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1.
The synthesis of zirconia nanoparticles is achieved through a modified facile sol–gel route. The as-prepared gel is analyzed thermally using TGA and DTA techniques to spot the crystallization process of zirconia nanoparticles. The prepared gel is then annealed at different temperatures and the structure was found to change between tetragonal and monoclinic crystal systems. The first stable tetragonal phase is achieved after annealing for 2?h at 400°C. The annealed powders between 600°C and 800°C demonstrate mixed tetragonal/monoclinic phases. Annealing at 1000°C and higher temperatures up to 1200°C resulted in pure monoclinic phase. Cubic phase was not detected within the annealing temperature range in this study. The elemental analysis of the annealed powder confirmed the formation of zirconia nanoparticles with the chemical formula ZrO2. The FTIR spectra of the annealed samples introduced a variation in the vibrational bands especially around the phase transition temperature. HR-TEM images reported the formation of nano-zirconia crystals with apparently large particle sizes. The optical energy gap of zirconia nanoparticles is investigated and determined. 相似文献
2.
The electrical conductivity of ZrO2 doped with Co3O4 has been measured at various temperatures for different molar ratios. The conductivity increases due to the migration of vacancies created by doping. The conductivity is also found to increase with rise in temperature up to 120°C, and after attaining a maximum the conductivity decreases due to a collapse of the lattice framework. A second rise in conductivity around 460°C in all the compositions confirms the phase transition in ZrO2 from monoclinic to tetragonal symmetry. X-ray powder diffraction and DTA studies were carried out for confirming the doping effects and the transition in ZrO2. 相似文献
3.
S. Abermann C. Henkel O. Bethge G. Pozzovivo P. Klang E. Bertagnolli 《Applied Surface Science》2010,256(16):5031-5034
The impact of the ZrO2/La2O3 film thickness ratio and the post deposition annealing in the temperature range between 400 °C and 600 °C on the electrical properties of ultrathin ZrO2/La2O3 high-k dielectrics grown by atomic layer deposition on (1 0 0) germanium is investigated. As-deposited stacks have a relative dielectric constant of 24 which is increased to a value of 35 after annealing at 500 °C due to the stabilization of tetragonal/cubic ZrO2 phases. This effect depends on the absolute thickness of ZrO2 within the dielectric stack and is limited due to possible interfacial reactions at the oxide/Ge interface. We show that adequate processing leads to very high-k dielectrics with EOT values below 1 nm, leakage current densities in the range of 0.01 A/cm2, and interface trap densities in the range of 2-5 × 1012 eV−1 cm−2. 相似文献
4.
ZrO2–mullite nanocomposites were fabricated by in-situ-controlled crystallization of Si–Al–Zr–O amorphous bulk at 800–1250°C. The structural evolution of the Si–Al–Zr–O amorphous, annealed at different temperatures, was studied by X-ray diffraction, infrared, Laser Raman spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy. The materials consisted of an amorphous phase up to 920°C at which phase separation of Si-rich and Al, Zr-rich clusters occurred. The crystalline phases of t-ZrO2 and mullite were observed at 950°C and 1000°C, respectively. Mullite with a tetragonal structure, formed by the reaction between Al–Si spinel and amorphous silica at low temperature, changed into an orthorhombic structure with the increase of temperature. It was the phase segregation that improved crystallization of the Si–Al–Zr–O amorphous bulk. The anisotropic growth of mullite was observed and the phase transformation from t-ZrO2 to m-ZrO2 occurred when the temperature was higher than 1100°C. 相似文献
5.
A.M. Torres-Huerta M.A. Domínguez-Crespo J.R. Vargas-García 《Applied Surface Science》2009,255(9):4792-4795
The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO2 thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces. 相似文献
6.
Bulk nanocomposites ZnO–SnO2–TiO2 were synthesized by solid-state reaction method. The X-ray diffraction patterns and Raman spectra of bulk nanocomposite as a function of sintering temperature (700 °C–1300 °C) indicate that the structural phases of SnO2 and TiO2 depend on the sintering temperature while the ZnO retains its hexagonal wurtzite phase at all sintering temperatures and SnO2 started to transform into SnO at 900 °C and completely converted into SnO at 1100 °C, whereas the titanium dioxide (TiO2) exhibits its most stable phase such as rutile at low sintering temperature (≤900°C) and it transforms partially into brookite phase at high sintering temperature (≥ 900 °C). The optical band gap of nanocomposite ZnO–SnO2–TiO2 sintered at 700 °C, 900 °C, 1100 °C and 1300 °C for 16 hours is calculated using the transformed diffuse reflectance ultra violet visible near infra red (UV–VisNIR) spectra and has been found to be 3.28, 3.29, 3.31 and 3.32 eV, respectively. 相似文献
7.
R. Yuvakkumar 《Phase Transitions》2015,88(9):897-906
Niobium oxide nanocrystals were successfully synthesized employing the green synthesis method. Phase formation, microstructure and compositional properties of 1, 4 and 7 days incubation treated samples after calcinations at 450 °C were examined using X-ray diffraction, Raman, photoluminescence (PL), infrared, X-ray photoelectron spectra and transmission electron microscopic characterizations. It was observed that phase formation of Nb2O5 nanocrystals was dependent upon the incubation period required to form stable metal oxides. The characteristic results clearly revealed that with increasing incubation and aging, the transformation of cubic, orthorhombic and monoclinic phases were observed. The uniform heating at room temperature (32 °C) and the ligation of niobium atoms due to higher phenolic constituents of utilized rambutan during aging processing plays a vital role in structural phase transitions in niobium oxide nanocrystals. The defects over a period of incubation and the intensities of the PL spectra changing over a period of aging were related to the amount of the defects induced by the phase transition. 相似文献
8.
9.
The nanocrystalline LaMnO3+δ perovskite was synthesized by the microwave-assisted glycothermal method and calcined at several temperatures up to 1500°C. The prepared samples were examined by the X-ray powder diffraction with the aim to show that LaMnO3+δ exhibits the size-induced structural phase transitions. The as-received nanocrystals of LaMnO3+δ are of tetragonal, pseudo-cubic symmetry not known for bulk material. The samples calcined at temperatures 750–1100°C have trigonal symmetry known from the high-temperature phase of LaMnO3 single crystal. The samples calcined from 1200°C to 1500°C have two phases: trigonal and orthorhombic. Thus, the observed phase sequence is inverted with respect to that of the bulk material, which is the characteristic of the size-induced mechanism of phase transitions in the nanocrystals. The critical crystallite sizes for both structural transitions were evaluated as 20 and 100?nm. 相似文献
10.
L.Y. Zhu 《Optics Communications》2008,281(9):2548-2551
Ni2+-doped ZrO2 precursor fibers were prepared via sol-gel technique by dry-spinning method and then heat-treated at different temperatures. The surface of the fibers is smooth with uniform diameter and no cracks have been observed by scanning electron microscopy (SEM). The emission intensity reaches a maximum value at 1 mol% Ni2+ because of the concentration quenching. The photoluminescence (PL) relative intensity is apparently intensifying with increasing temperature before 700 °C due to the crystallinity of the ZrO2 lattice improvement. The PL results show that the typical emission center is at 510 nm excited at 315 nm. 相似文献
11.
Zirconia (ZrO2) nanostructures of various sizes have been synthesized using sol–gel method followed by calcination of the samples from 500 to 700 °C. The calcined ZrO2 powder samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infra-red spectroscopy (FT-IR), UV–visible spectroscopy (UV–vis.), Raman spectroscopy (RS) and thermogravimetric analysis (TGA). The phase transformation from tetragonal (t) to monoclinic (m) was observed. The average diameter of the ZrO2 nanostructures calcined at 500, 600 and 700 °C was calculated to be 8, 17 and 10 nm, respectively. The ZrO2 sample calcined at 500 °C with tetragonal phase shows a direct optical band gap of 5.1 eV. The value of optical band gap is decreased to 4.3 eV for the ZrO2 calcined at 600 °C, which contains both tetragonal (73%) and monoclinic (27%) phases. On further calcination at 700 °C, where the ZrO2 nanostructures have 36% tetragonal and 64% monoclinic phases, the optical band gap is calculated to be 4.8 eV. The enhancement in optical band gap for ZrO2 calcined at 700 °C may be due to the rod like shape of ZrO2 nanostructures. The tetragonal to monoclinic phase transformation was also confirmed by analyzing Raman spectroscopic data. The TG analysis revealed that the ZrO2 nanostructure with dominance of monoclinic phase is found to be more stable over the tetragonal phase. In order to confirm the phase stability of the two phases of ZrO2, single point energy is calculated corresponding to its monoclinic and tetragonal structures using density functional theory (DFT) calculations. The results obtained by theoretical calculations are in good agreement with the experimental findings. 相似文献
12.
High-energy ball milling of monoclinic ZrO2–30 mol% anatase TiO2 mixture at different durations results in the formation of m-ZrO2–a-TiO2 solid solution from which the nucleation of nanocrystalline cubic (c) ZrO2 polymorphic phase sets in. Post-annealing of 12 h ball-milled sample at different elevated temperatures for 1 h results in almost complete formation of c-ZrO2 phase. Microstructure of the unmilled, all the ball milled and annealed samples has been characterized by Rietveld's X-ray powder structure refinement method. Particle size, rms lattice strain, change in lattice parameters and phase content of individual phases have been estimated from Rietveld analysis, and are utilized to interpret the results. In course of milling, (1 1 1) of cubic lattice became parallel to () plane of monoclinic lattice due to the orientation effect and cubic phase may have been formed on the (0 0 1) of the m-ZrO2–a-TiO2 solid solution lattice. A comparative study of microstructure and phase transformation kinetics of ZrO2–10, 20 and 30 mol% a-TiO2 ball-milled and post-annealed samples reveals that rate of phase transformation m→c-ZrO2 increases with increasing a-TiO2 concentration and 30 mol% of nanocrystalline c-ZrO2 phase can be obtained within 4 h of milling time in the presence of 30 mol% of a-TiO2. The post-annealing treatment at 773, 873 and 973 K for 1 h duration each reveals that rate of c-ZrO2 formation with increasing temperature is retarded with increasing a-TiO2 concentration but the amount of c-ZrO2 becomes almost equal (95 mol%) at 973 K. It suggests that almost fully stabilized nanocrystalline c-ZrO2 can be formed by adding a tetravalent solute to m-ZrO2. 相似文献
13.
The luminescence properties of LaNbO4 synthesized by the citric gel process were investigated. The crystallized orthorhombic and monoclinic biphasic structure forms at temperatures below 1100 °C and well-crystallized monoclinic LaNbO4 is obtained by heat treatment at a temperature of 1200 °C for 3 h. All of LaNbO4 phosphors derived from the citric gel method exhibit red-shifted excitation spectra as the calcining temperature increased from 700 to 1200 °C. The effect of the heat treatment conditions on the peak shape and the peak positions of the photoluminescence (PL) emission are undetectable, and the PL spectra excited at 260 nm have a blue emission band maximum at 408 nm, corresponding to the self-activated luminescence center of LaNbO4. The sample heat treated at 1100 °C for 3 h showed the highest absorption and fluorescence intensities among the prepared samples. 相似文献
14.
This paper presents the adsorption and thermal decomposition mechanism of formic acid on an H-birnessite sample. Changes in the surface and structure were characterized using infrared spectroscopy, N2 gas adsorption–desorption, and thermal analysis techniques. The acid sites of H-birnessite were investigated by infrared and thermal analysis using pyridine as a molecular probe. Decomposition of formic acid started on H-birnessite at 120°C and was complete at 400°C. Infrared spectra revealed that the molecularly adsorbed formic acid species were transformed to a formate species, and the formate species were transformed to CO. The most stable adsorption structure for formic acid was found as a molecular monodentate configuration. 相似文献
15.
《Current Applied Physics》2009,9(5):993-996
Single-phase cubic Ba(Fe,Nb)0.5O3 (BFN) powder was synthesized by solid-state reaction at 900, 1000, 1100, 1200 °C for 4 h in air. X-ray diffraction indicated that the BFN oxide mixture calcined at 1200 °C crystallizes to the pure cubic perovskite phase. The crystallite size of the BFN increases slightly with increasing temperature, while the lattice strain progressively decreases. BFN ceramics were produced from this powder by sintering at 1350–1400 °C for 4 h in air. Samples prepared under these conditions achieved up to 97.4% of the theoretical density. The temperature dependence of their dielectric constant and loss tangent, measured at difference frequencies, shows an increase in the dielectric constant with sintering temperature and measurement frequency which is probably due to disorder on the B site ion of the perovskite. The Mössbauer spectra of these sintered BFN ceramics suggests the presence of a superstructure on the B-cation sublattice. 相似文献
16.
Nickel-doped anatase TiO2 nanoparticles have been prepared by sol-gel method. The X-ray powder diffraction study reveals that all the prepared samples have pure anatase phase tetragonal system. The average crystallite size of the prepared sample is 14 nm, when found through transmission electron microscope. A strong frequency dependence of both dielectric constant (?′) and dielectric loss (tan δ) were observed for various dopant levels at room temperature in the frequency range of 42 Hz to 5 MHz. At low frequency, the piling up of mobile charge carriers at the grain boundary produces interfacial polarization giving rise to high dielectric constant. The asymmetric shape of frequency dependence of the dielectric loss for the primary relaxation process is observed for each concentration. From the ac conductivity studies, the reduction in conductivity may arise due to the decreasing particle with the increase in Ni-dopant level. 相似文献
17.
Tatsuo Nakagawa Satoshi Fukura Munenori Nakai Kazumasa Sugiyama Ryohei Kokawa Hiroyuki Kagi 《Optical Review》2006,13(4):269-275
We constructed a scanning near-field optical microscope (SNOM) on a commercially available atomic force microscopy (AFM) apparatus
(SPM-9500J2; Shimadzu Corp.) to measure the stress distribution in ceramic composite materials. Features of our SNOM system
are: (1) a compact SNOM head substituted for the original AFM head; (2) a wide scanning range (125 × 125 μm2) inherited from the original scanner; (3) use of conventional shear-force regulation; (4) an optical system for the illumination-collection
(I-C) mode; (5) excitation by a 488 nm line of an Ar-ion laser, and (6) light detection by photon counting or a polychromator
equipped with an electronically cooled charge coupled device (CCD). This SNOM system was used to measure the surface structure
and stress distribution of an Al2O3/ZrO2 eutectic composite. We simultaneously measured topographic images and fluorescence spectra of an Al2O3/ZrO2 eutectic composite. We estimated its peak intensity, peak position, and peak width from the fluorescence spectrum during
scanning, which respectively correspond to the abundance of Al2O3, stress in the grain, and the anisotropy of that stress. Mapping images showed that the stress and its anisotropy were weaker
in the center of the Al2O3 grain than its boundary between Al2O3 and ZrO2. That observation suggests that Al2O3 underwent intense anisotropic stress induced by volume expansion in the phase transition of ZrO2 from the cubic phase to the monoclinic phase during preparation. 相似文献
18.
ZrW2O8 as the typical negative thermal expansion (NTE) material has attracted much attention for the potential applications in various fields such as tailored coefficient of thermal expansion (CTE) composites. The hexagonal ZrW2O8 (h-ZrW2O8), with the combination of ZrO2 and WO3 in a composite, was synthesized at a pressure of 2 GPa and the temperature between 600°C and 700°C. We found h-ZrW2O8 decomposes to ZrO2+WO3 oxides that start from 500°C and end at 800°C, and determined the CTE of h-ZrW2O8 is?16.3×10?6°C?1 in the temperature range from 150°C to 450°C. The results show that ZrW2O8 with a hexagonal structure is metastable and exhibits high NTE property like its cubic structure. 相似文献
19.
采用传统的固相反应法,在1400–1500 ℃下烧结,制备得到Al2O3-Y2O3-ZrO2三相复合陶瓷.样品的结构、形貌和电性能分别用X射线衍射(XRD)、扫描电子显微镜(SEM)及介电谱表征.XRD表明此三相复合体系无其他杂相,加入Y2O3及ZrO2后使得Al2O3成瓷温度降低;SEM表明此体系晶粒直径为200–500 nm,并且样品随烧结温度的升高而变得更加致密,晶界更加清晰;介电损耗谱中出现峰值弛豫现象,根据Cole-Cole复阻抗谱得出其为非德拜弛豫.
关键词:
2O3-Y2O3-ZrO2三相陶瓷')" href="#">Al2O3-Y2O3-ZrO2三相陶瓷
介电弛豫
阻抗谱
热导率 相似文献
20.
Abstract A phase transition from Ca(OH)2 I (portlandite) to Ca(OH)2 II at high pressure and temperature has been confirmed, using in situ x-ray diffraction in a multianvil high pressure device (DIA). The structure was determined at 9.5 GPa and room temperature from data collected after heating the sample at 300°C at 7.2 GPa in a diamond anvil cell. Both the Le Bail fit and preliminary Rietveld refinement suggest that the new phase, which reverts to Ca(OH), I during pressure release, has a structure related to that of baddeleyite (ZrO1); it is monoclinic (P21/c) with a= 4.887(2), b= 5.834(2), c = 5.587(2), β = 99.74(2)°. The coordination number of Ca increases from six to seven (5 + 2) across the transition. At 500°C, the phase boundary is bracketed at 5.7 ± 0.4 GPa by reversal experiments performed in the DIA. 相似文献