溶胶-凝胶法制备La0.8Sr0.2CoO3纳米材料

以La(NO3)3·6H2O、Sr(NO3)2、Co(NO3)2·6H2O为原料,用EDTA络合溶胶-凝胶法制备La0.8Sr0.2CoO3凝胶,在700℃、800℃、900℃煅烧,制得La0.8Sr0.2CoO3粉体.用DTA、FT-IR、XRD、SEM等手段对制备过程、热分解机理及粉体的性能进行了研究.在700℃焙烧2 h得到La0.8Sr0.2CoO3纯相纳米粉,颗粒呈球形.选取700℃焙烧2 h的La0.8Sr0.2CoO3粉体制成管状传感器,进行NO2敏感性能测试,探讨了相同NO2浓度下,传感器敏感信号与温度的关系.结果表明:纳米La0.8Sr0.2CoO3粉体在450℃时对NO2的敏感信号最大,输出的电动势信号与NO2浓度之间呈线性关系.     

螯合物-凝胶法制备La0.8Sr0.2MnO3粉体

以La(NO3)3·6H2O,Sr(NO3)2和Mn(NO3)3·6H2O为起始原料,采用螯合物-凝胶法制备出La0.8Sr0.2MnO3粉体.首先在混合盐溶液中入柠檬酸形成螯合的柠檬酸盐,然后加入单体和交联剂,在引发剂和催化剂的作用下形成湿凝胶.干燥后的前驱体为无定形的,DTA和XRD测试表明晶化温度在400℃～500℃.在500℃～1 200℃范围内煅烧,颗粒尺寸由500℃时的约38 nm 长大到1 200℃时的500 nm.     

溶胶凝胶法制备纳米贵金属稀土复合氧化物研究

通过溶胶凝胶法以无机盐为原料制备纳米贵金属稀土复合氧化物,并采用透射电镜(TEM)、低温氮吸附、X射线衍射(XRD)和程序升温H2还原(TPR-H2)对其形貌特征和物化性能进行了研究.复合氧化物为无定形或不规则多晶物质,以不规则球形粒子聚集成团存在,平均粒径约为70 nm.其比表面积和总孔容适中,孔容呈现双峰分布特征.其储氧值和还原起点温度分别为2767 μmol/g和200℃,具有作为汽车尾气净化三元催化剂涂层料的潜在优异起燃和储氧特性.     

纳米MnO2的制备及电化学性能研究

采用溶胶-凝胶法(sol-gel)制备了纳米MnO2,并对其进行了酸化和高温处理.采用化学分析、XRD、红外光谱、循环伏安、恒流放电等测试方法对处理前后的样品进行分析.研究结果表明,酸化后的样品氧化度和表面积增大,粒径减小,放电容量增大;经过500℃高温及酸化处理后的样品,其氧化度更高,粒径更小,其原因可能是高温酸化后,样品中的质子与O2-更易结合,从而使样品的活性提高.制备的纳米MnO2与电解二氧化锰(EMD)相比,在-0.4 V处,其放电容量高出52%.     

纳米金属颗粒分散氧化物Ag/NiO薄膜的制备与光吸收特性

利用溶胶-凝胶法制备了纳米金属颗粒分散氧化物Ag/NiO复合薄膜,用X射线荧光光谱、X射线衍射分析、透射电子显微镜、紫外可见分光光度计表征了薄膜的成分、相结构、微结构以及光吸收特性.X射线衍射分析结果表明存在NiO相和单质Ag相.光吸收谱研究表明,Ag/NiO薄膜在410 nm波长附近有明显的表面等离子共振吸收峰,随着Ag含量的增加,吸收峰变窄,蓝移,强度增加.当Ag含量接近41%(质量分数)时,Ag/NiO薄膜在414 nm波长附近表现的吸收峰呈现最大的吸收强度;当Ag分散颗粒的含量超过41%(质量分数)后,吸收峰的强度开始下降.随着保温时间的延长,薄膜的光学吸收峰的强度增强,并且吸收峰峰位向波长短的方向移动.     

pH值对溶胶-凝胶法制备La0.65Sr0.35MnO3的影响

利用溶胶-凝胶法制备亚锰酸盐化合物La0.65Sr0.35MnO3,通过XRD和SEM研究不同pH值对合成粉体相组成和微观形貌的影响。结果发现:在pH值为0.5的酸性环境和pH为8.0的弱碱性环境中,均可以获得具有钙钛矿结构且尺寸均匀的La0.65Sr0.35MnO3粉体。在pH值为0.5的酸性环境中,有利于形成二维层状结构的凝胶,而在pH为8.0的弱碱性环境中,有利于形成三维空间网络结构的凝胶,金属离子可以有效地分散于这两种凝胶中,避免了后期热处理过程中化学组分的偏差及团聚的生成。     

稀土锰氧化物La0.6A0.4MnO3(A代表Cu,Ag,Na)的晶体结构及元素价态研究

采用溶胶-凝胶(sol-gel)法制备La0.6A0.4MnO3(A代表Cu,Ag,Na)多晶样品材料,用X射线衍射(XRD)以及X射线光电子能谱(XPS)对其进行了研究,发现La0.6Cu0.4MnO3,La0.6Na0.4MnO3均为单相菱面体钙钛矿结构,而La0.6Ag0.4MnO3则由菱面体结构的钙钛矿相和立方结构的金属Ag相组成.对LaMnO3母体进行A位掺杂,随着离子半径不同的金属阳离子的掺入,会导致样品产生晶格畸变,从而使样品的晶格常数,晶胞体积发生变化,变化趋势与掺入的金属阳离子半径有关.随着掺杂离子半径的增大,样品晶格常数、晶胞体积也相应增大.La在La0.6A0.4MnO3(A代表Cu,Ag,Na)’中均以正三价形式存在,表明La在化合物中是起稳定作用的组分.随着低价态的金属阳离子(Cu2+,Ag+,Na+)替代La3+,将有更多的Mn3+通过Mn-O-Mn的双交换作用变为MMn4+,从而满足试样整体电荷守恒.     

纳米金属颗粒分散氧化物Ag／NiO薄膜的制备与光吸收特性

利用溶胶．凝胶法制备了纳米金属颗粒分散氧化物Ag／NiO复合薄膜，用X射线荧光光谱、X射线衍射分析、透射电子显微镜、紫外可见分光光度计表征了薄膜的成分、相结构、微结构以及光吸收特性。X射线衍射分析结果表明存在NiO相和单质Ag相。光吸收谱研究表明，Ag／NiO薄膜在410nm波长附近有明显的表面等离子共振吸收峰，随着Ag含量的增加，吸收峰变窄，蓝移，强度增加。当Ag含量接近41％（质量分数）时，Ag／NiO薄膜在414nm波长附近表现的吸收峰呈现最大的吸收强度；当Ag分散颗粒的含量超过41％（质量分数）后，吸收峰的强度开始下降。随着保温时间的延长，薄膜的光学吸收峰的强度增强，并且吸收峰峰位向波长短的方向移动。     

纳米氧化物粉体的制备

综合介绍了近十年来纳米氧化物粉体的各种制备方法及其适用性。     

烧结温度对La0.9Sr0.1 MnO3/Fe2O3体系结构和磁性的影响

采用软化学方法制备了纳米材料La0.9Sr0.1MnO3和软磁材料γ-Fe2O3,并将两者按不同比例进行复合,而后在不同温度下对其进行烧结,分别用扫描电子显微镜和X射线技术观察了样品的形貌特征和相结构,并用振动样品磁强计对烧结后的样品磁性进行测量.结果表明,经高温烧结后的复合体系,组成物质间没有发生反应,仍以各自相独立存在;复合体系剩磁Br及饱和磁化强度随烧结温度的升高而增加.烧结温度对样品晶粒和尺寸的影响是导致矫顽力Hc的变化的直接原因.     

凝胶注模制备La0．8Sr0．2MnO3多孔阴极材料

采用凝胶注模技术原位合成造孔剂制备出开孔气孔率为20％～30％的La0．8Sr0．2MnO3多孔阴极材料。结果表明，合适的烧结温度为l100℃～1150℃；开口气孔位于三角晶界，中位孔径约为400nm；多孔材料的电导率随着温度的升高而升高，由ln(σT)-1／T曲线，可得电导活化能Ea为10．99kJ／mol。     

Microwave absorbing properties of La0.8Ba0.2MnO3 nano-particles

La0.8Ba0.2MnO3 nano-particles were synthesized by sol-gel process, and the crystal structure and morphology＇ were characterized by XRD and SEM, respectively. The complex permittivity and permeability were determined by microwave vector network analyzer in the frequency range of 2-18 GHz. The relationship between reflection coefficient and microwave frequency of La0.8Ba0.2 MnO3 was calculated based on measured data. The results show that the average diameter of La0.8Ba0.2MnO3 crystal powders is about 80 nm and the crystal structure is perovskite when being calcined at 800 ℃ for 2 h. The microwave absorbing peak is 13 dB at 6.7 GHz and the effective absorbing bandwidth above 10 dB reaches 1.8 GHz for the sample with the thickness of 2.6 mm. The microwave absorption can be attributed to both the dielectric loss and the magnetic loss from the loss tangents of the sample, but the former is greater than the latter.     

Microstructure and Electrochemical Behavior of La0.8Sr0.2MnO3 Deposited by Solution Precursor Plasma Spraying

采用液料等离子喷涂方法(SPPS)制备固体氧化物燃料电池多孔La0.8Sr0.2MnO3(LSM)阴极。用SEM观察LSM的微结构,用XRD研究其相结构。考察了喷涂距离和热处理温度对LSM微结构的影响规律。结果表明,SPPSLSM在1050℃热处理2h后形成连续的具有微纳介孔结构的涂层,且LSM具有单一的钙钛矿结构。利用电化学交流阻抗谱方法研究了LSM极化行为。微结构对极化性能有显著影响,1000℃时,LSM在喷涂距离为60mm时具有最佳的电化学性能,阴极极化电阻约为0.3Ω·cm2。通过工艺的控制,SPPS可以实现SOFC阴极相和微结构的优化。     

Preparation and characterization of La0.8Cu0.2MnO(3±δ) perovskite-type catalyst for methane combustion

La0.8 Cu0.2 MnO(3±δ) perovskite-type catalyst for methane combustion prepared through sol-gel process was characterized by X-ray Diffractometry(XRD), X-ray Photoelectron Spectroscopy(XPS) and Scanning Electron Microscopy(SEM). XPS analyses reveal that the surface characteristics of the catalyst are changed. The lattice defects and oxygen vacancies on the catalyst surface are enhanced due to a part of La3+ being substituted by Cu2+.Temperature-programmed-desorption(TPD) and temperature-programmed-reduction(TPR) analyses were carried out to study the catalytic behavior. It is found that there are two O2-desorption peaks at 350 ℃ and 650 ℃ in the TPD pattern, and two CH4-consumption peaks at 420 ℃ and 750 ℃ in the TPR patterns respectively, which indicates that the two kinds of oxygen species, so-called α and β oxygen, can react with the methane during catalytic combustion process. The catalytic activity tests were performed in a fixed-bed reactor, and the results show that the T1/2 at which the conversion of methane attains 50 % of La0.8 Cu0.2 MnO(3±δ) is lower by 55 ℃ than that of LaMnO3.This indicates that the catalytic activity of La0.8 Cu0. 2 MnO(3±δ) is increased with partial substitution of Cu2+ for La3+.     

Molten salt synthesis of La0.8Sr0.2MnO3 powders for SOFC cathode electrode

For La_0.8Sr_0.2MnO₃ (LSM) perovskite, used as the cathode material for solid oxide fuel cells (SOFC), it is known that the formation of a triple-phase-boundary is restrained due to the formation of a second phase at the YSZ/electrode interface at high temperature. To decrease the 2^nd phase, lowering the sintering temperature has been used. LSM powder was synthesized by molten salt synthesis method to control its particle size, shape, and agglomeration. We have characterized the phase formation, particle size, shape, and sintering behavior of LSM in the synthesis using the variation of KCl, LiCl, KF and its mixed salts as raw materials. In the case of KCl and KCl-KF salts, the particle size and shape of the LSM was well controlled and synthesized. However, in the case of LiCl and KCl-LiCl salts, LiMnO_x as 2^nd phase and LSM were synthesized simultaneously. In the case of the mixed salt of KCl-KF, the growth mechanism of the LSM particle was changed from ‘diffusion-controlled’ to ‘reaction-controlled’ according to the amount of mixed salt. The sintering temperature can be decreased below 1000 °C by using the synthesized LSM powder.     

Fabrication and performance of La0.8Sr0.2MnO3/YSZ graded composite cathodes for SOFC

The performance of multi-layer (1-x)La0.8Sr0.2MnO3/xYSZ graded composite cathodes was studied as electrode materials for intermediate solid oxide fuel cells (SOFC). The thermal expansion coefficient, electrical conductivity, and electrochemical performance of multi-layer composite cathodes were investigated. The thermal expansion coefficient and electrical conductivity decreased with the increase in YSZ content. The (1-x)La0.8Sr0.2MnO3/xYSZ composite cathode greatly increased the length of the active triple phase boundary line (TPBL) among electrode, electrolyte, and gas phase, leading to a decrease in polarization resistance and an increase in polarization current density. The polarization current density of the triple-layer graded composite cathode (0.77 A/cm2) was the highest and that of the monolayer cathode (0.13 A/cm2) was the lowest. The polarization resistance (Rp) of the triple-layer graded composite cathode was only 0.182Ω·cm2 and that of the monolayer composite cathode was 0.323Ω·cm2. The power density of the triple-layer graded composite cathode was the highest and that of the monolayer composite cathode was the lowest. The triple-layer graded composite cathode had superior performance.     

La0．9Sr0．1Ga0．8Mg0．2O2．85固体电解质合成及其性能

在NH4OH-(NH4)2CO3沉淀体系中用相转移分离法制备了La0.9Sr0.1Ga0.8Mg0.2O2.85(LSGM1020)固体电解质前驱体,并在较低的烧结温度得到了纯度较高,杂质含量低的电解质陶瓷.用XRD,Raman光谱,直流四电极,交流阻抗谱和扫描电镜分析了电解质的晶体结构,电化学性能和显微结构.XRD和Raman分析表明LSGM1020电解质具有菱方钙钛矿结构,800oC时测量得到的氧离子电导率达到0.12S?cm-1.SEM和交流阻抗分析表明,烧结体具有良好的微观结构.采用相转移分离法合成LSGM1020有利于降低烧结温度,改善电解质的性能.