溶胶-凝胶法在合成纳米La2Zr2O7中的应用

由L9(34)试验确立了溶胶-凝胶法(sol-gel)制备La2Zr2O7粉末最佳的反应条件,并初步讨论了各因子对凝胶质量的影响机理.采用XRD和TEM对产物进行了物相及结构分析,研究发现为具有烧绿石结构的La2Zr2O7单一相.     

表面改性剂在溶胶-凝胶法制备纳米氧化锌中的应用

以草酸与二水合醋酸锌为原料,采用溶胶-凝胶法制备纳米氧化锌。探讨了不同表面改性剂及其用量对氧化锌粉体的粒度、形貌及分散性的影响。利用SEM、TG、IR、XRD对氧化锌粉体进行了表征。结果表明十二烷基硫酸钠和聚乙二醇6000能有效地分散颗粒和控制颗粒的团聚。制得粒径在80 nm左右、纯度高、晶型良好、分散性好的纳米氧化锌。     

溶胶-凝胶法制备碳酸钙晶须

用溶胶-凝胶法制备碳酸钙晶须,研究恒温水浴温度、搅拌速度、热处理温度和时间对碳酸钙晶须形貌的影响,并对影响机理进行分析.制备时,首先在恒温水浴搅拌条件下把碳酸钙溶入乙酸,稍后加入柠檬酸得到含Ca中间体,最后加热保温使中间体分解获得碳酸钙晶须.研究表明,在水浴温度80℃,搅拌速度150 r/min,热处理温度700℃和保温2 h的条件下,可得到直径100～150 nm,长约4μm的碳酸钙晶须.     

溶胶-凝胶法制备的LaxSr1-xMnO3纳米粉末微波吸收特性研究

采用溶胶-凝胶法制备了稀土锰氧化物LaxSr1-xMnO3(x =0.5,0.7,0.9)纳米粉末,用XRD分析了该材料的相结构,并用AV3618型微波矢量网络分析仪测试了样品在8.2GHz～12.5GHz范围内的微波吸收特性.结果表明,在1000℃焙烧后样品出现单一的钙钛矿型结构,当材料涂层厚度为1mm、x=0.7时,La0.7Sr0.3MnO3的吸波性能最佳.在测试频段内有五个明显的吸收峰,最高吸收峰在11.2GHz处,其吸收峰值达34dB,20 dB以上频带宽度达3GHz,是一种有发展前景的微波吸收材料.     

超声波-溶胶-凝胶法制备纳米二氧化锡粉末

用超声波－溶胶－凝胶法制得了纳米SnO2粉末，用XRD和TEM等方法对粉末进行表征，并研究了超声场，pH值和洗涤方式对产品粒度与团聚的影响。     

硬脂酸溶胶凝胶法-共沸蒸馏法制备钙钛矿型纳米LaCoO3

用硬脂酸溶胶凝胶-共沸蒸馏法制备了纳米LaCoO3,用差热-热重、 透射电镜及红外等手段对粉体进行了表征,并对配合物溶胶-共沸蒸馏脱水的干燥机制进行了探讨.实验结果表明:硬脂酸溶胶凝胶法制备纳米粉体时,配合物溶胶的干燥脱水是不可缺少的一步.共沸蒸馏所用的溶剂苯是通过物理吸附作用替代了配合物溶胶中的水,其机理是靠降低粒子间毛细管力来减少聚集作用的,从而防止了干燥及后续煅烧阶段的粉体团聚.     

溶胶-凝胶自燃烧法制备镧取代锶铁氧体

采用溶胶-凝胶自燃烧法制备了镧取代锶铁氧体(Sr1-xLaxFe12O19),用X射线衍射仪(XRD)、扫描电镜(SEM)和HB8510网络矢量分析仪研究了镧取代对锶铁氧体的结构、形貌和电磁性能的影响。结果表明,经900℃煅烧后,纯六角晶系磁铅石结构的锶铁氧体晶相生成。La3+取代摩尔数为0.1和0.2时,锶铁氧体的结构没有变化,未出现杂相。La3+具有抑制铁氧体晶粒生长的作用。当La3+取代量为0.1时,可使锶铁氧体的复介电常数和复磁导率的值升高,但当La3+取代量增加到0.2时,又使复介电常数和复磁导率的值降低。Sr0.9La0.1Fe12O19的样品具有最大的介电损耗角正切tanδε值和磁损耗角正切tanδμ值,分别为0.01和0.26。     

溶胶-凝胶法制备YAG:Ho~(3+),Yb~(3+)纳米晶

以稀土氧化物和硝酸铝为原料,采用溶胶-凝胶法合成了YAG:1%Ho~(3+),1%Yb~(3+)纳米晶,并通过正交试验法确定其干凝胶的合成条件.采用DTA-TG、XRD及TEM对干凝胶的合成过程、纳米晶的晶相组成及形貌进行了研究,表明干凝胶经1 200 ℃煅烧后形成了结晶完全的YAG相,无中间相产生.吸收光谱和上转换发射光谱分析表明,Yb~(3+)在材料的发光过程中具有传递能量的作用,Ho~(3+)在跃迁过程中发射出中心波长为650 nm的红色上转换荧光及540 nm的绿色上转换荧光.     

纳米粉体的溶胶-凝胶法制备技术

系统地概述了溶胶-凝胶法制备纳米粉体的技术方法、特点和研究进展,并认为溶胶-凝胶法具有许多优点,是一种极有应用前景的纳米粉体的制备方法。     

溶胶-凝胶法制备稀土CeO2掺杂纳米钨粉的研究

以偏钨酸铵(AMT)、柠檬酸和硝酸铈为原料,用溶胶-凝胶法(sol-gel)制备稀土CeO2掺杂纳米钨粉。通过热重-差热(TG-DSC)、X射线衍射(XRD)、扫描电子显微镜(SEM)、比表面积法(BET)等测试手段对复合粉体的合成工艺、物相、颗粒形貌和粒径进行了分析。结果表明:当pH值为1时,还原后的粉体颗粒呈准球形,无团聚,稀土元素以CeO2形式存在且均匀地分布在钨粉中,平均颗粒粒径为80nm左右,满足制备高性能掺杂稀土氧化物亚微米结构浸渍阴极的要求。     

Sol-Gel Synthesis of LaMO3 (M = Cr, Mn, Fe, Co, Ni) Nanocrystalline Powders

Sol-gel synthesis of LaMO3 ( M = Cr, Mn, Fe, Co, Ni) nanocrystalline Powders was investigated. DSC measurement shows that precursors decomposed at about 403 K and 620 K to bum out of N, C, and H. The calcined samples at 1073 K were determined by XRD to be single phase. SEM observation shows that the prepared samples are nanocrystalline powders in broad sense. The average grain size of LaM'O3 (M'= Cr, Mn, Fe, Ni) is 150 ～700 nm,and the grain size of LaCoO3 is about 30 nm.     

Synthesis of Nanocrystalline La1-xSrxCrO3 by Sol-Gel Method

The nanocrystalline La1-xSrxCrO3 was prepared by sol-gel method using La( NO3 )3 · 6H2O, Sr( NO3 )2 and respectively. The phase transformation from dry-gel to crystal was investigated by means of TG, DSC and XRD. Influences of temperature and Sr quantity on particle-diameters were observed by HREM. The experimental results show that the best calcined temperature is near 800 ℃. The particle-diameters decrease with the increase of Sr quantity. The chromite phase formed continuously during crystallization process, which is mainly composed of four steps: ( 1 ) Carbonates first formed by decomposing metal citrates. (2) The decomposition of carbonates occurred metal oxides. (3) La0. 9Sr0.1 CrO4 were synthesized by the reaction of metal oxides. (4) Chromite phase formed lastly due to the decomposition of chromate phase.     

溶胶-凝胶法制备的(La1-xCex)2/3Sr1/3MnO3超微粉末微波吸收特性研究

采用溶胶-凝胶法制备了钙钛矿型锰氧化物(La1-x Cex)2/3Sr1/3 MnO3(x=0.1,0.3,0.5)超微粉末,用XRD分析了该材料的相结构,并用AV3618型微波矢量网络分析仪测试了样品在8.2GHz～12.5GHz范围内的微波吸收特性.结果表明,样品在1000℃焙烧后出现单一的钙钛矿型结构,当材料涂层厚度为1mm、x=0.3时,(La1-x Cex)2/3 Sr1/3 MnO3的吸波性能最佳.在测试频段内有三个吸收峰,最高的吸收峰在9.1GHz处,峰值高达36.8dB,并且吸收衰减量大于18dB的频带宽度达2.2GHz.     

Synthesis and Electrical Properties of La0.6M0.4FeO3-δ(M=Ca, Sr, Ba) as Cathodes for SOFCs

A series samples of La0.6M0.4FeO3-δ (M=Ca, Sr, Ba) perovskite-type oxides were prepared by glycine nitrate process (GNP). FTIR, TG-DSC, XRD and TEM techniques were used to characterize the chemical constitution, thermal stability and phase structure. The electrical conductivity of the samples was investigated by four-probe technique. With the increase of substituted-ionic radius, the temperature of phase formation increases, and the solid solubility decreases gradually, respectively. The La0.6Ca0.4FeO3-δ(LCF)powder is pure cubic perovskite-type crystalline after fired at 850 ℃ for 2 h. The XRD patterns of La0.6Sr0.4FeO3-δ(LSF) powder shows a small quantity of SrO peaks sintered at 1050 ℃ for 2 h. The electrical conductivity of LCF and LSF at 500～800 ℃ is over 100 S·cm-1, and the value of LCF is 1170 S·cm-1 at 800 ℃, which indicate that LCF and LSF may be used as a profitable cathode for IT-SOFCs. The characteristic of La0.6Ba0.4FeO3-δ(LBF) is poor, and the electrical conductivity at intermediate temperatures is 1/20 less than that of LSF.     

Synthesis and Characterization of Er3+∶Y3Al5O12 Nanocrystalline Powders Prepared by Sol-Gel Method

Nano-sized Er3 ∶Y3Al5O12 powders was successfully prepared via a simple sol-gel route at as low a temperature at 800 ℃ whereas a temperature much higher is necessary to obtain this compound by solid state synthesis (about 1500 ℃). The phase purity, composition and microstructural features of the materials were analyzed by means of X-ray diffraction(XRD), infrared spectroscopy(IR) and transmission electron microscopy(TEM), and no other intermediate phase were observed to form in the range of 700～1000 ℃. The luminescence spectra of Er3 substituted for Y3 in YAG in 1% content was characterized on samples at different temperature.     

Preparation of Perovskite-Type Oxides La1-x Srx Fe1-y Coy O3 Using EDTA Sol-Gel Method

Two series of perovskite-type oxides with composition La1-xSrxFeO3 (x≤0.8)and La1-xSrxFe1-yCoyO3( x = 0.2；y = 0.2, 0.4 ) powder productions were synthesized by EDTA complexing sol-gel method. The products were characterized by XRD, TEM, SEM, BET method (N2 adsorption)and laser granularity analysis for different synthesis conditions to obtain the optimum conditions for the preparation process. Single-phased, uniform perovskite-type oxides with small particle size were obtained by EDTA sol-gel process with high stability and repeatability,and the process temperature is much lower than that of solid state reaction method.     

Preparation and Sinterability of Mn-Zn Ferrite Powders by Sol-Gel Method

Mn-Zn spinel ferrites were synthesized by sol-gel method. Effects of calcined temperature on structure and particle size of MnZnFe2O4 were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD patterns indicate that the ultra fine Mn-Zn ferrite exhibits a spinel crystal structure. SEM images show that the powder fired at 900 ℃ for 2 h has an average diameter of 60～90 nm. The particle size becomes larger with the increasing of calcined temperature and the distribution of particle becomes even more homogeneous. Sintering behaviors of synthesized ferrite powders depend on the powder characteristics and high temperatures have induced the good crystallization of particles.     

La0.7Sr0.3Mn1-xRxO3(R=Co,Ni)的共沉淀法合成及磁性研究

用液相共沉淀法合成了La0.7Sr0.3Mn1-xRxO3(R=Co,Ni)样品.利用XRD对样品结构进行表征,结果表明,由于Co2 半径与Mn3 离子半径不匹配,当Co2 含量x>0.07时,样品La0.7Sr0.3Mn1-xRxO3的结构由正交晶系向单斜晶系转变,而Ni2 离子半径与Mn3 离子半径相近,Ni的掺杂并没有改变系列样品La0.7Sr0.3Mn1-xRxO3的晶体结构.通过振动样品磁强计测试样品的磁性,结果表明,La0.7Sr0.3Mn1-xRxO3(R=Co,Ni)系列样品的比饱和磁化强度随掺杂浓度的增加而减少,这是由于Co2 和Ni2 取代Mn3 后,引起B位离子的电场差的减少.样品的稳定性降低,而使得比饱和磁化强度降低.