Densification Behaviour of Nano-Size CeO2

2007 ◽  
Vol 555 ◽  
pp. 189-194 ◽  
Author(s):  
D. Djurović ◽  
Matvei Zinkevich ◽  
Snezana Bošković ◽  
V. Srot ◽  
Fritz Aldinger

A nano-sized CeO2 powder was synthesized by a modified glycine nitrate process (MGNP). The synthesized powder was characterized by X-ray diffraction (XRD), the Brunauer Emmett Teller (BET) method, and transmission electron microscopy (TEM). The lattice parameter and crystallite size were determined by the Rietveld refinement of X-ray diffraction patterns. The shrinkage kinetics of the green body was continuously monitored in air and in oxygen atmospheres using a high temperature dilatometer up to 1500°C. During the high temperature sintering in air a redox reaction occurred (Ce4+ was partially reduced to Ce3+, and oxygen gas was released). The redox reaction influenced the sintering behaviour of CeO2, resulting in a decrease in density. On the basis of shrinkage kinetics data in oxygen atmosphere a master sintering curve for CeO2 was constructed. Using the concept of the master sintering curve, the densification behaviour in oxygen atmosphere was successfully predicted from early to final stages of sintering. During sintering of CeO2 at lower temperature in air atmosphere a significant contribution of the surface diffusion was observed.

2020 ◽  
Vol 28 ◽  
pp. 14-19
Author(s):  
Zamir V. Shomakhov ◽  
Akhmed M. Karmokov ◽  
Oleg A. Molokanov ◽  
Olga O. Molokanova ◽  
Rita Y. Karmokova ◽  
...  

Studies of the temperature dependence of the electrical properties of glasses show that the high-temperature annealing in glasses observed irreversible processes. These processes lead to changes in electrical conductivity, dielectric permittivity, and hence the electrical capacitance, dielectric loss tangent, and other parameters. Obviously, this is due to structural changes in the glass as a result of high-temperature annealing. In this regard, this paper presents studies of structural and phase transformations in glasses used for the production of microchannel plates in the process of high-temperature annealing in vacuum and in the air atmosphere at different times. The studies were conducted by x-ray phase and X-ray diffraction analysis, as well as X-ray fluorescence elemental analysis.


2019 ◽  
Vol 34 (3) ◽  
pp. 242-250 ◽  
Author(s):  
J. Anike ◽  
R. Derbeshi ◽  
W. Wong-Ng ◽  
W. Liu ◽  
D. Windover ◽  
...  

Structural characterization and X-ray reference powder pattern determination have been conducted for the Co- and Zn-containing tridymite derivatives Ba(Co1−xZnx)SiO4 (x = 0.2, 0.4, 0.6, 0.8). The bright blue series of Ba(Co1−xZnx)SiO4 crystallized in the hexagonal P63 space group (No. 173), with Z = 6. While the lattice parameter “a” decreases from 9.126 (2) Å to 9.10374(6) Å from x = 0.2 to 0.8, the lattice parameter “c” increases from 8.69477(12) Å to 8.72200(10) Å, respectively. Apparently, despite the similarity of ionic sizes of Zn2+ and Co2+, these opposing trends are due to the framework tetrahedral tilting of (ZnCo)O4. The lattice volume, V, remains comparable between 626.27 Å3 and 626.017 (7) Å3 from x = 0 to x = 0.8. UV-visible absorption spectrum measurements indicate the band gap of these two materials to be ≈3.3 and ≈3.5 eV, respectively, therefore potential UV photocatalytic materials. Reference powder X-ray diffraction patterns of these compounds have been submitted to be included in the Powder Diffraction File (PDF).


2020 ◽  
Vol 1010 ◽  
pp. 65-70
Author(s):  
Zahraa Zulnuraini ◽  
Noraziana Parimin

This paper investigates the performance of Fe-33Ni-18Cr alloy at high temperature oxidation. The samples were isothermally oxidized at three different oxidation temperatures, namely, 600 °C, 800 °C and 1000 °C for 150 hours. This alloy was ground by using several grits of SiC paper as well as weighed by using analytical balance and measured by using Vernier caliper before oxidation test. The characterization was carried out using scanning electron microscope (SEM) equipped with energy dispersive x-ray (EDX) and x-ray diffraction (XRD). The results show that, the higher oxidation temperatures, the weight gain of the samples were increase. Sample of 1000 °C indicate more weight gain compared to samples oxidized at 600 °C and 800 °C. The kinetic of oxidation of all samples followed the parabolic rate law. The surface morphology of oxide scale at lower temperature is thin and form a continuous layer, while at high temperature, the oxide scale develops thick layer with angular oxide particles.


2017 ◽  
Vol 31 (33) ◽  
pp. 1750318 ◽  
Author(s):  
D. Venkatesh ◽  
K. V. Ramesh

Polycrystalline Cu substituted Ni–Zn ferrites with chemical composition Ni[Formula: see text]Zn[Formula: see text]-Cu[Formula: see text]Fe2O4 (x = 0.00 to 0.25 in steps of 0.05) have been prepared by citrate gel autocombustion method. The samples for electrical properties have been sintered at 900[Formula: see text]C for 4 h. The X-ray diffraction patterns of all samples indicate the formation of single phase spinel cubic structure. The value of lattice parameter is decreases with increasing Cu concentration. The estimated cation distribution can be derived from X-ray diffraction intensity calculations and IR spectra. The tetrahedral and octahedral bond lengths, bond angles, cation–cation and cation–anion distances were calculated by using experimental lattice parameter and oxygen positional parameters. It is observed that Cu ions are distributed in octahedral site and subsequently Ni and Fe ions in tetrahedral site. The grain size of all samples has been calculated by Scanning Electron Microscopy (SEM) images. The variations in DC electrical resistivity and dielectric constant have been explained on the basis of proposed cation distribution.


2012 ◽  
Vol 727-728 ◽  
pp. 982-987
Author(s):  
E. de Carvalho ◽  
Marcelo Bertolete ◽  
Izabel Fernanda Machado ◽  
E.N.S. Muccillo

Polycrystalline CaCu3Ti4O12 ceramics were prepared by solid state reactions by spark plasma sintering (SPS) technique. In this study, the effects of the dwell temperature on structural, microstructural and dielectric properties of CaCu3Ti4O12 ceramics have been investigated. Powder mixtures were calcined at 900°C for 18 h before SPS consolidation. The dwell temperatures were 850, 900, 915 and 930°C. Sintered pellets were characterized by X-ray diffraction, scanning electron microscopy and impedance spectroscopy. X-ray diffraction patterns show evidences of a single-phase perovskite-type structure. The calculated lattice parameter is 7.40 Å. The hydrostatic density increases slightly with increasing dwell temperature. Scanning electron microscopy observations revealed a heterogeneous microstructure for all samples. The dielectric loss remains constant over a wide temperature range. The obtained permittivity is approximately 103 at 1 kHz. The increase of the dwell temperature is found to produce a brittle ceramic.


2018 ◽  
Vol 71 (11) ◽  
pp. 914
Author(s):  
Yanfang Xia ◽  
Min Liu ◽  
Duxin Li

Co0.76Cu0.74[Fe(CN)6]·7.5H2O was prepared as a powder by a chemical co-precipitation method. The powder X-ray diffraction patterns were indexed to the typical face-centred cubic structure with the lattice parameter a 10.55(2) Å. The temperature dependence of the χ−1 curve obeys the Curie–Weiss law (χ = C/(T – θ)) in the temperature range of 180–300 K. According to Curie–Weiss law, the calculated θ value is −54.82 K. In the paramagnetic state at 300 K, the effective magnetic moment (μeff = (8χT)1/2) is 3.58 μB per formula unit. The calculated theoretical effective magnetic moment is 4.06 μB. The magnetic field cooling measurements under a 200 Oe applied magnetic field show that the saturation magnetization value at 2 K of the complex Co0.76Cu0.74[Fe(CN)6]·7.5H2O is 1.528 emu g−1.


2007 ◽  
Vol 280-283 ◽  
pp. 259-262 ◽  
Author(s):  
Lina Zhang ◽  
Su Chuan Zhao ◽  
Liao Ying Zheng ◽  
Guo Rong Li ◽  
Qing Rui Yin

A study was conducted on the effects of donor dopants, Nb2O5 and WO3, on microstructure and electric properties of Bi4Ti3O12 (BIT) ceramics. X-ray diffraction patterns of the materials showed a single orthorhombic phase structure. The microstructure results revealed the appearance of plate-like grain. The donor doping decreased the conductivity of BIT by as much as 3 orders of magnitude. The dielectric and ferroelectric properties of doped-BIT materials were also investigated. The decrease in the electrical conductivity allowed the doped samples to be poled to develop piezoelectricity. Thermal annealing studies of the samples indicated the donor-doped BIT were suitable candidate materials for high-temperature piezoelectric applications.


MRS Advances ◽  
2016 ◽  
Vol 1 (62) ◽  
pp. 4133-4137 ◽  
Author(s):  
E. Epifano ◽  
R. C. Belin ◽  
J-C Richaud ◽  
R. Vauchy ◽  
M. Strach ◽  
...  

ABSTRACTIn the frame of minor actinide recycling, (U,Am)O2 are promising transmutation targets. To assess the thermodynamic properties of the U-Am-O system, it is essential to have a thorough knowledge of the binary phase diagrams, which is difficult due to the lack of thermodynamic data on the Am-O system. Nevertheless, an Am-O phase diagram modelling has been recently proposed by Gotcu. Here, we show a recent investigation of the Am-O system using in-situ High Temperature X-ray Diffraction under controlled atmosphere. By coupling our experimental results with the thermodynamic calculations based on the Gotcu model, we propose for the first time a relation between the lattice parameter and the departure from stoichiometry.


1989 ◽  
Vol 169 ◽  
Author(s):  
Ashok Kumar ◽  
L. Ganapathi ◽  
J. Narayan

AbstractWe have prepared highly textured superconducting thin films from Bi1.5pb0.5Ca3Sr2Cu4Ox (2324) on (100) YS-ZrO2 (Yttria stabilized zirconia) and Bi1.5Pb0.5Ca2Sr2Cu3°x (2223) on LaAlC-3 (100) and MgO (100) substrates at 650°C by pulsed laser ablation method.These films showed 2212 type of phase of the (BiPb)2(Ca,Sr)n+1CunO2n+4+5 family with onset transition temperature ( Tc ) ~ 110 K, confirming our earlier observations of 110 K superconductivity in a n = 2 bulk material. Thin films deposited from 2324 bulk target on YS-Z1O2 showed zero resistance temperature (Tco ) of 68 K but post annealing for one hour at 400°C in oxygen improved Tco from 68 K to 82 K. Thin films from 2223 target on LaAlO3 ( 100 ) and MgO ( 100 ) exhibited a Tco of 65 K and 74 K respectively while onset remained the same at 110 K. Further annealing at 400°C for one hour in oxygen did not show any improvement in Tco. X-ray diffraction (XRD), scanning electron microscopy (SEM) and Rutherford backscattering (RBS) channeling studies were performed on these films for correlation between crystal structure, microstructure and superconducting properties. X-ray diffraction patterns indicated 2212 type phase with a= 5.39 Å and c=30.76 Å; preferential orientation of c-axis perpendicular to the substrate was observed. The lattice parameter and x-ray diffraction patterns were found to be invariant with annealing treatments.


1999 ◽  
Vol 14 (1) ◽  
pp. 31-35 ◽  
Author(s):  
J. M. Loezos ◽  
T. A. Vanderah ◽  
A. R. Drews

Experimental X-ray powder diffraction patterns and refined unit cell parameters for two barium hollandite-type compounds, BaxFe2xTi8−2xO16, with x=1.143 and 1.333, are reported here. Compared to the tetragonal parent structure, both compounds exhibit monoclinic distortions that increase with Ba content [Ba1.333Fe2.666Ti5.334O16: a=10.2328(8), b=2.9777(4), c=9.899(1) Å, β=91.04(1)°, V=301.58(5) Å3, Z=1, ρcalc=4.64 g/cc; Ba1.143Fe2.286Ti5.714O16: a=10.1066(6), b=2.9690(3), c=10.064(2) Å, β=90.077(6)°, V=301.98(4) Å3, Z=1, ρcalc=4.48 g/cc]. The X-ray powder patterns for both phases contain a number of broad, weak superlattice peaks attributed to ordering of the Ba2+ ions within the tunnels of the hollandite framework structure. According to the criteria developed by Cheary and Squadrito [Acta Crystallogr. B 45, 205 (1989)], the observed positions of the (0k1)/(1k0) superlattice peaks are consistent with the nominal x-values of both compounds, and the k values calculated from the corresponding d-spacings suggest that the Ba ordering within the tunnels is commensurate for x=1.333 and incommensurate for x=1.143. High-temperature X-ray diffraction data indicate that the x=1.333 compound undergoes a monoclinic→tetragonal phase transition between 310 and 360 °C.


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