scholarly journals Локальная структура и процессы гидратации галогензамещенных перовскитов на основе Ba-=SUB=-4-=/SUB=-In-=SUB=-2-=/SUB=-Zr-=SUB=-2-=/SUB=-O-=SUB=-11-=/SUB=-

2019 ◽  
Vol 126 (4) ◽  
pp. 419
Author(s):  
Н.А. Тарасова ◽  
А.О. Галишева ◽  
И.Е. Анимица

AbstractHalogen-substituted perovskites Ba_4In_2Zr_2O_10.95F_0.1 and Ba_4In_2Zr_2O_10.95Cl_0.1 are synthesized, and their single-phase composition is verified by X-ray diffraction analysis. Their ability of the studied phases to hydrate and form energetically unequal OH^– groups is proved. It is found that introduction of halide ions leads to a decrease in the hydration degree with respect to the matrix composition, which is explained by a decrease in the crystal unit cell free volume Processes.

1991 ◽  
Vol 6 (6) ◽  
pp. 1230-1237 ◽  
Author(s):  
D. Legzdina ◽  
I.M. Robertson ◽  
H.K. Birnbaum

The distribution and chemistry of hydrides produced in single and dual phase alloys with a composition near TiAl have been investigated by using a combination of TEM and x-ray diffraction techniques. The alloys were exposed at 650 °C to 13.8 MPa of gaseous H2 for 100 h. In the single-phase gamma alloy, large hydrides preferentially nucleated on the grain boundaries and matrix dislocations and a population of small hydrides was distributed throughout the matrix. X-ray and electron diffraction patterns from these hydrides indicated that they have an fcc structure with a lattice parameter of 0.45 nm. EDAX analysis of the hydrides showed that they were enriched in Ti. The hydrides were mostly removed by vacuum annealing at 800 °C for 24 h. On dissolution of the hydrides, the chemistry of hydride-free regions of the grain boundary returned to the matrix composition, suggesting that Ti segregation accompanied the hydride formation rather than Ti enrichment causing the formation of the hydride. The hydrogen content in the two-phase (γ-α2) alloy was approximately three times that of the single phase alloy, which was presumably a consequence of the presence of the α2-Ti3Al phase in the two-phase alloy. The hydrides in the two-phase material were shown by x-ray diffraction to have an fcc structure and were removed on annealing in vacuum at 800 °C for 24 h.


Author(s):  
Edgar S. Etz ◽  
Thomas D. Schroeder ◽  
Winnie Wong-Ng

We are investigating by Raman microprobe measurements the superconducting and related phases in the LnBa2Cu3O7-x (for x=0 to 1) system where yttrium has been replaced by several of the lanthanide (Ln = Nd,Sm,Eu,Ho,Er) elements. The aim is to relate the observed optical spectra (Raman and fluorescence) to the compositional and structural properties of these solids as part of comprehensive materials characterization. The results are correlated with the methods of synthesis, the processing techniques of these materials, and their superconducting properties. Of relevance is the substitutional chemistry of these isostructural systems, the differences in the spectra, and their microanalytical usefulness for the detection of impurity phases, and the assessment of compositional homogeneity. The Raman spectra of most of these compounds are well understood from accounts in the literature.The materials examined here are mostly ceramic powders prepared by conventional solid state reaction techniques. The bulk samples are of nominally single-phase composition as determined by x-ray diffraction.


Author(s):  
L. A. Giannuzzi ◽  
A. S. Ramani ◽  
P. R. Howell ◽  
H. W. Pickering ◽  
W. R. Bitler

The δ phase is a Zn-rich intermetallic, having a composition range of ∼ 86.5 - 92.0 atomic percent Zn, and is stable up to 665°C. The stoichiometry of the δ phase has been reported as FeZn7 and FeZn10 The deviation in stoichiometry can be attributed to variations in alloy composition used by each investigator. The structure of the δ phase, as determined by powder x-ray diffraction, is hexagonal (P63mc or P63/mmc) with cell dimensions a = 1.28 nm, c = 5.76 nm, and 555±8 atoms per unit cell. Later work suggested that the layer produced by hot-dip galvanizing should be considered as two distinct phases which are characterized by their morphological differences, namely: the iron-rich region with a compact appearance (δk) and the zinc-rich region with a columnar or palisade microstructure (δp). The sub-division of the δ phase was also based on differences in diffusion behavior, and a concentration discontinuity across the δp/δk boundary. However, work utilizing Weisenberg photographs on δ single crystals reported that the variation in lattice parameters with composition was small and hence, structurally, the δk phase and the δp phase were the same and should be thought of as a single phase, δ. Bastin et al. determined the average cell dimensions to be a = 1.28 nm and c = 5.71 nm, and suggested that perhaps some kind of ordering process, which would not be observed by x-ray diffraction, may be responsible for the morphological differences within the δ phase.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


2019 ◽  
Vol 484 (1) ◽  
pp. 41-43
Author(s):  
E. A. Malinina ◽  
V. K. Skachkova ◽  
I. V. Kozerozhets ◽  
V. V. Avdeeva ◽  
L. V. Goeva ◽  
...  

The method of nanoscaled sodium dodecahydro-closo-dodecaborate Na2[B12H12] synthesis is presented. The composite is heated to 200°C to yield the desired product, forming with the introduction of triethyl- ammonium salt [Et3NH]2[B12H12] into the silicate matrix of a sodium liquid glass. The morphology and phase composition of the synthesized sample are studied through SEM and X-ray diffraction methods, in comparison to those of a standard salt sample Na2[B12H12]. Based on the obtained data, the sample under study is an amorphous composite, on the surface of which nanoscale crystals of Na2[B12H12] form.


Author(s):  
Mariola Kądziołka-Gaweł ◽  
Maria Czaja ◽  
Mateusz Dulski ◽  
Tomasz Krzykawski ◽  
Magdalena Szubka

AbstractMössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopies were used to examine the effects of temperature on the structure of two aluminoceladonite samples. The process of oxidation of Fe2+ to Fe3+ ions started at about 350 °C for the sample richer in Al and at 300 °C for the sample somewhat lower Al-content. Mössbauer results show that this process may be associated with dehydroxylation or even initiate it. The first stage of dehydroxylation takes place at a temperature > 350 °C when the adjacent OH groups are replaced with a single residual oxygen atom. Up to ~500 °C, Fe ions do not migrate from cis-octahedra to trans-octahedra sites, but the coordination number of polyhedra changes from six to five. This temperature can be treated as the second stage of dehydroxylation. The temperature dependence on the integral intensity ratio between bands centered at ~590 and 705 cm−1 (I590/I705) clearly reflects the temperature at which six-coordinated polyhedra are transformed into five-coordinated polyhedra. X-ray photoelectron spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p and O1s core levels, highlighted a route to identify the position of Si, Al, K and Fe cations in a structure of layered silicates with temperature. All the measurements show that the sample with a higher aluminum content and a lower iron content in octahedral sites starts to undergo a structural reorganization at a relatively higher temperature than the less aluminum-rich sample does. This suggests that iron may perform an important role in the initiation of the dehydroxylation of aluminoceladonites.


2021 ◽  
Vol 56 (19) ◽  
pp. 11237-11247 ◽  
Author(s):  
Johannes Pötschke ◽  
Manisha Dahal ◽  
Mathias Herrmann ◽  
Anne Vornberger ◽  
Björn Matthey ◽  
...  

AbstractDense (Hf, Ta, Nb, Ti, V)C- and (Ta, Nb, Ti, V, W)C-based high-entropy carbides (HEC) were produced by three different sintering techniques: gas pressure sintering/sinter–HIP at 1900 °C and 100 bar Ar, vacuum sintering at 2250 °C and 0.001 bar as well as SPS/FAST at 2000 °C and 60 MPa pressure. The relative density varied from 97.9 to 100%, with SPS producing 100% dense samples with both compositions. Grain size measurements showed that the substitution of Hf with W leads to an increase in the mean grain size of 5–10 times the size of the (Hf, Ta, Nb, Ti, V,)C samples. Vacuum-sintered samples showed uniform grain size distribution regardless of composition. EDS mapping revealed the formation of a solid solution with no intermetallic phases or element clustering. X-ray diffraction analysis showed the structure of mostly single-phase cubic high-entropy carbides. Hardness measurements revealed that (Hf, Ta, Nb, Ti, V)C samples possess higher hardness values than (Ta, Nb, Ti, V, W)C samples.


2020 ◽  
Vol 10 (03) ◽  
pp. 2050003
Author(s):  
M. R. Hassan ◽  
M. T. Islam ◽  
M. N. I. Khan

In this research, influence of adding Li2CO3 (at 0%, 2%, 4%, 6%) on electrical and magnetic properties of [Formula: see text][Formula: see text]Fe2O4 (with 60% Ni and 40% Mg) ferrite has been studied. The samples are prepared by solid state reaction method and sintered at 1300∘C for 6[Formula: see text]h. X-ray diffraction (XRD) patterns show the samples belong to single-phase cubic structure without any impurity phase. The magnetic properties (saturation magnetization and coercivity) of the samples have been investigated by VSM and found that the higher concentration of Li2CO3 reduces the hysteresis loss. DC resistivity increases with Li2CO3 contents whereas it decreases initially and then becomes constant at lower value with temperature which indicates that the studied samples are semiconductor. The dielectric dispersion occurs at a low-frequency regime and the loss peaks are formed in a higher frequency regime, which are due to the presence of resonance between applied frequency and hopping frequency of charge carriers. Notably, the loss peaks are shifted to the lower frequency with Li2CO3 additions.


2004 ◽  
Vol 37 (6) ◽  
pp. 967-976 ◽  
Author(s):  
Andrew C. Jupe ◽  
Stuart R. Stock ◽  
Peter L. Lee ◽  
Nikhila N. Naik ◽  
Kimberly E. Kurtis ◽  
...  

Spatially resolved energy dispersive X-ray diffraction, using high-energy synchrotron radiation (∼35–80 keV), was used nondestructively to obtain phase composition profiles along the radii of cylindrical cement paste samples to characterize the progress of the chemical changes associated with sulfate attack on the cement. Phase distributions were acquired to depths of ∼4 mm below the specimen surface with sufficient spatial resolution to discern features less than 200 µm thick. The experimental and data analysis methods employed to obtain quantitative composition profiles are described. The spatial resolution that could be achieved is illustrated using data obtained from copper cylinders with a thin zinc coating. The measurements demonstrate that this approach is useful for nondestructively visualizing the sometimes complex transformations that take place during sulfate attack on cement-based materials. These transformations can be spatially related to microstructure as seen by computed microtomography.


2012 ◽  
Vol 545 ◽  
pp. 275-278 ◽  
Author(s):  
Lili Widarti Zainuddin ◽  
Norlida Kamarulzaman

A ceramics sample of LiTaO3 was prepared using a sol-gel method. The sample is annealed at 750 °C for 48 hours. X-ray diffraction analysis indicate the formation of single phase, rhombohedral structure. An ac impedance study was used to analyse the conductivity of LiTaO3 at room temperature and at various temperatures.


Sign in / Sign up

Export Citation Format

Share Document