Fabrication of 239/238Pu-Zirconolite Ceramic Pellets by Natural Sintering

2003 ◽  
Vol 807 ◽  
Author(s):  
T. Advocat ◽  
F. Jorion ◽  
T. Marcillat ◽  
G. Leturcq ◽  
X. Deschanels ◽  
...  
Keyword(s):  
Grain Size ◽  
Radioactive Waste ◽  
Nuclear Waste ◽  
Chemical Stability ◽  
Minor Actinides ◽  
Loading Capacity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Physical And Chemical ◽  
Inorganic Matrix

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.

scholarly journals Preparation of high-entropy carbides by different sintering techniques

2021 ◽  
Vol 56 (19) ◽  
pp. 11237-11247 ◽  
Author(s):  
Johannes Pötschke ◽  
Manisha Dahal ◽  
Mathias Herrmann ◽  
Anne Vornberger ◽  
Björn Matthey ◽  
...  
Keyword(s):  
Grain Size ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Vacuum Sintering ◽  
X Ray ◽  
High Entropy ◽  
Mean Grain Size ◽  
The Mean ◽  
Gas Pressure Sintering ◽  
Hardness Values

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.

scholarly journals X-ray diffraction analysis of kaolin M1 and M2 via the Williamson–Hall and Warren–Averbach methods

2021 ◽  
pp. 174751982098472
Author(s):  
Lalmi Khier ◽  
Lakel Abdelghani ◽  
Belahssen Okba ◽  
Djamel Maouche ◽  
Lakel Said
Keyword(s):  
Grain Size ◽  
High Temperature ◽  
Low Temperature ◽  
Diffraction Analysis ◽  
Mechanical Resistance ◽  
X Ray Diffraction ◽  
Integral Breadth ◽  
X Ray ◽  
Mullite Phase

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.

Monitoring of Fluctuations in the Physical and Chemical Properties of a High-Calcium Fly Ash

1987 ◽  
Vol 113 ◽  
Author(s):  
Scott Schlorholtz ◽  
Ken Bergeson ◽  
Turgut Demirel
Keyword(s):  
Fly Ash ◽  
Chemical Properties ◽  
Operating Conditions ◽  
Physical And Chemical Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Studies ◽  
High Calcium ◽  
Physical And Chemical ◽  
And Chemical Properties

ABSTRACTThe physical and chemical properties of fly ash produced at Ottumwa Generating Station have been monitored since April, 1985. The fly ash is produced from burning a low sulfur, sub-bituminous coal obtained from the Powder River Basin near Gillette, Wyoming. One-hundred and sixty samples of fly ash were obtained during the two year period. All of the samples were subjected to physical testing as specified by ASTM C 311. About one-hundred of the samples were also subjected to a series of tests designed to monitor the self-cementing properties of the fly ash. Many of the fly ash samples were subjected to x-ray diffraction and fluorescence analysis to define the mineralogical and chemical composition of the bulk fly ash as a function of sampling date. Hydration products in selected hardened fly ash pastes, were studied by x-ray diffraction and scanning electron microscopy. The studies indicated that power plant operating conditions influenced the compressive strength of the fly ash paste specimens. Mineralogical and morphological studies of the fly ash pastes indicated that stratlingite formation occurred in the highstrength specimens, while ettringite was the major hydration product evident in the low-strength specimens.

Nanocrystalline Solutions as Precursors to The Spray Deposition of Cdte Thin Films

1995 ◽  
Vol 382 ◽  
Author(s):  
Martin Pehnt ◽  
Douglas L. Schulz ◽  
Calvin J. Curtis ◽  
Helio R. Moutinho ◽  
Amy Swartzlander ◽  
...  
Keyword(s):  
Thin Films ◽  
Atomic Force Microscopy ◽  
Grain Size ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Cdte Nanoparticles ◽  
Atomic Force ◽  
Vis Spectroscopy ◽  
Cdte Thin Films

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.

Effect of Nitridation Magnetic Properties of Nanocrystalline Fe-Co Alloy Powders

2010 ◽  
Vol 654-656 ◽  
pp. 1106-1109
Author(s):  
Ya Qiong He ◽  
Chang Hui Mao ◽  
Jian Yang
Keyword(s):  
Grain Size ◽  
Magnetic Properties ◽  
Alloy Powder ◽  
High Energy ◽  
X Ray Diffraction ◽  
Powder Mixtures ◽  
X Ray ◽  
Transmission Electron ◽  
Nitridation Temperature ◽  
Microstructure And Magnetic Properties

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.

Structural and thermodynamic properties of nanocrystalline fcc metals prepared by mechanical attrition

1992 ◽  
Vol 7 (7) ◽  
pp. 1751-1761 ◽  
Author(s):  
J. Eckert ◽  
J.C. Holzer ◽  
C.E. Krill ◽  
W.L. Johnson
Keyword(s):  
Thermal Analysis ◽  
Grain Size ◽  
Melting Point ◽  
Grain Boundary ◽  
Bulk Modulus ◽  
Atomic Level ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fcc Metals ◽  
Mechanical Attrition

Nanocrystalline fcc metals have been synthesized by mechanical attrition. The crystal refinement and the development of the microstructure have been investigated in detail by x-ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The deformation process causes a decrease of the grain size of the fcc metals to 6–22 nm for the different elements. The final grain size scales with the melting point and the bulk modulus of the respective metal: the higher the melting point and the bulk modulus, the smaller the final grain size of the powder. Thus, the ultimate grain size achievable by this technique is determined by the competition between the heavy mechanical deformation introduced during milling and the recovery behavior of the metal. X-ray diffraction and thermal analysis of the nanocrystalline powders reveal that the crystal size refinement is accompanied by an increase in atomic-level strain and in the mechanically stored enthalpy in comparison to the undeformed state. The excess stored enthalpies of 10–40% of the heat of fusion exceed by far the values known for conventional deformation processes. The contributions of the atomic-level strain and the excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth in the nanocrystalline fcc metals are investigated by thermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis, and estimates of the grain boundary enthalpy are given.

Magnetic Properties of Sputtered Fe-O and Co-O Thin Films

1995 ◽  
Vol 403 ◽  
Author(s):  
D. V. Dimitrov ◽  
A. S. Murthy ◽  
G. C. Hadjipanayis ◽  
C. P. SWANN
Keyword(s):  
Grain Size ◽  
Low Temperatures ◽  
Room Temperature ◽  
Oxide Films ◽  
X Ray Diffraction ◽  
Dc Magnetron Sputtering ◽  
Large Shift ◽  
X Ray ◽  
Grain Size And Shape ◽  
Spherical Grains

AbstractFe-O and Co-O films were prepared by DC magnetron sputtering in a mixture of Ar and O2 gases. By varying the oxygen to argon ratio, oxide films with stoichiometry FeO, Fe3O4, α-Fe2O3, CoO and Co3O4 were produced. TEM studies showed that the Fe – oxide films were polycrystalline consisting of small almost spherical grains, about 10 nm in size. Co-O films had different microstructure with grain size and shape dependent on the amount of oxygen. X-ray diffraction studies showed that the grains in Fe-O films were randomly oriented in contrast to Co-O films in which a <111> texture was observed. Pure FeO and α-Fe2O3 films were found to be superparamagnetic at room temperature but strongly ferromagnetic at low temperatures in contrast to the antiferromagnetic nature of bulk samples. A very large shift in the hysteresis loop, about 3800 Oe, was observed in field cooled Co-CoO films indicating the presence of a large unidirectional exchange anisotropy.

Ionic conductivity in nanocrystalline Gd doped ceria

2008 ◽  
Vol 1122 ◽  
Author(s):  
Gianguido Baldinozzi ◽  
David Simeone ◽  
Dominique Gosset ◽  
Mickael Dollé ◽  
Georgette Petot-Ervas
Keyword(s):  
Grain Size ◽  
Ionic Conductivity ◽  
Sol Gel ◽  
Doped Ceria ◽  
Narrow Size Distribution ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grain Sizes ◽  
The Impact

AbstractWe have synthesized Gd-doped ceria polycrystalline samples (5, 10, 15 %mol), having relative densities exceeding 95% and grain sizes between 30 and 160 nm after axial hot pressing (750 °C, 250 MPa). The samples were prepared by sintering nanopowders obtained by sol-gel chemistry methods having a very narrow size distribution centered at about 16 nm. SEM and X-ray diffraction were performed to characterize the sample microstructures and to assess their structures. We report ionic conductivity measurements using impedance spectroscopy. It is important to investigate the properties of these systems with sub-micrometric grains and as a function of their composition. Therefore, samples having micrometric and nanometric grain sizes (and different Gd content) were studied. Evidence of Gd segregation near the grain boundaries is given and the impact on the ionic conductivity, as a function of the grain size and Gd composition, is discussed and compared to microcrystalline samples.

scholarly journals Chemical Stability of Ti3C2 MXene with Al in the Temperature Range 500–700 °C

Materials ◽  
2018 ◽  
Vol 11 (10) ◽  
pp. 1979 ◽  
Author(s):  
Jing Zhang ◽  
Shibo Li ◽  
Shujun Hu ◽  
Yang Zhou
Keyword(s):  
Electron Microscopy ◽  
Chemical Stability ◽  
Metal Matrix ◽  
Matrix Composites ◽  
X Ray Diffraction ◽  
X Ray ◽  
Temperature Range ◽  
Transmission Electron ◽  
Work First ◽  
Scanning Electron

Ti3C2Tx MXene, a new 2D nanosheet material, is expected to be an attractive reinforcement of metal matrix composites because its surfaces are terminated with Ti and/or functional groups of –OH, –O, and –F which improve its wettability with metals. Thus, new Ti3C2Tx/Al composites with strong interfaces and novel properties are desired. To prepare such composites, the chemical stability of Ti3C2Tx with Al at high temperatures should be investigated. This work first reports on the chemical stability of Ti3C2Tx MXene with Al in the temperature range 500–700 °C. Ti3C2Tx is thermally stable with Al at temperatures below 700 °C, but it reacts with Al to form Al3Ti and TiC at temperatures above 700 °C. The chemical stability and microstructure of the Ti3C2Tx/Al samples were investigated by differential scanning calorimeter, X-ray diffraction analysis, scanning electron microscopy, and transmission electron microscopy.

The Synthesis of Cu0.81Ni0.19 Intermetallics by Mechanical Alloying

2012 ◽  
Vol 496 ◽  
pp. 379-382
Author(s):  
Rui Song Yang ◽  
Ming Tian Li ◽  
Chun Hai Liu ◽  
Xue Jun Cui ◽  
Yong Zhong Jin
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Grain Size ◽  
Mechanical Alloying ◽  
Milling Time ◽  
Elemental Powder ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scherrer Equation ◽  
Scanning Electron

The Cu0.81Ni0.19 has been synthesized directly from elemental powder of nickel and copper by mechanical alloying. The alloyed Cu0.81Ni0.19 alloy powders are prepared by milling of 8h. The grain size calculated by Scherrer equation of the NiCu alloy decreased with the increasing of milling time. The end-product was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM)

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