钙钛矿化合物（ABO_3）的合成及表征
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摘要
钙钛矿(ABO3)型复合氧化物由于具有独特性质,可用作多种材料,近年来受到广泛的关注。
本论文采用熔盐法制备了钙钛矿型化合物LaMO3(M=Fe, Co, Ni)和SrFeO3,并通过TG、XRD和SEM等技术进行了系统的研究。结果表明,熔盐介质,烧结温度(主要是450-850℃),熔盐的碱性、氧化性等制备条件对产物的组成、晶相、微观形貌和晶粒大小有重要的影响。其中,Na2O2的加入使得体系的碱性提高,同时高氧化态的物质变得更加稳定。合成温度为750℃时,在系统B2中所得的LaCoO3的形貌为球型颗粒,而加入Na2O2后(系统C2),LaCoO3转化为立方体,同时,颗粒大小从0.63μm大幅增加到4.0μm。在NaNO3-KNO3-Na2O2共融物中制备的LaNiO3纳米晶体的颗粒大小远大于在NaNO2熔盐中所得。纯相的SrFeO3纳米晶体能够在NaNO3-KNO3-Na2O2共熔物中合成出,而以NaOH, KOH以及NaNO3-KNO3共融物均得不到SrFeO3纳米晶体。Na2O2的加入促进了SrCO3与Fe2O3之间的反应,使SrFeO3能够在400℃的相对低温的条件下合成出。
本论文还以柠檬酸为燃料,系统考察了K2CO3、NaOH、KOH和氨水等不同pH调节剂调节前驱物溶液pH值,对溶液燃烧法制备的纳米LaFeO3和LaMnO3粉体的晶相组成、晶粒大小和微观形貌的影响。结果表明：
1、氨水调节前驱物溶液pH值5、7和9,可以制备得到纯相LaFeO3纳米晶体,对应产物的平均晶粒尺寸分别为29.4、37.2和32.3nm,而pH=13时,产物为Fe2O3相和无定形相的混合物。NaOH溶液为pH调节剂,前驱物溶液在pH值5至13范围内均能制的纯相LaFeO3纳米晶体；其中pH=7的中性环境中产物为多孔网状蓬松纳米结构,具有最大的晶粒尺寸30.5nm,而在酸性和碱性环境中制的产物为无规则颗粒的聚集体。
2、以KOH作pH调节剂,pH=13的碱性环境中产物多为立方体的钙钛矿纳米LaMnO3晶粒,以氨水作pH调节剂,pH=10时产物为蓬松多孔的结构。而以K2CO3和NaOH为调节剂制的产物为无规则颗粒的聚集体。
Perovskite compound LaMO3 (M= Fe, Co, Ni) nanocrystals were successfully synthesized in molten nitrates or nitrites from a mixture of lanthanum nitrate and an M-containing nitrate for 2 h. The effect of the various process parameters on the phase purity, crystallite size, specific surface area and morphology of the synthesized nanocrystals were systematically studied by XRD, scanning electron microscopy (SEM), simultaneous TG/DSC and BET measurements. The results showed that salt medium, annealing temperatures (mainly 450-850℃), oxidising properties and basicity of the melt played an important role in the synthesis of LaMO3. The addition of Na2O2 facilitated the reaction between La2O3 and NiO or Co3O4, leading to the formation of LaNiO3 and LaCoO3 at a much lower temperature of 450℃. Pure hexagonal LaNiO3 nanocrystals were obtained in molten NaNO3-KNO3 eutectic with Na2O2 at 550-750℃. Pure perovskite compound SrFeO3 nanocrystals were successfully synthesized in molten NaNO3-KNO3 eutectic with Na2O2 from a mixture of strontium nitrate and ferric nitrate. It was found that metal nitrates is the suitable precursors and NaNO3-KNO3 eutectic with Na2O2 is the suitable salt medium, which results in the formation of pure SrFeO3 nanocrystals at a much lower temperature of 400℃.
Perovskite compound LaFeO3 was prepared by solution combustion synthesis using lanthanum nitrate and ferric nitrate as oxidants, citric acid as organic fuel and ammonia and NaOH solution as pH regulator. The results showed that the pH regulator and the pH value of precursor solution had significant effect on the phase composition, crystallite size and morphology of LaFeO3. When the pH value of precursor solution was adjusted to 5,7 and 9 by ammonia, pure phase LaFeO3 could be obtained by solution combustion method and had a crystallite size of 29.4、37.2 and 32.3 nm, respectively, while a mixture of amorphous phase and Fe2O3 was obtained at pH=13. In contrast to this, NaOH solution as pH regulator, pure phase LaFeO3 could be obtained in the pH range of 5 to 13, and the LaFeO3 nanocrystals prepared at pH=7 had a net-like porous structure with the largest crystallite size of 30.5 nm. However, under the acidic and basic conditions, the obtained LaFeO3 products were an aggregate of irregular particles. Cubic LaMnO3 nanocrystals appeared in SEM photography when the product was prepared at pH=13 and using KOH as pH regulator. The LaMnO3 nanocrystals prepared at pH=10 and using ammonia as pH regulator had a net-like porous structure. With other pH regulators, the products were an aggregate of irregular particles.
本论文采用熔盐法制备了钙钛矿型化合物LaMO3(M=Fe, Co, Ni)和SrFeO3,并通过TG、XRD和SEM等技术进行了系统的研究。结果表明,熔盐介质,烧结温度(主要是450-850℃),熔盐的碱性、氧化性等制备条件对产物的组成、晶相、微观形貌和晶粒大小有重要的影响。其中,Na2O2的加入使得体系的碱性提高,同时高氧化态的物质变得更加稳定。合成温度为750℃时,在系统B2中所得的LaCoO3的形貌为球型颗粒,而加入Na2O2后(系统C2),LaCoO3转化为立方体,同时,颗粒大小从0.63μm大幅增加到4.0μm。在NaNO3-KNO3-Na2O2共融物中制备的LaNiO3纳米晶体的颗粒大小远大于在NaNO2熔盐中所得。纯相的SrFeO3纳米晶体能够在NaNO3-KNO3-Na2O2共熔物中合成出,而以NaOH, KOH以及NaNO3-KNO3共融物均得不到SrFeO3纳米晶体。Na2O2的加入促进了SrCO3与Fe2O3之间的反应,使SrFeO3能够在400℃的相对低温的条件下合成出。
本论文还以柠檬酸为燃料,系统考察了K2CO3、NaOH、KOH和氨水等不同pH调节剂调节前驱物溶液pH值,对溶液燃烧法制备的纳米LaFeO3和LaMnO3粉体的晶相组成、晶粒大小和微观形貌的影响。结果表明：
1、氨水调节前驱物溶液pH值5、7和9,可以制备得到纯相LaFeO3纳米晶体,对应产物的平均晶粒尺寸分别为29.4、37.2和32.3nm,而pH=13时,产物为Fe2O3相和无定形相的混合物。NaOH溶液为pH调节剂,前驱物溶液在pH值5至13范围内均能制的纯相LaFeO3纳米晶体；其中pH=7的中性环境中产物为多孔网状蓬松纳米结构,具有最大的晶粒尺寸30.5nm,而在酸性和碱性环境中制的产物为无规则颗粒的聚集体。
2、以KOH作pH调节剂,pH=13的碱性环境中产物多为立方体的钙钛矿纳米LaMnO3晶粒,以氨水作pH调节剂,pH=10时产物为蓬松多孔的结构。而以K2CO3和NaOH为调节剂制的产物为无规则颗粒的聚集体。
Perovskite compound LaMO3 (M= Fe, Co, Ni) nanocrystals were successfully synthesized in molten nitrates or nitrites from a mixture of lanthanum nitrate and an M-containing nitrate for 2 h. The effect of the various process parameters on the phase purity, crystallite size, specific surface area and morphology of the synthesized nanocrystals were systematically studied by XRD, scanning electron microscopy (SEM), simultaneous TG/DSC and BET measurements. The results showed that salt medium, annealing temperatures (mainly 450-850℃), oxidising properties and basicity of the melt played an important role in the synthesis of LaMO3. The addition of Na2O2 facilitated the reaction between La2O3 and NiO or Co3O4, leading to the formation of LaNiO3 and LaCoO3 at a much lower temperature of 450℃. Pure hexagonal LaNiO3 nanocrystals were obtained in molten NaNO3-KNO3 eutectic with Na2O2 at 550-750℃. Pure perovskite compound SrFeO3 nanocrystals were successfully synthesized in molten NaNO3-KNO3 eutectic with Na2O2 from a mixture of strontium nitrate and ferric nitrate. It was found that metal nitrates is the suitable precursors and NaNO3-KNO3 eutectic with Na2O2 is the suitable salt medium, which results in the formation of pure SrFeO3 nanocrystals at a much lower temperature of 400℃.
Perovskite compound LaFeO3 was prepared by solution combustion synthesis using lanthanum nitrate and ferric nitrate as oxidants, citric acid as organic fuel and ammonia and NaOH solution as pH regulator. The results showed that the pH regulator and the pH value of precursor solution had significant effect on the phase composition, crystallite size and morphology of LaFeO3. When the pH value of precursor solution was adjusted to 5,7 and 9 by ammonia, pure phase LaFeO3 could be obtained by solution combustion method and had a crystallite size of 29.4、37.2 and 32.3 nm, respectively, while a mixture of amorphous phase and Fe2O3 was obtained at pH=13. In contrast to this, NaOH solution as pH regulator, pure phase LaFeO3 could be obtained in the pH range of 5 to 13, and the LaFeO3 nanocrystals prepared at pH=7 had a net-like porous structure with the largest crystallite size of 30.5 nm. However, under the acidic and basic conditions, the obtained LaFeO3 products were an aggregate of irregular particles. Cubic LaMnO3 nanocrystals appeared in SEM photography when the product was prepared at pH=13 and using KOH as pH regulator. The LaMnO3 nanocrystals prepared at pH=10 and using ammonia as pH regulator had a net-like porous structure. With other pH regulators, the products were an aggregate of irregular particles.
引文
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