Preparation of ferromagnetic binary alloy fine fibers by organic gel-thermal reduction process

Ferromagnetic metal fibers with a high aspect ratio (length/diameter) are attractive for use as high performance electromagnetic interference shielding materials. Ferromagnetic binary alloy fine fibers of iron-nickel, iron-cobalt and cobalt-nickel were prepared by the organic gel-thermal reduction process from the raw materials of critic acid and metal salts. These alloy fibers synthesized were featured with a diameter of about 1 μm and a length as long as 1 m. The structure, thermal decomposition process and morphologies of the gel precursors and fibers derived from thermal reduction of the gel precursors were characterized by FTIR, XRD, TG/DSC and SEM. The gel spinnability largely depends on the molecular structure of metal- carboxylates formed during the gel formation. The gel consisting of linear-type structural molecules shows good spinnability.

Thermal stability and luminescence properties of 1,10-phenanthroline-tris (m-methylbenzoate) europium (or terbium) complexes in SiO_2 gel

Silica gel luminophors containing 1, 10-phenanthroline-tris(M-Methylbenzoate) europium (or terbium) com- plexes were prepared bysol-gel method. The thermal decomposition, excitation and emissionspectra for the gel phos- phors were measured and compared with thatof solid complex powders. The thermal stability of the complexes wasen- hanced in SiO_2 host matrix and the luminescence intensityremained unchanged.

Metal Fe,Ni and Fe-Ni Fine Fibers Derived from the Organic Gel-Thermal Reduction Process

The organic gel-thermal reduction process was successfully used for the preparation of magnetic metal Ni, Fe, Fe-Ni fine fibers from raw materials of citric acid or lactic acid and metal salts. Ni, Fe and Fe-Ni fine fibers synthesized were featured with diameters of around 1 μm and lengths of as long as 2 m for Ni fibers, 0.5 m for iron fibers, 1 m for Fe-Ni fibers. The structure, thermal decomposition process and morphologies of the gel precursors and fibers derived from thermal reduction of these gel precursors were characterized by FTIR, XRD,TG/DSC and SEM, respectively. The gel spinnability largely depends on molecular structures of metal-carboxylate complexes formed in the gel. It is reasoned that these gels consist of linear-type structural molecules [（C6H6O7）Ni]n or [（C6H5O7）2Ni3] for the nickel citrate gel, [（C3H5O3）3Fe] for the ferric lactate gel, [（C6H5O7）5（NiFe）3] for the iron-nickel citrate gel respectively and the gels obtain showed a good spinning performance.

Synthesis of Nano-sized Yttria via a Sol-Gel Process Based on Hydrated Yttrium Nitrate and Ethylene Glycol and Its Catalytic Performance for Thermal Decomposition of NH_4ClO_4

Nano-sized yttria particles were synthesized via a non-aqueous sol-gel process based on hydrated yttrium nitrate and ethylene glycol. The effects of the molar ratio of ethylene glycol to yttrium ion and calcination temperature on crystallite size of the products were studied. The catalytic performance of the as-prepared yttria for the ammonium perchlorate （AP） decomposition was investigated by differential scanning calorimetry （DSC）. The results indicate that the nano-sized cubic yttria particles with less than 20 nm in average crystallite size can be obtained after 2 h reflux at 70℃, dried at 90 ℃, forming xerogel, and followed by annealing of xerogel for 2 h, and that the addition of the nano-sized yttria to AP incorporates two small exothermic peaks of AP in the temperature ranges of 310 - 350 ℃ and 400 - 470 ℃ into a strong exothermic peak of AP and increases the apparent decomposition heat from 515 to over 1110 J·g^- 1. It is also clear that the temperature of AP decomposition exothermic peak decreases and the apparent decomposition heat of AP increases with the increase of the amount of nano-sized yttria. The fact that the addition of the 5 % nano-sized yttria to AP decreases the temperature of AP exothermic peak to 337.7℃ by reduction of 114.6℃ and increases the apparent decomposition heat from 515 to 1240 J·g^-1, reveals that nano-sized yttria shows strong catalytic property for AP thermal decomposition.

Thermal Characteristics of Gel Grown Lanthanum Heptamolybdate crystals

Thermal characteristics of Ianthanum heptamolybdate crystals grown by gel technique, employing thermoanalytical techniques, viz. TG, DTA and DSC, are reported. It is established that the rare-earth lanthanum heptamolybdate crystals are associated with thirty water molecules;the composition being La2Mo7O24.3OH2O. It is shown that all the thirty water molecules associated with lanthanum heptamolybdate crystal are lost during its decomposition, leading to its anhydrous form. Results obtained on application of TG based models, viz. Horowitz-Metzger,Coats-Redfern and Piloyan-Novikova and of DSC based methods viz. Roger-Morris-Smith and Barret, regarding solid state reaction kinetics are also reported. The random nucleation model is shown to be the one that is relevant to the decomposition of lanthanum heptamolybdate. The kinetic parameters, viz.the order of reaction. frquency factor, energy of activation and entropy using above mentioned models are computed and shown to bear reasonably good agreement

Thermal aging behavior of high performance poly(vinyl alcohol) hydrogel

The thermal aging behavior of poly （ vinyl alcohol ） （ PVA ） hydrogel was studied at four different temperatures of 40 ℃, 50 ℃, 60 ℃ and 70 ℃ in one year. The samples of PVA hydrogel were closely covered by plastic film. The changes of their chemical structures and physical properties during aging were measured through different measurable techniques including tensile testing, gel permeation chromatography （ GPC ）, viscosity analysis, and Fourier transform infrared （FTIR） spec- trum. The results showed that the molecular weight of PVA in hydrogel changed little with time and temperature. FTIR spectra of PVA in all the samples were similar to those of the original samples. The tensile strength of PVA hydrogel didn＇t change until the 330th days.

Thermal relaxation and mechanical relaxation of rice gel

Rice gel was prepared by simulating the production processes of Chinese local rice noodles,and the properties of thermal relaxation and mechanical relaxation during gelatinization were studied by differential scanning calorimetry(DSC) measurement and dynamic rheometer.The results show that during gelatinization,the molecular chains of rice starch undergo the thermal relaxation and mechanical relaxation.During the first heating and high temperature holding processes,the starch crystallites in the rice slurry melt,and the polymer chains stretch and interact,then viscoelastic gel forms.The cooling and low temperatures holding processes result in reinforced networks and decrease the viscoelasticity of the gel.During the second heating,the remaining starch crystallites further melt,the network is reinforced,and the viscoelasticity increases.The viscoelasticity,the molecular conformation and texture of the gel are adjusted by changing the temperature,and finally construct the gel with the textural characteristics of Chinese local rice noodle.

Synthesis, Characterization and Thermal Stability of CeO_2 Stabilized ZrO_2 Ultra Fine Nanoparticles Via a Sol-gel Route

CeO_2 stabilized ZrO_2 ultra fine nanoparticles were successfully synthesized via a simple and effective sol-gel synthetic approach by using zirconylchloride octahydrate, cerium nitrate hexahydrate, and citric acid as starting materials. A series of techniques, including X-ray diffraction（XRD）, thermogravimetry（TG）, differential scanning calorimetry（DSC）, Fourier transform infrared spectroscopy（FTIR）, transmission electron microscopy（TEM）, and N_2-sorption analysis, were used to characterize the structure and morphology of the asprepared samples. XRD studies indicate that the as-synthesized sample is of well crystallized tetragonal phase of CeO_2 stabilized ZrO_2 with high purity. TEM images show that the as-synthesized sample is composed of a large number of fine dispersive nanoparticles with an average size about 10 nm. The as-synthesized tetragonal CeO_2 stabilized ZrO_2 sample was heated at different temperatures in order to evaluate its thermal stability. The exprimental results reveal that the as-synthesized tetragonal CeO_2 stabilized ZrO_2 sample exhibits excellent stability without the occurrence of phase transformation.

Thermal Stability and Luminescence Properties of Eu^(3+) and Tb^(3+) Complexes with a Silica Matrix by Sol-Gel Method

Ternary complexes of europium and terbium with benzoic acid and 1, 10 phenanthroline [RE(BA) 3phen] (BA=benzoate phen=1,10 phenanthroline) were introduced into a silica matrix by sol gel method. The thermal stability and luminescence behavior of the complexes in silica gels were studied in comparison with the corresponding solid state complexes by thermal decomposition, excitation and emission spectra. The thermal stability of the complexes is enhanced in silica gel matrix and the luminescence remaines unchanged.

纳米掺铁二氧化钛的sol-gel法制备与表征(Ⅰ)热重红外联用分析掺铁二氧化钛凝胶的热分解和晶化特性

本文通过热分析、红外联用和 X射线衍射分析了不同煅烧温度下的纳米掺铁二氧化钛样品，研究了 sol-gel方法制备的纯二氧化钛和掺铁二氧化钛干凝胶的热分解和晶化过程。结果表明，干凝胶有较为明显的两个阶段的热分解。在实验条件下得到的二氧化钛干凝胶粉为无定形，无定形二氧化钛加热晶化过程是一个持续的过程，没有明显的晶化温度。

基于非水解sol-gel法的碳热还原氮化合成氮化铝超细粉体

以无水氯化铝和异丙醚为原料,采用非水解溶胶-凝胶法制备出氧化铝凝胶。其经800℃煅烧才析出少量γ-Al2O3晶体,γ-Al2O3向α-Al2O3晶型转变在1200℃附近,经900℃煅烧后比表面积仍高达145m2/g,具有介孔结构。以该高活性氧化铝凝胶作为铝源,采用碳热还原氮化工艺合成氮化铝粉体。结果表明,氧化铝凝胶经300℃预煅烧,按n(C)/n(Al)=7.8与碳黑混合,在流量80mL/min高纯N2中,于1450℃还原氮化2h便可合成出平均粒径在400nm的高纯六方相AlN粉体。

PZT铁电薄膜Sol-Gel技术制备和电性能研究

以乙酸铅(Pb(CH3COO)2·3H2O)、钛酸四丁酯(Ti(OC4H9)4)、硝酸锆(Zr(NO3)4·5H2O)替代锆醇盐为原料,通过在Pt/Ti/siO2/si基片与PZT薄膜之间引入PT种子层,采用改进的sol-gel工艺制备出无裂纹,致密性好,晶粒尺寸小且分布均匀的单一钙钛矿结构的Pb(Zr0.53Ti0.47)O3铁电薄膜.实验结果表明,具有PT种子层的PZT铁电薄膜电性能较好.经600℃热处理的具有PT种子层的PZT薄膜,在1kHz测试频率下,其剩余极化强度和矫顽场分别为20μC/cm2和59kV/cm,介电常数和介电损耗分别为385和0.030.

快速退火Sol-Gel PZT铁电薄膜的性能研究

报道了以乙酸铅、乙酸氧锆和钛酸正丁酯为原料，用溶胶-凝胶（Sol-Gel）法，经多次旋转涂膜，在Pt／Ti／SiO2／Si衬底上制备了PZT凝胶薄膜。用快速退火（RTA）作薄膜的热解和结晶热处理，制备了以（100）取向为主的PZT薄膜。用X射线衍射（XRD）和RT66A测试了膜的结晶取向、漏电流、电滞回线和抗疲劳性能等。结果表明，经RTA处理的溶胶凝胶法PZT膜具有良好的性能。

PREPARATION OF HIGH THERMAL EXPANSION COEFFICIENT PORCELAINS FUSED TO METALS

Usually the thermal expansion coefficients (TEC) of metals are higher than that of porcelains. In order to match the TECs in the case of coating porcelains on metals, high TEC porcelains are needed. In this research, the high TEC phase leucite (KAlSi2 O6) in the high TEC porcelain was prepared by sol-gel method. The crystal size of leucite made by sol-gel is about 77nm through controlling the process parameters. The process from xerogel to leucite was investigated by means of DSC (differential scanning calorimetry), TG (thermogravimetry), XRD ( X-ray diffraction) and IR (infrared absorption spectrum). Leucite had been detected after the gel was treated at 900℃, this formation temperature is about 250℃ lower than that of melting method. The porcelain made from 50% of the leucite powder and 50% of low fused temperature frit has an average TEC of 19.2×10-6/℃ C from room temperature to 450℃, which is much higher than the common porcelains.

Preparation and characterization of BaMgAl_(10)O_(17)∶Eu phosphor coated with MgF_2 by sol-gel process

In order to prevent BaMgAl10O17∶Eu （BAM） phosphor from thermal degradation, MgF2-coatings on the surface of BAM were prepared by a sol-gel process. The coatings were characterized by X-ray photoelectron spectroscopy and scanning electron microscopy. The results indicate that BAM is successfully coated with homogenous, close MgF2 coatings. The photoluminescence and anti-thermal degradation properties of coated BAM were investigated under 254 and 147 nm excitations. The optimum anti-thermal degradation properties are obtained at the mass ratio of MgF2 to BAM 0.2% under 254 nm excitation and 0.5% under 147 nm excitation, respectively. It is considered that trace MgO formed after baked would cause different optimum coating thicknesses under 254 and 147 nm excitations.

Fullerenol-containing Materials Derived by Sol-gel Processing

Water soluble fullerenols were synthesized and incorporated in SiO2, SiO2-TiO2, GPTMS-SiO2, GPTMS-ATPS inorganic and organic-inorganic materials by sol-gel processes. The maximum concentrations of C60(OH)n and C70(OH)n in the obtained SiO2 gels were estimated to be about 0.6% and 1.5% in weight, respectively. The characteristics of the UV/visible spectra of fullerenols in H2O and various gels were measured and compared. The thermal stability of fullerenols in gels was investigated with differential thermal analysis (DTA). The results indicate that the absorption features of fullerenols in solid gels are similar to those in H2O and the fullerenols in SiO2 are stable at 400℃. The optical limiting effect of the fullerenols was investigated preliminarily.

Synthesis of Lithium-cobalt Oxides by Sol-gel Method and their Cathodical Discharge Behavior at 500 ℃

Three kinds of lithium cobalt oxides with lithium to cobalt atomic ratios of 0.6, 0.8 and 1.0 respectively were prepared using nitrates and citric acid by sol gel process. During the baking of the dry gel powder, two exothermic peaks occur, followed by the formation of Li 2O and Co 3O 4 and then the combination of LiCoO 2, which is testified by DTA and XRD. The powder formed from an alkaline sol is finer than that from the acidic one. There are a single phase intercalation of lithium ion and an electrochemical reduction reaction for higher valence cobalt ion when simulating the discharging process of Li B/LiCl KCl/lithium cobalt oxides at 500 ℃, and the voltage and specific capacity are not sensitive to the initial ratios of lithium to cobalt.

快速热处理中退火温度对Sol-gel法制备PZT铁电薄膜性能的影响

利用Sol-Gel法在Pt/TiO2/SiO2/Si基底上用快速热处理(Rapid Thermal Processing,RTP)退火工艺制备出了致密的PZT铁电薄膜,主要研究了在退火时间为500s时退火温度对薄膜的结晶结构、表面形貌和铁电性能的影响。通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)和铁电测试仪对制备的薄膜进行了性能表征。研究结果表明,当退火温度为6000C时,PZT薄膜具有(111)择优取向,表面致密无裂纹,且具有较好的铁电性能(其饱和极化值约为30 C/cm2,剩余极化约为20 C/cm2,矫顽场约为150KV/cm)。在100KV/cm电场下,电流密度J在10-1A/cm2数量级,表明所制的PZT纳米薄膜质量较好,能承受较高的场强以达到饱和极化状态而不被击穿。

Sol-gel Derived TiO_2-Bioactive glass-Hydroxyapatite Bioactive Coating on Titanium Alloy Substrate

Coating the hydroxyapatite （HA） on the titanium alloy surface can obtain a bioactive implant with high mechanical properties However, the bonding force between the titanium alloy and the HA was low due to their different coefficient of thermal expansion （CET）. Preparing the multi-layer coating with alleviated thermal stress on titanium alloy substrate is few reported. Fabrication of a TiO2-bioactive glass （BG）-HA bioactive coating was proposed to solve this problem. A particular TiO2 surface was prepared on the titanium alloy substrate by micro-arc oxidation treatment. The BG and HA coating were coated onto the TiO2 surface in turn by using a sol-gel method. The microstructure, surface morphology and phase composition of the coatings were analyzed. The bonding force of coatings was investigated by the nick apparatus. In vitro dissolution was performed by soaking the TiO2-BG-HA coated samples into the simulated body fluid for various periods. Micro-structural observations indicated that no delamination and crack occurred at the interface of HA/BG and BG/TiO2. The bonding between the substrate and coating consists of the mechanical interaction and the chemical bonding. The bonding force could reach about 45 N. The TiO2-BG-HA coating displayed the excellent forming ability of bone-like apatite when it was soaked into the simulated body fluid. This work suggests an innovative way to reduce the internal stress among coatings through varying BG composition to adjust its CTE, so as to enhance the bonding force.

Preparation of Light-weight Spinel Refractories by Foaming-gel Process

Light-weight magnesium -aluminate spinel materi- als were prepared by foaming-gel process with polyalumi- nium chloride （PAC） as gel. Effect of solid loading in initial slurry on microstructure, porosity, pore size distri- bution, thermal conductivity and mechanical properties was investigated. The results show that the bulk density of the light-weight magnesium -aluminate spinel mate- rials is in the range of O. 7 1.2 g cm-3 ; pore size distribution curves show single-peak characteristics and the mean pore size is in the range of 30. 83 - 61.37 μm ; with the increase of solid loading, the linear shrinkage of the green body during firing and the permanent change in dimensions on heating at l 600 ℃ for 3 h de- crease, but the bulk density increases, the mechanical properties increase obviously; the maximum compressive strength and bending strength reach 35. 25 MPa and 9. 92 MPa, respectively, while the bulk density is 1. 16 g · cm ; and the thermal conductivity at 1 000 ℃ tea- ches 0. 371 W · m-1 . K-1 while the bulk density is O. 7 -3 g · cm