A Study of Natural Metamict Yttrium Niobate as Analogue of Actinide Ceramic Waste Form

2014 ◽  
Vol 1665 ◽  
pp. 313-318 ◽  
Author(s):  
Cao Qiuxiang ◽  
Anton I. Isakov ◽  
Liu Xiaodong ◽  
Sergey V. Krivovichev ◽  
Boris E. Burakov
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Single Phase ◽  
Microprobe Analysis ◽  
Electron Microprobe Analysis ◽  
Original Sample ◽  
X Ray Diffraction ◽  
Average Chemical Composition ◽  
X Ray ◽  
Scanning Electron

ABSTRACTNatural metamict mineral found as large (1-3 cm in size) homogeneous grains (as assumed, former single crystals), was investigated by X-ray powder diffraction (pXRD), high-temperature pXRD, scanning electron microscopy (SEM) and electron microprobe analysis (EMPA). The average chemical composition obtained by EMPA is (wt. %): Nb2O5 – 42.6; Ta2O5 – 4.4; TiO2 – 9.2; UO3 – 4.4; ThO2 – 1.0; MnO – 1.3; FeO – 19.4; Y2O3 – 16.6.The untreated (original) sample is X-ray amorphous. The sample remained amorphous after annealing at 400 °C for 1 hour. The sample became almost fully crystalline after annealing at 700 °C for 1 hour with an X-ray diffraction pattern similar to that of Fe-columbite (ICCD: 01-074-7356). Further annealing at 1000 °C and higher temperatures caused changes in the phase composition of the sample. It was proposed that under self-irradiation a single-phase U-Th-bearing solid solution, based on monocrystalline Y-niobate, became metamict but remained homogeneous without evidence of solid solution destruction. However, this metamict solid solution is unstable under thermal treatment and recrystallization.

Influence of Annealing Time on Microstructure of Ni-W Alloys

2013 ◽  
Vol 747-748 ◽  
pp. 613-618
Author(s):  
Qiao Zhang ◽  
Shu Hua Liang ◽  
Chen Zhang ◽  
Jun Tao Zou
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Grain Size ◽  
Grain Boundaries ◽  
Annealing Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Average Grain Size ◽  
Scanning Electron

The as-cast Ni-W alloys with 15wt%W, 25wt%W and 30wt%W were annealed in hydrogen at 1100. The effect of the annealing time on the microstructure of Ni-W alloys was studied, and the phase constituents and microstructure of annealed Ni-W alloys were characterized by the X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that no any phase changed for Ni-15%W, Ni-25%W and Ni-30%W alloys annealed for 60 min, 90 min and 150 min, which were still consisted of single-phase Ni (W) solid solution. However, microstructure had a significant change after annealing. With increase of annealing time, the microstructure of Ni-15%W alloy became more uniform after annealing for 90 min, and the average grain size was 95μm, whereas the grain size of Ni-15%W alloy increased significantly after annealing for 150 min. For Ni-25%W and Ni-30%W, there was no obvious change on the grain size with increase of annealing time, and the amount of oxides at grain boundaries gradually reduced. After annealing for 150 min, the impurities at grain boundaries almost disappeared. Subsequently, the annealing at 1100 for 150 min was beneficial for the desired microstructure of Ni-25%W and Ni-30%W alloys.

Synthesis of Ti3Si0.4Al0.8C1.8 Solid Solution

2008 ◽  
Vol 368-372 ◽  
pp. 995-997
Author(s):  
Cui Wei Li ◽  
Hong Xiang Zhai ◽  
Yang Zhou ◽  
Shi Bo Li ◽  
Zhi Li Zhang
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Scanning Electron Microscopy ◽  
Single Phase ◽  
Lattice Parameters ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Powder Mixtures ◽  
X Ray ◽  
Scanning Electron

In this study, free Ti/Si/Al/C powder mixtures with molar ratio of 3:0.4:0.8:1.8 were heated in Argon with various schedules, in order to reveal the possibility for the synthesis of Ti3Si0.4Al0.8C1.8 solid solution powder. X-ray diffraction (XRD) was used for the evaluation of phase identities of the powder after different treatments. Scanning electron microscopy (SEM) was used to observe the morphology of the Ti3Si0.4Al0.8C1.8 solid solution. XRD results showed that predominantly single phase samples of Ti3Si0.4Al0.8C1.8 was prepared after heating at 1400oC for 5 min in Argon and the lattice parameters of Ti3Si0.4Al0.8C1.8 lay between those of Ti3SiC2 and Ti3AlC2.

Effects of V2O5 on the synthesis of Ba2Ti9O20 powders

2005 ◽  
Vol 20 (10) ◽  
pp. 2741-2744 ◽  
Author(s):  
Huixing Lin ◽  
Wei Chen ◽  
Lan Luo
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Scanning Electron Microscopy ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Eutectic Liquid ◽  
X Ray ◽  
Intermediate Phases ◽  
Phase Pure ◽  
Scanning Electron

Phase-pure Ba2Ti9O20 powders were made by doping 3 wt% of V2O5 to a Ba:Ti = 2:9 molar composition, and the effects of the dopant on the phase formation were investigated. The study shows that BaTiO3, BaTi2O5, and BaTi4O9 were the intermediate phases before the formation of Ba2Ti9O20 for samples with or without V2O5. However, with V2O5 doping, the temperature at which Ba2Ti9O20 occurred were lowered from 1150 to 1050 °C and single phase Ba2Ti9O20 powders was easily obtained at 1150 °C for 2 h. Microstructure of the powders was examined by field emission scanning electron microscopy. No evidence of V2O5–Ba2Ti9O20 solid-solution was found by x-ray diffraction and energy-dispersive spectroscopy. The benefit of V2O5 to facilitate the Ba2Ti9O20 synthesis is most probably due to a vanadium-containing eutectic liquid phase which accelerates the migration of reactant species.

Crystal Chemistry and Phase Equilibrium Studies of the Bao(baco3)‐r2o3‐cuo Systems. V. Melting Relations in ba2(y,nd,eu)cu3o6+x

1989 ◽  
Vol 169 ◽  
Author(s):  
Winnie Wong‐Ng ◽  
Lawrence P. Cook ◽  
Michael D. Hill ◽  
Boris Paretzkin ◽  
E.R. Fuller
Keyword(s):  
Electron Microscopy ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Equilibrium Studies ◽  
X Ray ◽  
Helium Gas ◽  
Ionic Size ◽  
Differential Thermogravimetric Analysis ◽  
Melting Relations ◽  
Scanning Electron

AbstractThe influence of the ionic size of the lanthanides R on melting relations of Ba2RCu3O6+x, where R=Y, Eu and Nd, was studied and compared with that of a high Tc superconductor mixed‐lanthanide phase Ba2(Y.75Eu.125Nd 125)Cu3O6+xThese materials have been characterized by a variety of methods including differential thermogravimetric analysis (DTA), scanning electron microscopy (SEM) with energy dispersive X‐ray spectroscopy (EDX) and X‐ray powder diffraction. Single phase samples of Ba2(Y.75Eu.125Nd.125)Cu3O6+x were annealed at 1004, 1040, 1052, 1060, 1078, 1107 and 1160°C and quenched into a helium gas container cooled by liquid nitrogen. The SEM micrographs of these samples showed the progressive chnages in features of the microstructures from sintering and grain growth through melting and then recrystallization from the melt. The addition of the SEM technique in conjunction with X‐ray diffraction has been helpful in the study of phase equilibria in this system.

Effect of Synthesis Conditions and Actinide Contents on Phase Composition of Actinide Bearing Ceramics

2003 ◽  
Vol 807 ◽  
Author(s):  
A. G. Ptashkin ◽  
S. V. Stefanovsky ◽  
S. V. Yudintsev ◽  
S. A. Perevalov
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Phase Composition ◽  
Fluorite Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Synthesis Conditions ◽  
Reducing Conditions ◽  
Dispersive System ◽  
Scanning Electron

ABSTRACTPu-bearing zirconolite and pyrochlore based ceramics were prepared by melting under oxidizing and reducing conditions at 1550 °C. 239Pu content in the samples ranged between ∼10 and ∼50 wt.%. Phase composition of the ceramics and Pu partitioning were studied using X-ray diffraction (XRD) and scanning electron microscopy with energy dispersive system (SEM/EDS). Major phases in the samples were found to be the target zirconolite and pyrochlore as well as a cubic fluorite structure oxide. Normally the Pu content in the Pu host phases was 10–12 wt.%. This corresponds to the Pu content recommended for matrices for immobilization of excess weapons plutonium. At higher Pu content (up to 50 wt.%) additional phases, such as a PuO2-based cubic fluorite-structured solid solution, perovskite, and rutile were found.

Nanocrystalline Barium Zirconium Titanate Synthesized by the Sonochemical Process

2013 ◽  
Vol 802 ◽  
pp. 119-123
Author(s):  
Supamas Wirunchit ◽  
Rangson Muanghlua ◽  
Supamas Wirunchit ◽  
Wanwilai Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Crystal Structure ◽  
Electron Microscopy ◽  
Reaction Time ◽  
Single Phase ◽  
Zirconium Titanate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Large Particles ◽  
Barium Zirconium Titanate ◽  
Scanning Electron

Nanocrystalline barium zirconium titanate, BaZr0.4Ti0.6O3, was synthesized successfully via the sonochemical process. The effects of reaction time on the precipitation of Ba(Zr,Ti)O3 particles were investigated briefly. The crystal structure as well as molecular vibrations and morphology were investigated. X-ray diffraction indicated that the powders exhibited a single phase perovskite structure, without the presence of pyrochlore or unwanted phases at the reaction time of 60 min. Nanocrystals were formed before being oriented and aggregated into large particles in aqueous solution under ultrasonic irradiation. A scanning electron microscopy (SEM) photograph showed the BZT powder as spherical in shape with uniform nanosized features.

scholarly journals Efflorescent Sulfate Crystallization on Fractured and Polished Colloform Pyrite Surfaces: A Migration Pathway of Trace Elements

Minerals ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 12
Author(s):  
Dimitrina Dimitrova ◽  
Vassilka Mladenova ◽  
Lutz Hecht
Keyword(s):  
Electron Microscopy ◽  
Trace Elements ◽  
Inductively Coupled Plasma ◽  
Microprobe Analysis ◽  
Electron Microprobe Analysis ◽  
X Ray ◽  
Inductively Coupled ◽  
Migration Pathway ◽  
Plasma Mass Spectrometry ◽  
Scanning Electron

The colloform pyrite variety incorporates many trace elements that are released in the environment during rapid oxidation. Colloform pyrite from the Chiprovtsi silver–lead deposit in Bulgaria and its oxidation efflorescent products were studied using X-ray diffractometry, scanning electron microscopy, electron microprobe analysis, and laser ablation inductively coupled plasma mass spectrometry. Pyrite is enriched with (in ppm): Co (0.1–964), Ni (1.8–3858), Cu (2.9–3188), Zn (3.1–77), Ag (1.2–1771), As (8179–52,787), Se (2.7–21.7), Sb (48–17792), Hg (4–2854), Tl (1.7–2336), Pb (13–7072), and Au (0.07–2.77). Gypsum, anhydrite, szomolnokite, halotrichite, römerite, copiapite, aluminocopiapite, magnesiocopiapite, coquimbite, aluminocoquimbite, voltaite, and ammoniomagnesiovoltaite were identified in the efflorescent sulfate assemblage. Sulfate minerals contain not only inherited elements from pyrite (Cr, Fe, Co, Ni, Cu, Zn, Ag, In, As, Sb, Hg, Tl, and Pb), but also newly introduced elements (Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Mn, Ga, Rb, Sr, Y, Zr, Sn, Cs, Ba, REE, U, and Th). Voltaite group minerals, copiapite, magnesiocopiapite, and römerite incorporate most of the trace elements, especially the most hazardous As, Sb, Hg, and Tl. Colloform pyrite occurrence in the Chiprovtsi deposit is limited. Its association with marbles would further restrict the oxidation and release of hazardous elements into the environment.

Nanoporous Ni and Ni-Cu Fabricated by Dealloying

2009 ◽  
Vol 1228 ◽  
Author(s):  
Masataka Hakamada ◽  
Yasumasa Chino ◽  
Mamoru Mabuchi
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Noble Metals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
The Difference ◽  
20 Nm ◽  
Good Workability ◽  
Scanning Electron

AbstractMetallic nanoporous architecture can be spontaneously attained by dealloying of a binary alloy. The nanoporous architecture can be often fabricated in noble metals such as Au and Pt. In this study, nanoporous Ni, Ni-Cu are fabricated by dealloying rolled Ni-Mn and Cu-Ni-Mn alloys, respectively. Unlike conventional Raney nickel composed of brittle Ni-Al or Cu-Al intermetallic compounds, the initial alloys had good workability probably because of their fcc crystal structures. After the electrolysis of the alloys in (NH4)2SO4 aqueous solution, nanoporous architectures of Ni and Ni-Cu with pore and ligament sizes of 10–20 nm were confirmed by scanning electron microscopy and transmission electron microscopy. X-ray diffraction analyses suggested that Ni and Cu atoms form a homogeneous solid solution in the Ni-Cu nanoporous architecture. The ligament sizes of nanoporous Ni and Ni-Cu were smaller than that of nanoporous Cu, reflecting the difference between diffusivities of Ni and Cu at solid/electrolyte interface. Ni can reduce the pore and ligament sizes of resulting nanoporous architecture when added to initial Cu-Mn alloys.

Synthesis, Phase Formation and Characterization of Co4Nb2O9 Powders Synthesized by Solid-State Reaction

2008 ◽  
Vol 55-57 ◽  
pp. 873-876 ◽  
Author(s):  
N. Chaiyo ◽  
R. Muanghlua ◽  
A. Ruangphanit ◽  
Wanwilai C. Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Solid State Reaction ◽  
Dwell Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Techniques ◽  
Scanning Electron

A corundum-type structure of cobalt niobate (Co4Nb2O9) has been synthesized by a solid-state reaction. The formation of the Co4Nb2O9 phase in the calcined powders was investigated as a function of calcination conditions by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Morphology and particle size have been determined by scanning electron microscopy (SEM). It was found that the minor phases of unreacted Co3O4 tend to form together with the columbite CoNb2O6 phase at a low calcination temperature and short dwell time. It seems that the single-phase of Co4Nb2O9 in a corundum phase can be obtained successfully at the calcination conditions of 900°C for 60 min, with heating/cooling rates of 20°C /min.

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