300°C. For a higher temperature of 500°C, the preferred orientation of the film disappeared and presented a random grain orientation. The hardness and elastic moduli of Ti-6Al-4V films obviously showed the dependence on the temperature. The relationships among temperature, microstructure and mechanical properties of Ti-6Al-4V films were discussed in this paper.


2014 ◽  
Vol 893 ◽  
pp. 69-74
Author(s):  
Johar Banjuraizah ◽  
Mohd. Haziq Che Ani ◽  
A.R. Mohamed

Transition metal oxide-doped CCTO (CaCu3Ti4O12) ceramics were prepared by a conventional solgel synthesis method and the effects of pure CCTO and CCTO doped with Mn, Fe, Co, Ni to the crystal structure, microstructures and dielectrical properties of samples were investigated. The phase composition and microstructure were studied by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD analysis reveals that all samples exhibited multiphases with the pseudo-perovskite cubic CCTO phase with space group Im-3 as the main phase in undoped and doped CCTO samples. Peaks of monoclinic CuO and peroveskite CaTiO3 could also be seen in all samples which indicate that solid solution of CuO in CaTiO3 lattice was incomplete.SEM results show that doping effectively enhanced densification. SEM micrographs also suggested that the morphologies of doped CCTO ceramics had showed a matrix consisting of large grains wherein the small grains were embedded between the larger grains. Dielectric properties of pure and doped CCTO were investigated in a broad frequency range of the dielectric constant reached a value as high as εr = 29.4 at room temperature for CCTO doped with Ni at frequency (1000 Hz). Besides the sintering conditions, the microstructure and the dielectric properties of the CCTO are strongly influenced by type of doping elements.


2008 ◽  
Vol 42 (1) ◽  
pp. 93-100 ◽  
Author(s):  
Stéphanie Albert ◽  
Julien Haines ◽  
Dominique Granier ◽  
Annie Pradel ◽  
Michel Ribes

The effect of pressure on both the structure and the electrical conductivity of the superionic Ag7GeSe5I phase has been studied at room temperature (i) by powder X-ray diffraction from 0.1 MPa to 10 GPa, (ii) by single-crystal X-ray diffraction from 0.1 MPa to 2 GPa and (iii) by impedance spectroscopy from 0.1 MPa to 1.5 GPa. The decrease in conductivity of about one order of magnitude when the pressure increases up to 1.5 GPa can be explained by compression of the cell. For a pressure increase up to 10 GPa, compression of the cell is about 6% in volume. The compressibility of the cell affects mainly two sites,i.e.I and one of the two Ag sites. Both sites have a very largeBisothat increases even further with pressure, to reach a value close to 11.5 Å2at 1.5 GPa. The occupancy of both Ag sites changes with pressure and becomes similar above 0.8 GPa. On the whole, it appears that the conduction mechanism is affected by pressure. While the conduction pathway is not changed, the limiting jump for ionic diffusion changes from an intercluster jump with a pseudo-potential barrier of about 257 meV at ambient pressure to an indirect jump with a pseudo-potential value of 240 meV at 1.8 GPa.


Author(s):  
C. Wolpers ◽  
R. Blaschke

Scanning microscopy was used to study the surface of human gallstones and the surface of fractures. The specimens were obtained by operation, washed with water, dried at room temperature and shadowcasted with carbon and aluminum. Most of the specimens belong to patients from a series of X-ray follow-up study, examined during the last twenty years. So it was possible to evaluate approximately the age of these gallstones and to get information on the intensity of growing and solving.Cholesterol, a group of bile pigment substances and different salts of calcium, are the main components of human gallstones. By X-ray diffraction technique, infra-red spectroscopy and by chemical analysis it was demonstrated that all three components can be found in any gallstone. In the presence of water cholesterol crystallizes in pane-like plates of the triclinic crystal system.


Author(s):  
Naoki Yamamoto ◽  
Makoto Kikuchi ◽  
Tooru Atake ◽  
Akihiro Hamano ◽  
Yasutoshi Saito

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.


2018 ◽  
Author(s):  
Katherine Marczenko ◽  
James Goettel ◽  
Gary Schrobilgen

Oxygen coordination to the Xe(VI) atom of XeO<sub>3</sub> was observed in its adducts with triphenylphosphine oxide, dimethylsulfoxide, pyridine-N-oxide, and acetone. The crystalline adducts were characterized by low-temperature, single-crystal X-ray diffraction and Raman spectroscopy. Unlike solid XeO<sub>3</sub>, which detonates when mechanically or thermally shocked, the solid [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub>, [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub>,<sub> </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> adducts are insensitive to mechanical shock, but undergo rapid deflagration when ignited by a flame. Both [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3 </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> are air-stable whereas [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> slowly decomposes over several days and [(CH<sub>3</sub>)<sub>2</sub>CO]<sub>3</sub>XeO<sub>3</sub> undergoes adduct dissociation at room temperature. The xenon coordination sphere of [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub> is a distorted square pyramid which provides the first example of a five-coordinate XeO<sub>3</sub> adduct. The xenon coordination spheres of the remaining adducts are distorted octahedra comprised of three Xe---O secondary contacts that are approximately trans to the primary Xe–O bonds of XeO<sub>3</sub>. Quantum-chemical calculations were used to assess the Xe---O adduct bonds, which are predominantly electrostatic σ-hole bonds between the nucleophilic oxygen atoms of the bases and the σ-holes of the xenon atoms.


2019 ◽  
Author(s):  
Chem Int

Optically transparent single crystals of potassium acid phthalate (KAP, 0.5 g) 0.05 g and 0.1 g (1 and 2 mol %) trytophan were grown in aqueous solution by slow evaporation technique at room temperature. Single crystal X- ray diffraction analysis confirmed the changes in the lattice parameters of the doped crystals. The presence of functional groups in the crystal lattice has been determined qualitatively by FTIR analysis. Optical absorption studies revealed that the doped crystals possess very low absorption in the entire visible region. The dielectric constant has been studied as a function of frequency for the doped crystals. The thermal stability was evaluated by TG-DSC analysis.


1988 ◽  
Vol 133 ◽  
Author(s):  
K. S. Kumar ◽  
S. K. Mannan

ABSTRACTThe mechanical alloying behavior of elemental powders in the Nb-Si, Ta-Si, and Nb-Ta-Si systems was examined via X-ray diffraction. The line compounds NbSi2 and TaSi2 form as crystalline compounds rather than amorphous products, but Nb5Si3 and Ta5Si3, although chemically analogous, respond very differently to mechanical milling. The Ta5Si3 composition goes directly from elemental powders to an amorphous product, whereas Nb5Si3 forms as a crystalline compound. The Nb5Si3 compound consists of both the tetragonal room-temperature α phase (c/a = 1.8) and the tetragonal high-temperature β phase (c/a = 0.5). Substituting increasing amounts of Ta for Nb in Nb5Si3 initially stabilizes the α-Nb5Si3 structure preferentially, and subsequently inhibits the formation of a crystalline compound.


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