La_(0.5)Sr_(0.5)MnO_3钙钛矿型复合氧化物的制备及表征
摘要
钙钛矿型复合氧化物引起了人们的广泛关注,其在汽车尾气处理方面的优越性能更吸引着越来越多的人们进行研究。本文主要采用水热法、共沉淀法两种方法分别合成钙钛矿型复合氧化物La0.5Sr0.5MnO3。同时,采用非离子表面活性剂PEG-4000对样品进行表面改性,从而研究PEG-4000对钙钛矿型复合氧化物La0.5Sr0.5MnO3的性能影响。本文主要通过XRD、TG、SEM、BET和H2-TPR等检测手段对样品进行了性能表征。
利用水热法制备钙钛矿型复合氧化物La0.5Sr0.5MnO3时,本文主要研究不同反应条件(如水热温度、焙烧条件)对产物物相生成的影响。经XRD结果表明,本实验采用的反应条件下均未能得到单一的、纯净的钙钛矿型复合氧化物La0.5Sr0.5MnO3,说明水热法不利于钙钛矿型复合氧化物La0.5Sr0.5MnO3的合成。
利用共沉淀法制备钙钛矿型复合氧化物La0.5Sr0.5MnO3时,本文亦讨论了焙烧温度、焙烧时间对产物物相形成的影响。结合热重分析确定了反应的焙烧温度,并通过计算和实验确定了共沉淀的pH值。最终获得的最佳反应条件为：共沉淀pH：10；焙烧温度：850℃；焙烧时间：4h。所得到的样品比表面积随温度的升高而减小。其中纯相的La0.5Sr0.5MnO3比表面积为6.86 m2.g-1。
为了研究PEG-4000对钙钛矿型复合氧化物La0.5Sr0.5MnO3的影响,设计并进行了一系列试验。其中,经XRD结果表明,所制备的样品为单一的、纯净的钙钛矿型复合氧化物结构且PEG-4000的用量对样品物相的生成没有影响。通过BET检测结果可知,PEG-4000的加入对样品比表面积和催化性能有较大影响。适当的加入PEG-4000,可以有效的增加样品的比表面积,并显著的增强其氧化性能。SEM结果分析表明,PEG-4000的加入可以有效的降低样品颗粒团聚,同时减弱温度对样品颗粒团聚现象的影响。通过H2-TPR结果分析表明,PEG-4000分散剂的加入可以显著的提高样品的低温氧化性能,并增强其在高温反应下的结构稳定性。
Perovskite mixed oxides have been raised world-wide concern because of their remarkable ability in the treatment of exhaust. This paper is mainly engaged in two ways to synthesize La0.5Sr0.5MnO3, namely hydrothermal method and co-precipitation method in order to find out which is the appropriate way to prepare the target product. Meanwhile, surfactant PEG-4000 has been adopted to optimize the physical and chemical capabilities of the product. XRD, TG, SEM, BET and H2-TPR have been used for the characterization of the product.
The effects of different hydrothermal temperature and calcination conditions on the phase formation of the product prepared by hydrothermal method have been studied. XRD shows that, no single-phased perovskite structured mixed oxides Lao.5Sro.5Mn03 can be obtained through hydrothermal method regardless of the change of experiment conditions. It can be concluded that hydrothermal method is not the appropriate way to synthesize La0.5Sr0.5MnO3.
The effects of calcination temperature as well as calcination time on the phase formation of the product prepared by co-precipitation method have also been discussed. The calcination temperature has been identified with XRD and TG analysis. pH value for co-precipitation has been found by calculation as well as experiment. The optimal experimental conditions are:Co-precipitaiton pH:10; calcination temperature:850℃, calcination time:4h. With the increase of the temperature, the specific surface area has been reduced. And the specific surface area of product with single phase has reached by 6.86 m2·g-1.
In order to study the effects of PEG-4000 on the physical and chemical capabilities of La0.5Sr0.5MnO3, a series of experiments have been designed. XRD results show that all the products obtained are single-phase and the amount of the dispersant has no effect on the phase formation. BET results show that PEG-4000 plays an important role in the specific surface area and the catalytic capabilities of the product. The appropriate amount of the dispersant can be beneficial for the specific surface area of the product, and remarkably improve its oxidizing capability. SEM results show that PEG-4000 is able to alleviate the agglomeration of the particles and reduce the effects of temperature on the particle agglomeration. H2-TPR show that, the product prepared with PEG-4000 has better oxidizing capability under low temperature and a higher structural stability under high temperature.
利用水热法制备钙钛矿型复合氧化物La0.5Sr0.5MnO3时,本文主要研究不同反应条件(如水热温度、焙烧条件)对产物物相生成的影响。经XRD结果表明,本实验采用的反应条件下均未能得到单一的、纯净的钙钛矿型复合氧化物La0.5Sr0.5MnO3,说明水热法不利于钙钛矿型复合氧化物La0.5Sr0.5MnO3的合成。
利用共沉淀法制备钙钛矿型复合氧化物La0.5Sr0.5MnO3时,本文亦讨论了焙烧温度、焙烧时间对产物物相形成的影响。结合热重分析确定了反应的焙烧温度,并通过计算和实验确定了共沉淀的pH值。最终获得的最佳反应条件为：共沉淀pH：10；焙烧温度：850℃；焙烧时间：4h。所得到的样品比表面积随温度的升高而减小。其中纯相的La0.5Sr0.5MnO3比表面积为6.86 m2.g-1。
为了研究PEG-4000对钙钛矿型复合氧化物La0.5Sr0.5MnO3的影响,设计并进行了一系列试验。其中,经XRD结果表明,所制备的样品为单一的、纯净的钙钛矿型复合氧化物结构且PEG-4000的用量对样品物相的生成没有影响。通过BET检测结果可知,PEG-4000的加入对样品比表面积和催化性能有较大影响。适当的加入PEG-4000,可以有效的增加样品的比表面积,并显著的增强其氧化性能。SEM结果分析表明,PEG-4000的加入可以有效的降低样品颗粒团聚,同时减弱温度对样品颗粒团聚现象的影响。通过H2-TPR结果分析表明,PEG-4000分散剂的加入可以显著的提高样品的低温氧化性能,并增强其在高温反应下的结构稳定性。
Perovskite mixed oxides have been raised world-wide concern because of their remarkable ability in the treatment of exhaust. This paper is mainly engaged in two ways to synthesize La0.5Sr0.5MnO3, namely hydrothermal method and co-precipitation method in order to find out which is the appropriate way to prepare the target product. Meanwhile, surfactant PEG-4000 has been adopted to optimize the physical and chemical capabilities of the product. XRD, TG, SEM, BET and H2-TPR have been used for the characterization of the product.
The effects of different hydrothermal temperature and calcination conditions on the phase formation of the product prepared by hydrothermal method have been studied. XRD shows that, no single-phased perovskite structured mixed oxides Lao.5Sro.5Mn03 can be obtained through hydrothermal method regardless of the change of experiment conditions. It can be concluded that hydrothermal method is not the appropriate way to synthesize La0.5Sr0.5MnO3.
The effects of calcination temperature as well as calcination time on the phase formation of the product prepared by co-precipitation method have also been discussed. The calcination temperature has been identified with XRD and TG analysis. pH value for co-precipitation has been found by calculation as well as experiment. The optimal experimental conditions are:Co-precipitaiton pH:10; calcination temperature:850℃, calcination time:4h. With the increase of the temperature, the specific surface area has been reduced. And the specific surface area of product with single phase has reached by 6.86 m2·g-1.
In order to study the effects of PEG-4000 on the physical and chemical capabilities of La0.5Sr0.5MnO3, a series of experiments have been designed. XRD results show that all the products obtained are single-phase and the amount of the dispersant has no effect on the phase formation. BET results show that PEG-4000 plays an important role in the specific surface area and the catalytic capabilities of the product. The appropriate amount of the dispersant can be beneficial for the specific surface area of the product, and remarkably improve its oxidizing capability. SEM results show that PEG-4000 is able to alleviate the agglomeration of the particles and reduce the effects of temperature on the particle agglomeration. H2-TPR show that, the product prepared with PEG-4000 has better oxidizing capability under low temperature and a higher structural stability under high temperature.
引文
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