纳米钙钛矿型氧化物的制备及性能研究
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摘要
钙钛矿型复合氧化物由于其结构稳定,性能优异,并可根据氧化物成矿机理成功制备组分丰富多样、结构复杂多变的材料,而引起普遍关注。本文在制备出分散性较好、且晶粒尺寸较小的纳米钙钛矿型氧化物粉体La_(1-x)Sr_xMnO_3并对其电催化性能进行充分研究的基础上,采用高压烧结法制备了La_(0.8)Sr_(0.2)MnO_3块状样品,并研究了其在高压下的晶粒演化情况,同时对高压处理后得到的样品进行了各种性能的研究。课题还研究了在室温下,采用溶胶-凝胶法和浸渍提拉技术在载玻片基底上制备纳米钙钛矿型La_(1-x)Sr_xMnO_3薄膜的最佳工艺条件,并对该类薄膜的光催化性能进行了研究。
采用TG/DTA技术结合傅立叶红外光谱分析了前驱体凝胶的热分解历程;以XRD对不同制备条件下所得产物进行物相分析并计算了其晶粒尺寸;根据BET法测定了粉末样品的比表面积;用TEM观察了不同条件下纳米粉体的颗粒尺寸及其分散状况,得出了采用柠檬酸溶胶-凝胶法合成晶粒尺寸较小且分散性较好的纳米钙钛矿型氧化物粉体的优化反应条件。
提出了采用无水乙醇代替水作溶剂制备具有高度分散性的纳米钙钛矿粉体的新工艺。结果表明,该方法可以有效地防止原生粒子的团聚,提高粉体的分散性;且制备出的氧化物粉体La_(0.8)Sr_(0.2)MnO_3其电催化活性明显优于普通溶胶-凝胶法制备出的该类粉体。将其作为空气电极的催化剂,可以将电池的开路电位提高到1.52 V,且在放电电压为1.4 V,放电电流密度为150 mA/cm2时,持续稳定的放电时间长达15 h,大大地提高了锌-空气电池的放电容量。
利用XRD并结合谢乐公式研究了采用高能球磨法制备纳米钙钛矿粉体时的晶化过程。结果表明,以La2O3、CaO和MnO_2为原料,采用高能球磨法在室温18 h就制备出纳米钙钛矿型氧化物La_(0.8)Ca_(0.2)MnO_3粉体;在该反应体系的球磨过程中,随球磨时间的增加,产物晶粒经历了先长大后细化的过程,且当球磨时间足够长时,晶粒的细化将达到极限。
采用高压烧结法制备出了比较致密且其内部晶粒尺寸小于100 nm的钙钛矿型La_(0.8)Sr_(0.2)MnO_3块状样品。分析了素坯的相对密度与成型压力的关系,应用XRD、拉曼光谱和场发射扫描电镜并结合晶粒生长动力学唯象理论研究了高压下La_(0.8)Sr_(0.2)MnO_3的晶粒演化行为。分析结果表明,纳米氧化物La_(0.8)Sr_(0.2)MnO_3成型过程中其内部晶粒的演化受温度和压力的共同影响:当烧结温度在300℃以下时,1～3 Gpa处理后La_(0.8)Sr_(0.2)MnO_3块状样品内部的晶粒生长速度随压力的升高而增大,4～5 GPa处理后其晶粒生长速度随压力的升高而减小;当烧结温度在300℃以上时,其晶粒生长速度随压力和温度的升高而不断增大。
通过测量高压烧结后样品的的表观密度、显微硬度和电磁性能,研究了La_(0.8)Sr_(0.2)MnO_3纳米材料的各种物理性能。实验结果表明,高压烧结后La_(0.8)Sr_(0.2)MnO_3纳米固体材料的显微硬度显著提高;且成型压力越大,表观密度也越大,5 GPa、500℃烧结后得到的样品其相对密度达到99.48%;当烧结温度为300℃时,不同压力下制得的样品的电阻率随制备压力的升高表现出先减小后增大的趋势;5 GPa,300℃时制备出的样品在室温下表现出典型的铁磁性能。
课题通过正交实验确定了在室温下采用溶胶-凝胶法和浸渍提拉技术在载玻片基底上制备纳米钙钛矿型La_(1-x)Sr_xMnO_3薄膜的最佳制备工艺。XRD分析表明,采用络合凝胶法制备出的La_(1-x)Sr_xMnO_3薄膜具有钙钛矿晶型结构,其平均晶粒度为10.32 nm;从薄膜的AFM图像可看出,La_(0.8)Sr_(0.2)MnO_3四层膜比较均匀,其表面粗糙度较小;台阶仪测试得出,薄膜的平均厚度为98.8 nm;
二价金属Sr的掺杂,使该类型薄膜有较好的光催化效果,在9 h内对酸性红A、酸性橙Ⅱ、弱酸性黄C-3GN、直接绿BE、弱酸性蓝C-RL的脱色率分别达到95.56%,89.70%,97.56%,98.40%和91.16%。
Perovskite type compound oxides have stable structure and outstanding performance. The various oxide materials with multiplex component and complex structure may be prepared successfully according to the pattern of metallogeny. Thus,it has aroused an universal interest. In this article, the nano-style perovskite type oxides La_(1-x)Sr_xMnO_3 with smaller grain sizes and better dispersion were prepared and the electric-catalytic activity of powders was researched adequately. La_(0.8)Sr_(0.2)MnO_3 massive sample was prepared under high pressure and agglomeration. The grain evolution regularity and various physical properties were researched for the samples which were prepared under high pressure. The optimum preparation condition and photo-catalysis were researched for La_(1-x)Sr_xMnO_3 thin film on the slide glass base using sol-gel method and dip-coating technology.
The heat decomposition of gel was analyzed by means of TG/DTA and FTIRS; The phase change were analyzed by XRD and its crystal grain size had been calculated; The size of particles and the dispersibility of powders are observed by TEM; The surface area of samples were tested by means of BET; All of above, the optimum preparation condition of perovskite nano-style oxides La_(1-x)Sr_xMnO_3 by citric acid sol-gel method can be obtained.
A kind of new technology is presented for preparing nano-style perovskite powder which has better dispersion. It was that absolute alcohol instead of water as the solvent. It was verified this method could remarkably improve the powders’decentralization and prevent original particles from reuniting. The electric catalysis of La_(0.8)Sr_(0.2)MnO_3 is superiors to the powders which were obtained by the common sol-gel method. It can improve the discharge voltage of air battery to 1.52 V. When the ampere density reaches 150 mA/cm2 and discharge voltage is 1.4 V, the battery can continuous discharge for 15 hours. Thus, the capability of zinc-air battery was increased greatly.
Crystallization process of nano-style oxide powders by high-enemy ball milling with mixing La2O3、MnO_2 and CaO was investigated by using X-ray diffraction patterns and Sherre equation. Results indicated that the La_(0.8)Ca_(0.2)MnO_3 can be synthesized by ball milling18 h under room temperature. The particle size of the powders showed a firstly increasing and subsequent decrescent trend with extending milling time while the grain refinement is limited as time grows.
The compact La_(0.8)Sr_(0.2)MnO_3 massive sample was prepared which crystal grain size less than 100 nm under high pressure and agglomeration. The relationship between relative density of biscuit and forming pressure was analyzed. The grain evolution was researched by XRD、Raman pattern、field emission scanning electron microscopy and the phenomenological kinetic grain growth equation. The results show that it was influenced by temperature and pressure. The grain growth rate under 3 Gpa is increased with increasing pressure while the rate is fall down as pressure continue rise when the agglomeration temperature below 300℃. The grain growth rate is all along increased with pressure increment when the agglomeration temperature over 300℃.
The various physical properties of agglomeration samples under high pressure were studied by testing apparent density、micro-hardness and electromagnetism character. Experimental results indicate that the micro-hardness of samples after high pressure agglomeration was obvious increased and the apparent density is also increased along with pressure. The relative density is 99.48% when sample was prepared under 500℃and 5 GPa. When sintering temperature was 300℃, the resistivity of samples showed first increasing then decreasing trend with increasing pressure and the sample which were prepared under 5 GPa、300℃has obvious ferromagnetic character at room-temperature.
The optimum preparation condition for La_(1-x)Sr_xMnO_3 thin film on the slide glass base using sol-gel method and dip-coating technology was gotten by orthogonal test design method. The phase change was analyzed by XRD and its crystal grain size had been calculated. The result shows that the La_(1-x)Sr_xMnO_3 thin film can be synthesized and average crystal grain size is 10.32 nm. We may see from the AFM Image that the film with four layers is more homogeneous; the surface roughness is less. The average thickness obtained from the step meter is 98.8 nm.
La_(1-x)Sr_xMnO_3 nano-style thin films have better photo-catalysis effect than LaMnO3. The photo-catalytic experiment shows that the de-coloration rates of Acid red A, Acid orangeⅡ,Weak-acid yellow C-3GN, Direct green BE, Weak-acid blue C-RL have reached to 95.56%, 89.70%, 97.56%, 98.40% and 91.16% respectively in 9h.
采用TG/DTA技术结合傅立叶红外光谱分析了前驱体凝胶的热分解历程;以XRD对不同制备条件下所得产物进行物相分析并计算了其晶粒尺寸;根据BET法测定了粉末样品的比表面积;用TEM观察了不同条件下纳米粉体的颗粒尺寸及其分散状况,得出了采用柠檬酸溶胶-凝胶法合成晶粒尺寸较小且分散性较好的纳米钙钛矿型氧化物粉体的优化反应条件。
提出了采用无水乙醇代替水作溶剂制备具有高度分散性的纳米钙钛矿粉体的新工艺。结果表明,该方法可以有效地防止原生粒子的团聚,提高粉体的分散性;且制备出的氧化物粉体La_(0.8)Sr_(0.2)MnO_3其电催化活性明显优于普通溶胶-凝胶法制备出的该类粉体。将其作为空气电极的催化剂,可以将电池的开路电位提高到1.52 V,且在放电电压为1.4 V,放电电流密度为150 mA/cm2时,持续稳定的放电时间长达15 h,大大地提高了锌-空气电池的放电容量。
利用XRD并结合谢乐公式研究了采用高能球磨法制备纳米钙钛矿粉体时的晶化过程。结果表明,以La2O3、CaO和MnO_2为原料,采用高能球磨法在室温18 h就制备出纳米钙钛矿型氧化物La_(0.8)Ca_(0.2)MnO_3粉体;在该反应体系的球磨过程中,随球磨时间的增加,产物晶粒经历了先长大后细化的过程,且当球磨时间足够长时,晶粒的细化将达到极限。
采用高压烧结法制备出了比较致密且其内部晶粒尺寸小于100 nm的钙钛矿型La_(0.8)Sr_(0.2)MnO_3块状样品。分析了素坯的相对密度与成型压力的关系,应用XRD、拉曼光谱和场发射扫描电镜并结合晶粒生长动力学唯象理论研究了高压下La_(0.8)Sr_(0.2)MnO_3的晶粒演化行为。分析结果表明,纳米氧化物La_(0.8)Sr_(0.2)MnO_3成型过程中其内部晶粒的演化受温度和压力的共同影响:当烧结温度在300℃以下时,1～3 Gpa处理后La_(0.8)Sr_(0.2)MnO_3块状样品内部的晶粒生长速度随压力的升高而增大,4～5 GPa处理后其晶粒生长速度随压力的升高而减小;当烧结温度在300℃以上时,其晶粒生长速度随压力和温度的升高而不断增大。
通过测量高压烧结后样品的的表观密度、显微硬度和电磁性能,研究了La_(0.8)Sr_(0.2)MnO_3纳米材料的各种物理性能。实验结果表明,高压烧结后La_(0.8)Sr_(0.2)MnO_3纳米固体材料的显微硬度显著提高;且成型压力越大,表观密度也越大,5 GPa、500℃烧结后得到的样品其相对密度达到99.48%;当烧结温度为300℃时,不同压力下制得的样品的电阻率随制备压力的升高表现出先减小后增大的趋势;5 GPa,300℃时制备出的样品在室温下表现出典型的铁磁性能。
课题通过正交实验确定了在室温下采用溶胶-凝胶法和浸渍提拉技术在载玻片基底上制备纳米钙钛矿型La_(1-x)Sr_xMnO_3薄膜的最佳制备工艺。XRD分析表明,采用络合凝胶法制备出的La_(1-x)Sr_xMnO_3薄膜具有钙钛矿晶型结构,其平均晶粒度为10.32 nm;从薄膜的AFM图像可看出,La_(0.8)Sr_(0.2)MnO_3四层膜比较均匀,其表面粗糙度较小;台阶仪测试得出,薄膜的平均厚度为98.8 nm;
二价金属Sr的掺杂,使该类型薄膜有较好的光催化效果,在9 h内对酸性红A、酸性橙Ⅱ、弱酸性黄C-3GN、直接绿BE、弱酸性蓝C-RL的脱色率分别达到95.56%,89.70%,97.56%,98.40%和91.16%。
Perovskite type compound oxides have stable structure and outstanding performance. The various oxide materials with multiplex component and complex structure may be prepared successfully according to the pattern of metallogeny. Thus,it has aroused an universal interest. In this article, the nano-style perovskite type oxides La_(1-x)Sr_xMnO_3 with smaller grain sizes and better dispersion were prepared and the electric-catalytic activity of powders was researched adequately. La_(0.8)Sr_(0.2)MnO_3 massive sample was prepared under high pressure and agglomeration. The grain evolution regularity and various physical properties were researched for the samples which were prepared under high pressure. The optimum preparation condition and photo-catalysis were researched for La_(1-x)Sr_xMnO_3 thin film on the slide glass base using sol-gel method and dip-coating technology.
The heat decomposition of gel was analyzed by means of TG/DTA and FTIRS; The phase change were analyzed by XRD and its crystal grain size had been calculated; The size of particles and the dispersibility of powders are observed by TEM; The surface area of samples were tested by means of BET; All of above, the optimum preparation condition of perovskite nano-style oxides La_(1-x)Sr_xMnO_3 by citric acid sol-gel method can be obtained.
A kind of new technology is presented for preparing nano-style perovskite powder which has better dispersion. It was that absolute alcohol instead of water as the solvent. It was verified this method could remarkably improve the powders’decentralization and prevent original particles from reuniting. The electric catalysis of La_(0.8)Sr_(0.2)MnO_3 is superiors to the powders which were obtained by the common sol-gel method. It can improve the discharge voltage of air battery to 1.52 V. When the ampere density reaches 150 mA/cm2 and discharge voltage is 1.4 V, the battery can continuous discharge for 15 hours. Thus, the capability of zinc-air battery was increased greatly.
Crystallization process of nano-style oxide powders by high-enemy ball milling with mixing La2O3、MnO_2 and CaO was investigated by using X-ray diffraction patterns and Sherre equation. Results indicated that the La_(0.8)Ca_(0.2)MnO_3 can be synthesized by ball milling18 h under room temperature. The particle size of the powders showed a firstly increasing and subsequent decrescent trend with extending milling time while the grain refinement is limited as time grows.
The compact La_(0.8)Sr_(0.2)MnO_3 massive sample was prepared which crystal grain size less than 100 nm under high pressure and agglomeration. The relationship between relative density of biscuit and forming pressure was analyzed. The grain evolution was researched by XRD、Raman pattern、field emission scanning electron microscopy and the phenomenological kinetic grain growth equation. The results show that it was influenced by temperature and pressure. The grain growth rate under 3 Gpa is increased with increasing pressure while the rate is fall down as pressure continue rise when the agglomeration temperature below 300℃. The grain growth rate is all along increased with pressure increment when the agglomeration temperature over 300℃.
The various physical properties of agglomeration samples under high pressure were studied by testing apparent density、micro-hardness and electromagnetism character. Experimental results indicate that the micro-hardness of samples after high pressure agglomeration was obvious increased and the apparent density is also increased along with pressure. The relative density is 99.48% when sample was prepared under 500℃and 5 GPa. When sintering temperature was 300℃, the resistivity of samples showed first increasing then decreasing trend with increasing pressure and the sample which were prepared under 5 GPa、300℃has obvious ferromagnetic character at room-temperature.
The optimum preparation condition for La_(1-x)Sr_xMnO_3 thin film on the slide glass base using sol-gel method and dip-coating technology was gotten by orthogonal test design method. The phase change was analyzed by XRD and its crystal grain size had been calculated. The result shows that the La_(1-x)Sr_xMnO_3 thin film can be synthesized and average crystal grain size is 10.32 nm. We may see from the AFM Image that the film with four layers is more homogeneous; the surface roughness is less. The average thickness obtained from the step meter is 98.8 nm.
La_(1-x)Sr_xMnO_3 nano-style thin films have better photo-catalysis effect than LaMnO3. The photo-catalytic experiment shows that the de-coloration rates of Acid red A, Acid orangeⅡ,Weak-acid yellow C-3GN, Direct green BE, Weak-acid blue C-RL have reached to 95.56%, 89.70%, 97.56%, 98.40% and 91.16% respectively in 9h.
引文
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