Molten salt synthesis of YAlO3 powders

In this work, the molten salt synthesis technique was applied to the synthesis of YAlO₃ powder using LiCl, NaCl or KCl salt as the flux. YAlO₃ powder was synthesized by reacting equimolar amounts of Y₂O₃ and Al₂O₃ powders in LiCl salt. The synthesis temperature for YAlO₃ using LiCl salt was 1300 °C which is by about 500 °C lower than that in the conventional mixed-oxide method. The synthesized powders have been characterized using powder X-ray diffraction (XRD) analysis and field emission scanning electron microscopy (FE-SEM). The effect of the salt type on the formation of YAlO₃ has also been investigated.     

Nonhydrolytic sol-gel synthesis and characterization of YAG

Yttrium–aluminum oxides are interesting compounds, which are widely used as hosts for lasers and phosphors due to their stable physical and chemical properties. The manufacture of YAG has been investigated thoroughly. YAG powders are traditionally synthesized through the reaction of aluminum and yttrium powders at high temperatures. The work reported here involved an investigation into the preparation of YAG by a nonhydrolytic sol-gel route and the influence of heating time at low temperatures to obtain YAG from inorganic precursors (yttrium and aluminum chloride). AlCl₃, YCl₃ and ethanol were reflux reacted under an argon atmosphere. Europium III chloride was added as a structural probe. The powder was treated at 800 °C for 1, 2, 4, 8 and 16 h. The YAG structure was analyzed by X-ray diffraction (XRD), nuclear magnetic resonance (NMR), thermal analysis (TA) and photoluminescence (PL). The XRD revealed only peaks corresponding to the YAG phase. PL data showed that the YAG phase was formed in 2 min with samples pretreated at 50 °C. For the samples pretreated at 800 °C, the YAG phase appeared in 30 s. The excitation spectra presented a maximum of 394 nm corresponding to the ⁵L₆ level, while the emission spectra of Eu III ions showed characteristic transition bands arising from the ⁵D₀ → ⁷F _J (J = 1, 2, 3, 4) manifolds at maximum excitation. The magnetic dipole ⁵D₀ → ⁷F₁ transition exhibited greater intensity than the electric dipole ⁵D₀ → ⁷F₂ transition. This methodology proved efficient for obtaining YAG phase.     

Ca3CO2O6的柠檬酸盐溶胶-凝胶合成、表征及电学性能

具有一维Co-O链的Ca3CO2O6是一类新型高温热电材料。通过柠檬酸盐溶胶-凝胶法合成粉体，采用常压烧结方式制备陶瓷体。结果表明，在700℃煅烧干凝胶就可以生成片状的Ca3CO4O9晶体，随着煅烧温度的升高，在850℃保温2h的条件下，Ca3CO4O9基本转化为短棒状的Ca3CO2O6晶体。Ca3CO2O6为P型半导体，电阻率随着温度的升高而降低，Sccbcck系数随着温度的升高而增加，功率因子也呈现单调增加。     

Spherical SiO2 @ GdPO4: Eu3+ core-shell phosphors: sol-gel synthesis and characterization

Nanocrystalline GdPO4 : Eu3+ phosphor layers were coated on non-aggregated, monodisperse and spherical SiO2 particles by Pechini sol-gel method, resulting in the formation of core-shell structured SiO2 @ GdPO4 : Eu3+ particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), time-resolved PL spectra and lifetimes were used to characterize the core-shell structured materials. Both XRD and FT-IR results indicate that GdPO4 layers have been successfully coated on the SiO2 particles, which can be further verified by the images of FESEM and TEM. Under UV light excitation, the SiO2 @ GdPO4 : Eu3+ phosphors show orange-red luminescence with Eu3+ 5D0-7F1 (593 nm) as the most prominent group. The PL excitation and emission spectra suggest that an energy transfer occurs from Gd3+ to Eu3+ in SiO2 @ GdPO4 : Eu3+ phosphors. The obtained core-shell phosphors have potential applications in FED and PDP devices.     

溶胶-凝胶法制备钛酸钡陶瓷纤维

首次采用乙酰丙酮作为钛醇盐的稳定剂，醋酸钡和钛酸丁酯为原料，无水乙醇-冰醋酸作为溶剂，用sol-gel法制备了长达50cm的BaTiO3凝胶纤维。用FT-IR、XRD、TGA．DTA、SEM等手段对凝胶纤维或陶瓷纤维进行一系列表征，最终得到单一钙钛矿相钛酸钡陶瓷纤维，纤维直径4～10μm，具有椭圆形截面。     

The synthesis,characterization and sintering of sol-gel derived cordierite ceramics for electronic applications

Cordierite ceramics were synthesized by sol-gel processing using alkoxides and acetate with an aim to use the material as substrate and packaging material. Preparation conditions were optimized by varying the amount and pH of water added and the amount of acetic acid as chelating agent. The powders were characterized by different analytical techniques such as thermogravimetric analysis, differential thermal analysis, surface area by BET, X-ray diffraction, transmission and scanning electron microscopies and infrared spectroscopy. The best product was obtained using 19.6 mol water and 0.34 mol acetic acid with respect to silicon ethoxide. The pH of the water added did not make any significant difference. Sintered materials were characterized by measuring different physical properties such as density, electrical and dielectric properties, thermal expansion, microstructure and composition. Well-sintered bodies could be achieved at 1000 °C in air with a soaking time of 2 h having a density of 99% theoretical, electrical resistivity of 10¹⁴ cm, dielectric constant of 5, dielectric loss 0.008 and thermal expansion coefficient of 28.5 × 10^–7 °C^–1, 25–200 °C. X-ray diffraction studies show the phase evolution in these materials is predominantly -cordierite (hexagonal high cordierite) and some -quartz. SEM reveals a uniformly dense microstructure with crystals of granular habit. X-ray photoelectron spectroscopy indicates that the surface composition of the sintered material is slightly enriched with aluminium and deficient in silicon.     

Preparation and characterization of sol-gel derived ZnTiO3 nanocrystals

Nanometer scale cubic ZnTiO₃ has been synthesized by sol-gel method at a lower temperature (600 °C). X-ray diffraction (XRD) analysis shows that the average crystalline size of the sample is ∼8-10 nm. The cubic to hexagonal phase transition of ZnTiO₃ is clearly observed from the XRD patterns of the sample. The thermal behavior of the sample was characterized by the thermogravimetric/differenthermal analysis (TG/DTA), XRD patterns, and the infrared spectra (IR). Transmission electron microscope (TEM) observations of the sample reveal a high microstructural uniformity.     

Synthesis and characterization of Al2O3 catalyst carriers by sol-gel

The sol-gel method has been used to synthesize alumina powder with high surface area from boehmite. The characteristics of the final powder product have been systematically studied in light of the preparation method and starting materials by fractional factorial design. The results show that the type of precursor and pH of the precursor sol are the most important parameters for the textural properties of the calcined alumina powder. When the calcination temperature is increased the type of precursor loses its significance, while the pH still has decisive importance after calcination at 1000°C, on pore volume and surface area. There is also a significant combined effect of several parameters on the surface area and the pore volume. The electrophoretic mobility, agglomerate size and size distribution have been determined as a function of the pH for one type of boehmite sol. The relation between characteristics of the precursor and powder properties is clearly emphasized.     

First-principles calculations of mechanical and thermodynamic properties of YAlO3

First-principles calculations are performed to investigate the crystal structure, electronic properties, the elastic properties, hardness and thermodynamic properties of YAlO₃. The calculated ground-state quantities such as lattice parameter, bulk modulus and its pressure derivative, the band structure and densities of states were in favorable agreement with previous works and the existing experimental data. The elastic constants C_ij, the aggregate elastic moduli (B, G, E), the Poisson’s ratio, and the elastic anisotropy have been investigated. YAlO₃ exhibits a slight elastic anisotropy according to the universal elastic anisotropy index A^U = 0.24. The estimated hardness for YAlO₃ is consistent with the experimental value, and Al–O bond in AlO₆ octahedra plays an important role in the high hardness. The Y–O bonds in YO₁₂ polyhedra exhibit different characteristic. Using the quasi-harmonic Debye model considering the phonon effects, the temperature and pressure dependencies of bulk modulus, heat capacity and thermal expansion coefficient are investigated systematically in the ranges of 0–20 GPa and 0–1300 K.     

钛酸锶钡(BaxSr1-xTiO3)陶瓷制备及其介电性能的研究

采用乙酸钡、乙酸锶和钛酸丁酯为原料的溶胶凝胶方法制备了BaxSn1-xTiO3(x=0．6)超细粉体,将BST超细粉体压制成型,进行烧结,得到(Ba0.6Sr004)TiO3陶瓷。通过热分析(DSC／TG)、X射线衍射(XRD)分析(Ba0.6Sr0.4)TiO3粉体合成过程及其相结构变化。采用扫描电子显微镜(SEM)描述(Ba0.6Sr0.4)TiO3烧结体的相结构和显微组织结构变化。阻抗分析仪测量(Ba0.6Sr0.4)TiO3陶瓷的-50～100℃介电温谱。实验结果表明BaxSn1-xTiO3粉体的相结构为立方相钙钛矿结构,其合成温度及烧结温度分别为800℃及1250℃,均低于传统工艺的相应温度。(Ba0.6Sr0.4)TiO3陶瓷在-50～100℃温度范围内,其电容率随着烧结温度升高而增大.介电损耗tgδ在-50～100℃温度范围内,随温度的增加而降低。1250℃的(Ba0.6Sr0.4)TiO3陶瓷烧结体样品存在介电峰弥散化。     

溶胶凝胶法制备钛酸锶钡(Ba1-xSrx)TiO3陶瓷及其介电性能的研究

采用硝酸钡、硝酸锶、钛酸丁酯和柠檬酸为原料的配合物溶胶凝胶方法制备了(Ba1-xSrx)TiO3(BST)陶瓷.实验结果表明,BST粉体合成温度及烧结温度分别为700及1250℃,均低于传统工艺的相应温度. Sr含量x≥0.40,(Ba1-xSrx)TiO3陶瓷的相结构为立方钙钛矿相;Sr含量x＜0.40,(Ba1-xSrx)TiO3陶瓷的相结构为四方钙钛矿型. (Ba1-xSrx)TiO3(0.5≤x≤0.70)陶瓷的电容率随温度变化曲线,说明存在由铁电四方相到顺电立方相的相变.且随锶(Sr)的摩尔量x的增加,(Ba1-xSrx)TiO3陶瓷样品的相变温度向低温方向移动,相变温度Tc的移动关系为Tc=394.1-272.6x(K).     

Preparation and characterization of ultra-thin sol-gel films

The formation and characterization of nanometer thick sol-gel films are reported. The films were prepared by spin-coating of a diluted solution of a silane precursor on a number of different substrates. The effect of dilution, rotation speed and nature of substrate on the thickness and homogeneity of the films was examined. Characterization of the films was carried out by profilometry, reflectance spectroscopy, atomic force microscopy, adhesion test and electrochemistry. We find that the dilution factor has a pronounced effect on the film thickness. Moreover, the time of dilution, namely, whether dilution was carried out before or after a period of hydrolysis, has a noticeable effect on the thickness as well as on the permeability of embedded species.     

Microscopic characterization of sol-gel processed cordierite

Different analytical techniques have been used to characterize green and sintered sol-gel processed cordierite on a microscopic scale. The sintered material, although identified macroscopically as -cordierite, contains many small precipitates of different chemical composition. Larger precipitates, characterized by an increased Mg concentration, result from inhomogeneities in the precursor gel. Smaller precipitates, identified as mullite and spinel, could not be related to gel heterogeneities. The amorphous phase surrounding the cordierite grains and the precipitates is Mg depleted and Si enriched. Neither -cordierite nor -cordierite were observed; slight variations of the -cordierite lattice parameters are attributed to some local perturbations due to a slight departure from stoichiometry or Si, Al ordering on tiny domains.     

柠檬酸溶胶凝胶法制备CaMnO3热电粉体及其表征

n型钙钛矿结构的CaMnO3热电氧化物是目前极有应用潜力的新型高温热电材料.利用Ca(NO3)2·2H2O、Mn(NO3)2为起始原料,去离子水为溶剂,加入适量乙二醇,以柠檬酸为络合剂,制备了CaMnO3溶胶.通过煅烧干凝胶前驱物制得了钙钛矿型CaMnO3多晶体粉末.利用TG-DTA、XRD、FT-IR及SEM分析了所得产物.结果表明,干凝胶前驱物经过950℃煅烧5h,可制得单一钙钛矿型CaMnO3多晶粉末.     

Synthesis and characterization of novel polyacrylate-clay sol-gel materials

Organo-functional silanes which were able to form chemical bonds with kaolinite and could also have an affinity to the materials of concern here, were studied by the sol-gel process. Polymethacrylate with trialkoxy silyl functional groups were prepared, hydrolysed and co-condensed with kaolinite. The progress of the hydrolysis, which proceeded very slowly, was followed by Karl-Fischer titration. Thermal behavior was investigated by differential thermal analysis. The extent of the reaction leading to network formation was qualitatively followed by Fourier transform-infrared spectroscopy and X-ray diffraction. Free-radical polymerization was carried out ultrasonically in the presence of a catalyst. Trimethoxy silane end-capped silane was found to be covalently bonded to kaolinite. The copolymers, with various amounts of kaolinite, were then hydrolysed and co-condensed in the presence of a catalyst to yield sol-gel materials which have a controllable combination of properties of both the polymer and kaolinite.     

The sol-gel process synthesis of GdAl3(BO3)4:Eu3+ nanophosphors

GdAl3(BO3)4:Eu3+ red phosphors were prepared using citric acid as complex agent by sol-gel technique. The preparation conditions of the precursor synthesis, including crystallization temperature and crystallization time were investigated. Their structure and luminescence properties were characterized by X-ray diffraction (XRD) analysis and fluorescence spectrometry. The results showed that GdAl3(BO3)4:Eu3+ phosphor crystallized at 960 degrees C for 2 h have been synthesized by sol-gel method. The phosphor is distributed into hexagonal system and the lattice parameters are a = 9.2992 nm c = 7.2577 nm. The excitation spectrum of Gd(0.95)Al3(BO3)4:Eu(0.05)3+ samples is complex and the frequency scale is wide. It consists of a number of main excitation transitions namely 8S(7/2) --> 6IJ (270 nm) of Gd3+, and the others 7F0 --> 5L6 (400 nm), 7F0 --> 5D2 (472 nm) and 7F0 --> 5D1 (542 nm) of Eu3+. The main emission peaks are 614 nm and 619 nm, which are the characteristic emission peaks of Eu3+. These emission peaks correspond to the transition from 5D0 to 7F2 of Eu3+. The shape and the wavelength range of the emission spectrum are similar when the sample was excited by different excitation spectrum. Only the relative intensity of the emission peaks is different from each other.     

Luminescent properties of YAlO3:Mn single crystalline films

The YAP:Mn single crystalline films (SCF) have been crystallized by liquid phase epitaxy (LPE) method onto YAP substrates. The cathode- (CL) and photo-luminescence (PL) spectra of the YAP:Mn SCF were analyzed for determination of the preferable valence states of manganese ions which are realized in these SCF depending on Mn content in the 0.01–0.81 at.% range. The thermoluminescence (TL) properties of YAP:Mn SCF with the different Mn content above the RT range were also examined in comparison with the properties of YAP:Mn single crystal counterpart. We show that YAP:Mn (0.01 at.%) SCF possesses effective TL properties both under α-particle and γ-quanta excitation with main TSL peaks at 130 and 195 °C. We assume that the different valence states of Mn ions are responsible for their TL properties, e.g. both emission and trapping centers in YAP:Mn are formed mainly by the different valence states of Mn ions.     

Preparation of silane-WO3 film through sol-gel method and characterization of photochromism

The sol of silane and WO₃ was prepared from tetraethyl orthosilicate (TEOS) and methacryloxy-propyl-trimethoxy silane (KH570) with a novel route as described in previous work, and the aqueous WO₃ solution was prepared from ammonium tungstate. These two sols were mixed by stirring for about 1 hour with a certain ratio. Through sol-gel method, the transparent hybrids coating of organic silane and tungsten oxide was prepared by spraying or dipping on the glass substrates, and then were heat-treated at a certain temperature. The photochromic properties were investigated. AFM was used to investigate the surface structure of the prepared coatings. The crystalline phase was studied through X-ray diffraction. UV lights with different wavelengths were used to get the coloration of the film. The results show that silane-WO₃ film exhibits better photo-chromic properties under UV light irradiation.