scholarly journals Формирование и трансформация моноклинной и орторомбической фаз в реакторных порошках сверхвысокомолекулярного полиэтилена

2018 ◽  
Vol 60 (9) ◽  
pp. 1847
Author(s):  
М.В. Байдакова ◽  
П.В. Дороватовский ◽  
Я.В. Зубавичус ◽  
Е.М. Иванькова ◽  
С.С. Иванчев ◽  
...  

AbstractUsing powerful synchrotron X-ray radiation of the beamline “Belok” operated by the National Research Center “Kurchatov Institute,” we perform X-ray diffraction (XRD) study of an intact, virgin (not subjected to any external mechanical loads) particle isolated from reactor powder of ultrahigh molecular weight polyethylene. Along with the peaks originating from the orthorhombic phase, we detect the peaks characteristic of the monoclinic phase that is stable only under mechanical stress, suggesting that the mechanical stress that leads to the formation of the monoclinic phase and persists at room temperature develops during the polymer synthesis. The monoclinic phase gradually disappears when the particle is heated stepwise in increments of 5 K, and its peaks become undetectable when the temperature reaches 340 K. We contrast the results obtained for the phase composition of the virgin particle to those for a tablet prepared by compaction of the same reactor powder at room temperature. XRD analyses of the tablet were performed on D2 Phaser (Bruker) instrument. The monoclinic phase that originates during the polymer synthesis and the one that forms in the tablet during compaction have different parameters. We discuss the mechanisms by which these two different monoclinic phases originate during the processes involved.

2019 ◽  
Vol 61 (10) ◽  
pp. 1965 ◽  
Author(s):  
В.М. Егоров ◽  
В.А. Марихин ◽  
Л.П. Мясникова ◽  
А.К. Борисов ◽  
Е.М. Иванькова ◽  
...  

AbstractWe analyze heat effects associated with the solid-state phase transition in ultrahigh molecular weight polyethylene from the unstable monoclinic phase into thermodynamically stable orthorhombic phase. The model proposed here for the structure of supramolecular formations of monoclinic phase does not contradict to earlier X-ray diffraction data for this polymer.


2020 ◽  
Vol 62 (8) ◽  
pp. 1326
Author(s):  
Д.В. Анохин ◽  
К.Н. Графская ◽  
Д.А. Иванов ◽  
Е.М. Иванькова ◽  
В.А. Марихин ◽  
...  

Annotation The X-ray analysis of a virgin particle taken directly from the synthesis products of an ultra-high molecular weight polyethylene (UHMWPE) and not subjected to any external stresses was carried out using nanofocus beamline ID13 European Synchrotron Radiation Facility (ESRF, Grenoble,France). In the X-ray diffraction curves obtained by scanning an arbitrarily selected portion of a particle with a size of (100 x 20) μm2 by a microbeam (0.3 x 0.3) μm2 with a step of 2 μm horizontally and 0.5 μm vertically, along with reflections from the orthorhombic phase, reflexes from the metastable monoclinic phase were observed. It is believed that the cause of its occurrence may be stresses that develop during specific structure formation in slurry synthesis and persist when cooled to room temperature and the solvent evaporates. The possibility of localization of the monoclinic phase in various morphological formations is discussed.


Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.


2011 ◽  
Vol 04 (03) ◽  
pp. 225-229 ◽  
Author(s):  
WENJUAN WU ◽  
DINGQUAN XIAO ◽  
JIAGANG WU ◽  
JING LI ◽  
JIANGUO ZHU

( K 0.48 Na 0.52) NbO 3-x% Co 2 O 3 (x = 0, 0.03 and 0.05) (KNN-x% Co2O3 ) lead-free piezoelectric ceramics were prepared by the conventional solid-state sintering method. An orthorhombic phase was observed for all KNN-x% Co2O3 ceramics at room temperature, and two phase transitions were confirmed by the high temperature X-ray diffraction and the temperature dependence of the dielectric constant. The Co2O3 greatly improves the density and decreases the sintering temperature of KNN ceramics. The KNN-0.05 mol%Co2O3 ceramic exhibits good properties (d33 = 120 pC/N , k p = 0.41, Q m = 213 and T c = 407°C) and a good age stability. The multiferroic behavior was also observed at room temperature for the KNN-0.05 mol%Co2O3 ceramic, as confirmed by P–E loops and magnetic behavior.


2014 ◽  
Vol 602-603 ◽  
pp. 677-680
Author(s):  
Mei Mei Wu ◽  
Yun Tao Liu

The structural and thermal expansion properties of solid solutions In2-xFexMo3O12have been characterized using X-ray diffraction. The lattice parameters decrease linearly with increasing Fe content at room temperature. All compounds exhibit monoclinic structure at room temperature, and transform to orthorhombic phase upon heating. Monoclinic In2-xFexMo3O12(x= 0.3, 1.0 and 1.3) possess strong positive thermal expansion, while the linear thermal expansion coefficient of orthorhombic phase varies from zero/near-zero to positive with increasing Fe3+content.


Author(s):  
Monika K. Krawczyk ◽  
Zbigniew Czapla ◽  
Adam Ingram ◽  
Andrzej Kozdraś ◽  
Tadeusz Lis ◽  
...  

On the basis of thermal analysis (DSC, DTA, DTG), single crystal X-ray diffraction experiments, dielectric studies and optical observation, it is found that the (N2H5)3[CdCl5] crystal exhibits several structural phase transitions. At room temperature, the studied crystal exhibits ferroelastic properties and undergoes phase transition from the monoclinic to the orthorhombic phase on heating above 327 K. Upon subsequent cooling, two structural phase transitions at about 323 and 319 K are observed, where the crystal adopts orthorhombic symmetry. The presented phase transitions are unique due to the fact the first heating run results in different structural changes compared to those observed during cooling and subsequent heating/cooling runs. In the studied crystal, N2H5 + ions and 1D chains built up from {CdCl5}3− units bridged by Cl atoms occur. The phase transitions observed can be associated with reorientation of cations and partial disorder of cations as well as Cl atoms.


2013 ◽  
Vol 770 ◽  
pp. 149-152 ◽  
Author(s):  
T. Plirdpring ◽  
M. Horprathum ◽  
C. Chananonnawathorn ◽  
P. Eiamchai ◽  
A. Harnwunggmoung ◽  
...  

Tantalum oxide (Ta2O5) films at 400 nm thickness were prepared at room temperature by DC reactive magnetron sputtering. The effect of annealing temperature on film crystallinity, microstructure and optical properties were investigated. In order to indentify the crystalline structure and film morphology, X-ray diffraction (XRD) and field-emission scanning electron microscope (FE-SEM) measurements were performance. The optical properties were determined by UV-Vis spectrophotometer and spectroscopic ellipsometry (SE). The result showed that, with the annealing treatment at high temperature (700-900°C), the as-deposited films were crystallized to orthorhombic phase of tantalum pentaoxide (β-Ta2O5). In addition, the transmittance spectrum percentage indicated 87%, which corresponded to the obtained optical characteristic. The refractive index varied at 550 nm from 2.17 to 2.21 with increased of the annealing temperature.


2020 ◽  
Vol 3 (1) ◽  
Author(s):  
Sarangi Venkateshwarlu ◽  
Lalitha K. Venkataraman ◽  
Valentin Segouin ◽  
Frederick P. Marlton ◽  
Ho Chin Hin ◽  
...  

Abstract In many ferroelectrics, large electromechanical strains are observed near regions of composition- or temperature- driven phase coexistence. Phenomenologically, this is attributed to easy re-orientation of the polarization vector and/or phase transition, although their effects are highly convoluted and difficult to distinguish experimentally. Here, we used synchrotron X-ray scattering and digital image correlation to differentiate between the microscopic mechanisms leading to large electrostrains in an exemplary Pb-free piezoceramic Sn-doped barium calcium zirconate titanate. Large electrostrains of ~0.2% measured at room-temperature are attributed to an unconventional effect, wherein polarization switching is aided by a reversible phase transition near the tetragonal-orthorhombic phase boundary. Additionally, electrostrains of ~0.1% or more could be maintained from room temperature to 140 °C due to a succession of different microscopic mechanisms. In situ X-ray diffraction elucidates that while 90° domain reorientation is pertinent below the Curie temperature (TC), isotropic distortion of polar clusters is the dominant mechanism above TC.


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.


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