Pechini法制备（类）钙钛矿复合氧化物及表征
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摘要
(类)钙钛矿型复合氧化物应用于三效催化剂引起了人们的广泛关注。本实验尝试采用Pechini法合成类钙钛矿型复合氧化物La1.8Sr0.2CuO4。在成功合成纯相La1.8Sr0.2CuO4的基础上,采用非离子表面活性剂聚乙二醇为分散剂制备分散性较好的复合氧化物。与此同时,用Pechini法制备了掺锶量不同的La2-xSrxCuO4(x=0-0.4)。最后,以Pechini法尝试合成钙钛矿型复合氧化物La0.8Sr0.2CuO3。采用XRD、FT-IR、SEM、TEM、BET和H2-TPR等检测手段进行了表征。
采用Pechini法制备La1.8Sr0.2CuO4时,主要讨论了不同的反应条件如金属离子总浓度、水浴温度、柠檬酸用量、焙烧温度对反应中形成的凝胶质量的影响及合成后的样品物相的影响。凝胶形成情况表明,在其他合成条件相同的情况下,水浴温度为70℃、金属离子总浓度为2mol/L时,形成的凝胶均匀透明,颜色清亮。XRD检测结果表明,焙烧温度和柠檬酸用量均对物相的形成有重要影响。最佳的焙烧温度和柠檬酸与金属离子的摩尔比分别为800℃和4。FT-IR结果与XRD结果相一致,进一步表明了合成的样品具有类钙钛矿结构。SEM结果显示,样品呈现多孔隙结构,部分有轻微团聚现象。
在合成Lai.8Sr0.2CuO4复合氧化物的过程中加入分散剂聚乙二醇,XRD检测表明,物相均为单一相类钙钛矿结构,PEG的分子量和用量对样品物相没有影响,但对比表面积和相应的催化性能有较大影响。随着PEG分子量的增加,比表面积减小,催化剂的氧化性能减弱。PEG用量的减少使得样品的比表面积增加,氧化性能增强。TEM分析表明,加入PEG后的样品的颗粒团聚现象较未加入的样品有所减少。H2-TPR结果表明,加入分散剂后的样品比未加入分散剂的样品低温氧化性能更好。
采用Pechini法制备La2-xSrxCuO4(x=0-0.4)时,主要讨论了不同掺锶量对物相,比表面积及催化性能的影响。XRD分析显示,当x>0时,所合成的物相均为单一的类钙钛矿结构,结合FT-IR分析,样品的结构发生了由正交晶型向四方晶型的转变。BET分析表明,掺锶量的增加使样品比表面积增加。H2-TPR结果表明,锶的掺入提高了复合氧化物的低温氧化性能。
采用Pechini法制备钙钛矿型复合氧化物La0.8Sr0.2O3时,XRD图谱表明未能获得单一相的复合氧化物,且焙烧温度对样品的物相有重要影响,随着焙烧温度的提高,颗粒的团聚现象更严重。H2-TPR表明,与类钙钛矿型复合氧化物La1.8Sr0.2CuO4相比,La1.8Sr0.2CuO4的低温催化活性更好,而La0.8Sr0.2O3的结构稳定性更高。
Perovskite(-like) mixed oxides as catalysts for three-way catalysts has attracted much interest. In the paper, Pechini method is used for the synthesis of a series of such mixed oxides. Mainly, the work has been divided into four parts:(1) Pechini method is used to prepare perovskite-like mixed oxides La1.8Sr0.2CuO4.(2) PEG is used as dispersant in order to obtain products with a higher specific surface area in a better compositional homogeneity compared with the sample prepared without PEG. (3) La2-xSrxCuO4 samples with x=0,0.1,0.2,0.3,0.4 are prepared by Pechini method.(4) Perovskite mixed oxides La0.8Sr0.2O3 is prepared by Pechini method. XRD, FT-IR, SEM, TEM, BET and H2-TPR are used to characterize the samples obtained.
Under the system that La1.8Sr0.2CuO4 is prepared by Pechini method, the effects of concentration of total metal nitrates, water-bath heat temperature, the amount of citric acid and calcination temperature on the quality of gel formed and phase formation of the samples obtained are discussed. The experiment shows that when the water-bath heat temperature is 70℃and the concentration of metal nitrates is 2mol/L, the gel obtained is transparent and homogenous. XRD results show that the calcinations temperature and the amount of citric acid have great influence on the phase formation. The optimized calcination temperature and citric acid to metal nitrates molar ratio are 800℃and 4 respectively. The results of FT-IR is in accordance with that of XRD, indicating a characteristic K2NiF4 structure.SEM results show that the sample obtained is porous, and some particle agglomeration can be found in the photograph.
PEG is used as dispersant in the synthesis of La1.8Sr0.2CuO4. XRD results show that the samples obtained are single mixed oxides without the presence of impure phase. The polemerization degree and amount of PEG have no effects on the phase formation of the samples, but play a significant role in the catalytic capability as well as specific surface area. With the increase in molecular weight of PEG, the specific surface area and oxidizing capacity of the sample decrease. TEM results show that the particle agglomeration of samples prepared in the presence of PEG is less seen compared with samples prepared without the dispersant. H2-TPR results demonstrate that the samples prepared in the presence of PEG have a better oxidizing capacity under low temperature than those without the dispersant.
La2-xSrxCuO4(x=0-0.4) are prepared by Pechini method. The effects of the substitution amount "x" on the phase formation, specific surface area and catalytic capability are studied. XRD results show that when x>0, all the samples obtained is single-phase perovskite-like mixed oxides. Taking FT-IR analysis into consideration, it can be concluded that the crystal structure of the samples shift from orthorhombic to tetragonal. With the increase of x, the specific surface area of the samples increase and the catalytic performance of samples at low temperature have been improved, as shown in BET results and H2-TPR results respectively.
La0.8Sr0.2O3 is synthesized by Pechini method. XRD patterns show that mixed oxides without impure phase can not be obtained under ambient conditions. It can also be seen from the XRD results and SEM photographs that the calcination temperature not only has great effects on the phase formation, but also influences the particle aggregation. H2-TPR results show that La1.8Sr0.2CuO4 has a better catalytic performance at low temperature when the structure of La0.8Sr0.2O3 has a higher stability at high temperature.
采用Pechini法制备La1.8Sr0.2CuO4时,主要讨论了不同的反应条件如金属离子总浓度、水浴温度、柠檬酸用量、焙烧温度对反应中形成的凝胶质量的影响及合成后的样品物相的影响。凝胶形成情况表明,在其他合成条件相同的情况下,水浴温度为70℃、金属离子总浓度为2mol/L时,形成的凝胶均匀透明,颜色清亮。XRD检测结果表明,焙烧温度和柠檬酸用量均对物相的形成有重要影响。最佳的焙烧温度和柠檬酸与金属离子的摩尔比分别为800℃和4。FT-IR结果与XRD结果相一致,进一步表明了合成的样品具有类钙钛矿结构。SEM结果显示,样品呈现多孔隙结构,部分有轻微团聚现象。
在合成Lai.8Sr0.2CuO4复合氧化物的过程中加入分散剂聚乙二醇,XRD检测表明,物相均为单一相类钙钛矿结构,PEG的分子量和用量对样品物相没有影响,但对比表面积和相应的催化性能有较大影响。随着PEG分子量的增加,比表面积减小,催化剂的氧化性能减弱。PEG用量的减少使得样品的比表面积增加,氧化性能增强。TEM分析表明,加入PEG后的样品的颗粒团聚现象较未加入的样品有所减少。H2-TPR结果表明,加入分散剂后的样品比未加入分散剂的样品低温氧化性能更好。
采用Pechini法制备La2-xSrxCuO4(x=0-0.4)时,主要讨论了不同掺锶量对物相,比表面积及催化性能的影响。XRD分析显示,当x>0时,所合成的物相均为单一的类钙钛矿结构,结合FT-IR分析,样品的结构发生了由正交晶型向四方晶型的转变。BET分析表明,掺锶量的增加使样品比表面积增加。H2-TPR结果表明,锶的掺入提高了复合氧化物的低温氧化性能。
采用Pechini法制备钙钛矿型复合氧化物La0.8Sr0.2O3时,XRD图谱表明未能获得单一相的复合氧化物,且焙烧温度对样品的物相有重要影响,随着焙烧温度的提高,颗粒的团聚现象更严重。H2-TPR表明,与类钙钛矿型复合氧化物La1.8Sr0.2CuO4相比,La1.8Sr0.2CuO4的低温催化活性更好,而La0.8Sr0.2O3的结构稳定性更高。
Perovskite(-like) mixed oxides as catalysts for three-way catalysts has attracted much interest. In the paper, Pechini method is used for the synthesis of a series of such mixed oxides. Mainly, the work has been divided into four parts:(1) Pechini method is used to prepare perovskite-like mixed oxides La1.8Sr0.2CuO4.(2) PEG is used as dispersant in order to obtain products with a higher specific surface area in a better compositional homogeneity compared with the sample prepared without PEG. (3) La2-xSrxCuO4 samples with x=0,0.1,0.2,0.3,0.4 are prepared by Pechini method.(4) Perovskite mixed oxides La0.8Sr0.2O3 is prepared by Pechini method. XRD, FT-IR, SEM, TEM, BET and H2-TPR are used to characterize the samples obtained.
Under the system that La1.8Sr0.2CuO4 is prepared by Pechini method, the effects of concentration of total metal nitrates, water-bath heat temperature, the amount of citric acid and calcination temperature on the quality of gel formed and phase formation of the samples obtained are discussed. The experiment shows that when the water-bath heat temperature is 70℃and the concentration of metal nitrates is 2mol/L, the gel obtained is transparent and homogenous. XRD results show that the calcinations temperature and the amount of citric acid have great influence on the phase formation. The optimized calcination temperature and citric acid to metal nitrates molar ratio are 800℃and 4 respectively. The results of FT-IR is in accordance with that of XRD, indicating a characteristic K2NiF4 structure.SEM results show that the sample obtained is porous, and some particle agglomeration can be found in the photograph.
PEG is used as dispersant in the synthesis of La1.8Sr0.2CuO4. XRD results show that the samples obtained are single mixed oxides without the presence of impure phase. The polemerization degree and amount of PEG have no effects on the phase formation of the samples, but play a significant role in the catalytic capability as well as specific surface area. With the increase in molecular weight of PEG, the specific surface area and oxidizing capacity of the sample decrease. TEM results show that the particle agglomeration of samples prepared in the presence of PEG is less seen compared with samples prepared without the dispersant. H2-TPR results demonstrate that the samples prepared in the presence of PEG have a better oxidizing capacity under low temperature than those without the dispersant.
La2-xSrxCuO4(x=0-0.4) are prepared by Pechini method. The effects of the substitution amount "x" on the phase formation, specific surface area and catalytic capability are studied. XRD results show that when x>0, all the samples obtained is single-phase perovskite-like mixed oxides. Taking FT-IR analysis into consideration, it can be concluded that the crystal structure of the samples shift from orthorhombic to tetragonal. With the increase of x, the specific surface area of the samples increase and the catalytic performance of samples at low temperature have been improved, as shown in BET results and H2-TPR results respectively.
La0.8Sr0.2O3 is synthesized by Pechini method. XRD patterns show that mixed oxides without impure phase can not be obtained under ambient conditions. It can also be seen from the XRD results and SEM photographs that the calcination temperature not only has great effects on the phase formation, but also influences the particle aggregation. H2-TPR results show that La1.8Sr0.2CuO4 has a better catalytic performance at low temperature when the structure of La0.8Sr0.2O3 has a higher stability at high temperature.
引文
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