scholarly journals Grain size dependent high-pressure elastic properties of ultrafine micro/nanocrystalline grossular

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Jin S. Zhang ◽  
T. Irifune ◽  
M. Hao ◽  
D. Zhang ◽  
Y. Hu ◽  
...  

AbstractWe have performed sound velocity and unit cell volume measurements of three synthetic, ultrafine micro/nanocrystalline grossular samples up to 50 GPa using Brillouin spectroscopy and synchrotron X-ray diffraction. The samples are characterized by average grain sizes of 90 nm, 93 nm and 179 nm (hereinafter referred to as samples Gr90, Gr93, and Gr179, respectively). The experimentally determined sound velocities and elastic properties of Gr179 sample are comparable with previous measurements, but slightly higher than those of Gr90 and Gr93 under ambient conditions. However, the differences diminish with increasing pressure, and the velocity crossover eventually takes place at approximately 20–30 GPa. The X-ray diffraction peaks of the ultrafine micro/nanocrystalline grossular samples significantly broaden between 15–40 GPa, especially for Gr179. The velocity or elasticity crossover observed at pressures over 30 GPa might be explained by different grain size reduction and/or inhomogeneous strain within the individual grains for the three grossular samples, which is supported by both the pressure-induced peak broadening observed in the X-ray diffraction experiments and transmission electron microscopy observations. The elastic behavior of ultrafine micro/nanocrystalline silicates, in this case, grossular, is both grain size and pressure dependent.

2020 ◽  
Vol 38 (2) ◽  
pp. 271-278
Author(s):  
Pijush Ch. Dey ◽  
Sumit Sarkar ◽  
Ratan Das

AbstractIn this work, jagged spherical CdS nanocrystals have been synthesized by chemical method to study their elastic properties. The synthesized CdS nanocrystal has been characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The transmission electron microscope images show that the average size of the nanocrystal is 100 nm approximately. X-ray diffraction (XRD) study confirms that the CdS nanocrystals are in cubic zinc blende structure. The size calculated from the XRD is consistent with the average size obtained from the TEM analysis. The XRD data have been analyzed to study the elastic properties of the jagged spherical CdS nanocrystals, such as intrinsic strain, stress and energy density, using WilliamsonHall plot method. Williamson-Hall method and size-strain plot (SSP) have been used to study the individual effect of crystalline size and lattice strain on the peak broadening of the jagged spherical CdS nanocrystals. Size-strain plot (SSP) and root mean square (RMS) strain further confirm the results obtained from W-H plots.


2015 ◽  
Vol 48 (2) ◽  
pp. 418-430 ◽  
Author(s):  
Gyula Zilahi ◽  
Tamás Ungár ◽  
Géza Tichy

X-ray diffraction peak broadening is discussed in terms of line broadening and rocking-curve broadening in a novel theoretical description. The nonlocal strain tensor is factorized by using the method of polar decomposition instead of the more conventional separation into symmetrical and antisymmetrical components. A number of X-ray line-broadening and rocking-curve experiments on the same single crystals or individual grains in bulk polycrystals prove that plastic deformation produces strained subgrains mutually rotated by rigid-body rotations. The novel theoretical description appropriately accounts for the rigid-body rotation and strain at the same time and provides straightforward separation of the two effects of line and rocking-curve broadening in the radial and normal directions of the diffraction vector. The mathematical results are discussed in terms of experiments of X-ray diffraction, Laue asterism and electron backscatter diffraction. From the experimental results it is shown that the simultaneous evaluation of line and rocking-curve broadening provides qualitative information about the redundant and geometrically necessary character of dislocations, not available if only one or the other is accessible.


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.


2021 ◽  
pp. 174751982098472
Author(s):  
Lalmi Khier ◽  
Lakel Abdelghani ◽  
Belahssen Okba ◽  
Djamel Maouche ◽  
Lakel Said

Kaolin M1 and M2 studied by X-ray diffraction focus on the mullite phase, which is the main phase present in both products. The Williamson–Hall and Warren–Averbach methods for determining the crystallite size and microstrains of integral breadth β are calculated by the FullProf program. The integral breadth ( β) is a mixture resulting from the microstrains and size effect, so this should be taken into account during the calculation. The Williamson–Hall chart determines whether the sample is affected by grain size or microstrain. It appears very clearly that the principal phase of the various sintered kaolins, mullite, is free from internal microstrains. It is the case of the mixtures fritted at low temperature (1200 °C) during 1 h and also the case of the mixtures of the type chamotte cooks with 1350 °C during very long times (several weeks). This result is very significant as it gives an element of explanation to a very significant quality of mullite: its mechanical resistance during uses at high temperature remains.


2003 ◽  
Vol 807 ◽  
Author(s):  
T. Advocat ◽  
F. Jorion ◽  
T. Marcillat ◽  
G. Leturcq ◽  
X. Deschanels ◽  
...  

ABSTRACTZirconolite is a potential inorganic matrix that is currently investigated in France, in the framework of the 1991 radioactive waste management law, with a view to provide durable containment of the trivalent and tetravalent minor actinides like neptunium, curium, americium and small quantities of unrecyclable plutonium separated from other nuclear waste. To confirm the actinide loading capacity of the zirconolite calcium site and to study the physical and chemical stability of this type of ceramic when subjected to alpha self-irradiation, zirconolite ceramic pellets were fabricated with 10 wt% plutonium oxide (isotope 239 or 238). The 55 pellets are dense (> 93.3% of the theoretical density on average) and free of cracks. They are characterized by a grain size of between 10 and 20 micrometers. X-ray diffraction analyses confirmed the presence of the zirconolite 2M crystalline structure.


1995 ◽  
Vol 382 ◽  
Author(s):  
Martin Pehnt ◽  
Douglas L. Schulz ◽  
Calvin J. Curtis ◽  
Helio R. Moutinho ◽  
Amy Swartzlander ◽  
...  

ABSTRACTIn this article we report the first nanoparticle-derived route to smooth, dense, phase-pure CdTe thin films. Capped CdTe nanoparticles were prepared by injection of a mixture of Cd(CH3)2, (n-C8H17)3 PTe and (n-C8H17)3P into (n-C8H17)3PO at elevated temperatures. The resultant nanoparticles 32-45 Å in diameter were characterized by x-ray diffraction, UV-Vis spectroscopy, transmission electron microscopy, thermogravimetric analysis and energy dispersive x-ray spectroscopy. CdTe thin film deposition was accomplished by dissolving CdTe nanoparticles in butanol and then spraying the solution onto SnO2-coated glass substrates at variable susceptor temperatures. Smooth and dense CdTe thin films were obtained using growth temperatures approximately 200 °C less than conventional spray pyrolysis approaches. CdTe films were characterized by x-ray diffraction, UV-Vis spectroscopy, atomic force microscopy, and Auger electron spectroscopy. An increase in crystallinity and average grain size as determined by x-ray diffraction was noted as growth temperature was increased from 240 to 300 °C. This temperature dependence of film grain size was further confirmed by atomic force microscopy with no remnant nanocrystalline morphological features detected. UV-Vis characterization of the CdTe thin films revealed a gradual decrease of the band gap (i.e., elimination of nanocrystalline CdTe phase) as the growth temperature was increased with bulk CdTe optical properties observed for films grown at 300 °C.


2016 ◽  
Vol 6 (1) ◽  
Author(s):  
Ryosuke Sinmyo ◽  
Elena Bykova ◽  
Sergey V. Ovsyannikov ◽  
Catherine McCammon ◽  
Ilya Kupenko ◽  
...  

Abstract Iron oxides are fundamentally important compounds for basic and applied sciences as well as in numerous industrial applications. In this work we report the synthesis and investigation of a new binary iron oxide with the hitherto unknown stoichiometry of Fe7O9. This new oxide was synthesized at high-pressure high-temperature (HP-HT) conditions, and its black single crystals were successfully recovered at ambient conditions. By means of single crystal X-ray diffraction we determined that Fe7O9 adopts a monoclinic C2/m lattice with the most distorted crystal structure among the binary iron oxides known to date. The synthesis of Fe7O9 opens a new portal to exotic iron-rich (M,Fe)7O9 oxides with unusual stoichiometry and distorted crystal structures. Moreover, the crystal structure and phase relations of such new iron oxide groups may provide new insight into the cycling of volatiles in the Earth’s interior.


2012 ◽  
Vol 102 (3) ◽  
pp. 413a
Author(s):  
Walter E. Teague ◽  
Olivier Soubias ◽  
Nola L. Fuller ◽  
R. Peter Rand ◽  
Klaus Gawrisch

2010 ◽  
Vol 654-656 ◽  
pp. 1106-1109
Author(s):  
Ya Qiong He ◽  
Chang Hui Mao ◽  
Jian Yang

Nanocrystalline Fe-Co alloy powders, which were prepared by high-energy mechanical milling, were nitrided under the mixing gas of NH3/H2 in the temperature range from 380°C to 510°C. X-ray diffraction (XRD) was used to analyze the grain size and reaction during the processing. The magnetic properties of the nitrided powders were measured by Vibrating Sample Magnetometer (VSM). The results show that with the appearance of Fe4N phase after nitride treatment, and the grain-size of FeCo phase decreases with the increase of nitridation temperature between 380°C to 450°C.The saturation magnetization of nitrided alloy powder treated at 480°C is about 18% higher than that of the initial Fe-Co alloy powder, accompanied by the reduction of the coercivity. Transmission electron microscope (TEM) was used, attempting to further analyze the effect of Fe4N phase on microstructure and magnetic properties of the powder mixtures.


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