Grain size measurement from two-dimensional micro-X-ray diffraction: Laboratory application of a radial integration technique

2015 ◽  
Vol 100 (8-9) ◽  
pp. 1899-1911 ◽  
Author(s):  
Michael S. Bramble ◽  
Roberta L. Flemming ◽  
Phil J.A. McCausland
2000 ◽  
Vol 321-324 ◽  
pp. 133-136 ◽  
Author(s):  
Yu.D. Yagodkin ◽  
G.V. Vekilova ◽  
R.S. Mungalov

1999 ◽  
Vol 12 (5-8) ◽  
pp. 657-660 ◽  
Author(s):  
T. Inami ◽  
M. Kobiyama ◽  
S. Okuda ◽  
H. Maeta ◽  
H. Ohtsuka

2004 ◽  
Vol 19 (2) ◽  
pp. 110-118 ◽  
Author(s):  
Bob Baoping He

X-ray diffraction analysis on small samples or micro-area of large samples is always a challenge due to weak diffraction and poor statistics, especially when dealing with samples containing large grain size, inhomogeneous phase distribution, and preferred orientation. Two-dimensional X-ray diffraction has many advantages in microdiffraction analysis. A two-dimensional detector can collect a large amount of data both in terms of speed and angular coverage. This paper covers some aspects about instrumentation of two-dimensional X-ray diffraction and its applications in phase identification and stress analysis on small samples and micro-area of large samples.


Author(s):  
K. H. Downing ◽  
S. G. Wolf ◽  
E. Nogales

Microtubules are involved in a host of critical cell activities, many of which involve transport of organelles through the cell. Different sets of microtubules appear to form during the cell cycle for different functions. Knowledge of the structure of tubulin will be necessary in order to understand the various functional mechanisms of microtubule assemble, disassembly, and interaction with other molecules, but tubulin has so far resisted crystallization for x-ray diffraction studies. Fortuitously, in the presence of zinc ions, tubulin also forms two-dimensional, crystalline sheets that are ideally suited for study by electron microscopy. We have refined procedures for forming the sheets and preparing them for EM, and have been able to obtain high-resolution structural data that sheds light on the formation and stabilization of microtubules, and even the interaction with a therapeutic drug.Tubulin sheets had been extensively studied in negative stain, demonstrating that the same protofilament structure was formed in the sheets and microtubules. For high resolution studies, we have found that the sheets embedded in either glucose or tannin diffract to around 3 Å.


2008 ◽  
Vol 73 (1) ◽  
pp. 24-31
Author(s):  
Dayu Wu ◽  
Genhua Wu ◽  
Wei Huang ◽  
Zhuqing Wang

The compound [Cd(4,4'-bpy)2(H2O)2](ClO4)2·(L)2 was obtained by the reaction of Cd(ClO4)2, bis(1-pyrazinylethylidene)hydrazine (L) and 4,4'-bipyridine in aqueous MeOH. Single-crystal X-ray diffraction has revealed its two-dimensional metal-organic framework. The 2-D layers superpose on each other, giving a channel structure. The square planar grids consist of two pairs of shared edges with Cd(II) ion and a 4,4'-bipyridine molecule each vertex and side, respectively. The square cavity has a dimension of 11.817 × 11.781 Å. Two guest molecules of bis(1-pyrazinylethylidene)hydrazine are clathrated in every hydrophobic host cavity, being further stabilized by π-π stacking and hydrogen bonding. The results suggest that the hydrazine molecules present in the network serve as structure-directing templates in the formation of crystal structures.


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.


2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.


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.


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