钙钛矿结构锰氧化物La_（1-x）Ca_xMnO_3的红外光学性质研究
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摘要
自从巨磁阻效应发现以来,具有钙钛矿结构的锰氧化物La1-xCaxMnO3一直备受人们的关注。因为其电荷、轨道、自旋、晶格之间的复杂的相互作用和影响,导致了其丰富的物理内涵,如磁性的转变,金属-绝缘体的转变,电荷有序态,相分离等现象。锰氧化物La1-xCaxMnO3是在母体材料LaMnO3基础上掺杂Ca替代La的位置,得到不同价态的锰离子,改变了原来母体材料的结构。随之而来的是其内在的微观作用的变化和微纳米尺度上的本征不均匀性,导致体系宏观物理性质的变化。这种掺杂的方式带来的很多的结构和相互作用的变化,丰富了这类强关联体系锰氧化物材料的物理内涵及其在实际生活生产的应用领域。
本文采用了溶胶-凝胶法制备了La1-xCaxMnO3 (x=0.5,0.67,0.75)系列粉体样品,采用了固相法制备了La1-xCaxMnO3 (x=0.5,0.67,0.75)系列块材样品。系统地研究了高掺杂的钙钛矿型锰氧化物La1-xCaxMnO3 (x=0.5,0.67,0.75)样品的电磁性质和红外光学性质。
我们运用X射线衍射仪测量了样品在室温下的X射线衍射图像对样品结构进行了研究,并应用Rietica精修软件拟合得到了样品的晶胞参数数据。对于粉体样品,我们系统的研究了烧结温度对样品结构特征的影响,发现随着烧结温度的升高,样品的结晶性越好,晶粒尺寸越大,样品的钙掺杂浓度越高时,样品成相所需要的烧结温度就越高。对于块材样品,我们发现随着钙掺杂浓度的升高,样品的晶胞体积和晶粒尺寸都有所增大。
对样品磁性的研究中,我们使用超导量子干涉仪(SQUID)和振动样品磁强计(VSM)测量了样品在μ0H=0.1T和1T外加磁场下的磁性质,发现随着钙掺杂浓度的提高,各样品都存在顺磁—反铁磁转变行为,且顺磁—反铁磁转变温度在不同的钙掺杂情况下不同。
对样品电学性质的研究中,我们运用标准的四探针法测量了样品在无外加磁场的条件下,在75K-300K的温度范围内的电阻率随温度变化的曲线。详细分析结果发现样品表现为绝缘体。电阻率对数对温度的导数曲线显示了样品的电荷有序相变点,有序相变的温度也因钙的掺杂量的不同而不同。
对样品的红外光学性质的研究中,对于粉体样品,我们运用傅立叶变换红外光谱仪测试了不同烧结温度所得样品的红外吸收光谱图,发现随着烧结温度的升高,Mn06八面体结构的扭曲度越小,振动频率越低。对于块材样品,我们在室温到液氮的温度范围内,每隔10K取—个温度点,利用同步辐射红外光谱仪测量了样品在4500-370cm-1,700-20cm-1的波段区间的中红外和远红外反射光谱图。通过软件拟合得到样品在上述频率区间连续完整的反射率曲线。并运用Kramers-Kroning分析,从反射率光谱数据得到样品的光电导率曲线及介电常数曲线。通过对这些红外光谱图的分析,发现La1-xCaxMnO3(x=0.5,0.67,0.75)系列样品都存在一个相变温度点,结合磁性和电输运性质的研究,揭示了样品的微观结构和性质随温度的变化。
The perovskite structure manganese oxide R1-xAxMnO3 (R:3 valence rare earth, A:2 valence alkaline earth) are paid attention since the discovery of colossal magnetoresistive effect. The complex interaction and interplay among the charge, orbital, spin and lattice give rise to the abundant physics properties the magnetic transition, metal-insulator transformation, charge-order and phase separation. Manganese Lai1-xCaxMnO3 that origins from the matrix of LaMnO3 by replacing the La with the Ca change the matrix structure and bring about the different valence of Mn. The change of micro role and the intrinsic inhomogeneity on micro-nanometer scale give rise to the change of the macroscopic physical properties. The change of structure and interaction enrich the physical sense and the application in life of this kind of strong-correlation manganese material.
The series of power and bulk sample of La1-xCaxMnO3 (x=0.5,0.67,0.75) are prepared by sol-gel and solid-state method respectively. The electronic, magnetic and infrared properties of high-doped manganese La1-xCaxMnO3 (x=0.5,0.67,0.75) are studied systematically.
The X-ray diffraction is applied to analyze structure of La1-xCaxMnO3 (x=0.5,0.67, 0.75). And the lattice structure parameter of La1-xCaxMnO3=0.5,0.67,0.75)is fitted by means of the Rietica refinement software. The studies of influence of sintering temperature on the structural characteristic signify that the higher sintering temperature will generate the better crystallinity and the bigger grain. Moreover, the more density doping of Ca require the higher sintering temperature. For bulk material, along with the increase of doping density of Ca, the volume of cell and the size of grain magnify.
The SQUID and VSM are employed for the magnetic properties of these manganese La1-xCaxMnO3 (x=0.5,0.67,0.75)underμ0H= 0.1 and 1T. As the doping density of Ca increase, the transformations from paramagnetic to the anti-ferromagnetic occur for every sample with different transformation temperature.
The standard four probe method is used for the electrical properties under zero magnetic fields and the curve of resistivity with the changing temperature at the range of 75K-300K. These samples are insulator on the basis of careful analysis about the results. The curve of differential coefficient of logarithm of resistivity about temperature displays the different charge-order phase transition for different doping density of Ca. For infrared properties of these samples, Fourierf transformation infrared spectrometer is applied to measure the infrared absorption spectrum of power samples obtained in different sintering temperature. We found the distortion of octahedral structure and the frequency decrease with the increasing sintering temperature. For bulk sample, synchrotron radiation infrared spectrograph is used for intermediate infrared (4500～370cm-1) and far infrared (700～20cm-1) at the interval of 10K from room temperature to the temperature of liquid nitrogen. The whole refraction curve at the range of intermediate and far infrared is fitted by appropriated software. Conductivity and permittivity can be obtained from the refraction spectrum data by means of Kramers-Kroning analysis. All these analysis about infrared spectrum show that the manganese La1-xCaxMnO3 (x=0.5,0.67,0.75) samples have phase transformation temperature, and the change of micro structures, electrical and magnetic properties according to the magnetic and electrical transport mechanism.
本文采用了溶胶-凝胶法制备了La1-xCaxMnO3 (x=0.5,0.67,0.75)系列粉体样品,采用了固相法制备了La1-xCaxMnO3 (x=0.5,0.67,0.75)系列块材样品。系统地研究了高掺杂的钙钛矿型锰氧化物La1-xCaxMnO3 (x=0.5,0.67,0.75)样品的电磁性质和红外光学性质。
我们运用X射线衍射仪测量了样品在室温下的X射线衍射图像对样品结构进行了研究,并应用Rietica精修软件拟合得到了样品的晶胞参数数据。对于粉体样品,我们系统的研究了烧结温度对样品结构特征的影响,发现随着烧结温度的升高,样品的结晶性越好,晶粒尺寸越大,样品的钙掺杂浓度越高时,样品成相所需要的烧结温度就越高。对于块材样品,我们发现随着钙掺杂浓度的升高,样品的晶胞体积和晶粒尺寸都有所增大。
对样品磁性的研究中,我们使用超导量子干涉仪(SQUID)和振动样品磁强计(VSM)测量了样品在μ0H=0.1T和1T外加磁场下的磁性质,发现随着钙掺杂浓度的提高,各样品都存在顺磁—反铁磁转变行为,且顺磁—反铁磁转变温度在不同的钙掺杂情况下不同。
对样品电学性质的研究中,我们运用标准的四探针法测量了样品在无外加磁场的条件下,在75K-300K的温度范围内的电阻率随温度变化的曲线。详细分析结果发现样品表现为绝缘体。电阻率对数对温度的导数曲线显示了样品的电荷有序相变点,有序相变的温度也因钙的掺杂量的不同而不同。
对样品的红外光学性质的研究中,对于粉体样品,我们运用傅立叶变换红外光谱仪测试了不同烧结温度所得样品的红外吸收光谱图,发现随着烧结温度的升高,Mn06八面体结构的扭曲度越小,振动频率越低。对于块材样品,我们在室温到液氮的温度范围内,每隔10K取—个温度点,利用同步辐射红外光谱仪测量了样品在4500-370cm-1,700-20cm-1的波段区间的中红外和远红外反射光谱图。通过软件拟合得到样品在上述频率区间连续完整的反射率曲线。并运用Kramers-Kroning分析,从反射率光谱数据得到样品的光电导率曲线及介电常数曲线。通过对这些红外光谱图的分析,发现La1-xCaxMnO3(x=0.5,0.67,0.75)系列样品都存在一个相变温度点,结合磁性和电输运性质的研究,揭示了样品的微观结构和性质随温度的变化。
The perovskite structure manganese oxide R1-xAxMnO3 (R:3 valence rare earth, A:2 valence alkaline earth) are paid attention since the discovery of colossal magnetoresistive effect. The complex interaction and interplay among the charge, orbital, spin and lattice give rise to the abundant physics properties the magnetic transition, metal-insulator transformation, charge-order and phase separation. Manganese Lai1-xCaxMnO3 that origins from the matrix of LaMnO3 by replacing the La with the Ca change the matrix structure and bring about the different valence of Mn. The change of micro role and the intrinsic inhomogeneity on micro-nanometer scale give rise to the change of the macroscopic physical properties. The change of structure and interaction enrich the physical sense and the application in life of this kind of strong-correlation manganese material.
The series of power and bulk sample of La1-xCaxMnO3 (x=0.5,0.67,0.75) are prepared by sol-gel and solid-state method respectively. The electronic, magnetic and infrared properties of high-doped manganese La1-xCaxMnO3 (x=0.5,0.67,0.75) are studied systematically.
The X-ray diffraction is applied to analyze structure of La1-xCaxMnO3 (x=0.5,0.67, 0.75). And the lattice structure parameter of La1-xCaxMnO3=0.5,0.67,0.75)is fitted by means of the Rietica refinement software. The studies of influence of sintering temperature on the structural characteristic signify that the higher sintering temperature will generate the better crystallinity and the bigger grain. Moreover, the more density doping of Ca require the higher sintering temperature. For bulk material, along with the increase of doping density of Ca, the volume of cell and the size of grain magnify.
The SQUID and VSM are employed for the magnetic properties of these manganese La1-xCaxMnO3 (x=0.5,0.67,0.75)underμ0H= 0.1 and 1T. As the doping density of Ca increase, the transformations from paramagnetic to the anti-ferromagnetic occur for every sample with different transformation temperature.
The standard four probe method is used for the electrical properties under zero magnetic fields and the curve of resistivity with the changing temperature at the range of 75K-300K. These samples are insulator on the basis of careful analysis about the results. The curve of differential coefficient of logarithm of resistivity about temperature displays the different charge-order phase transition for different doping density of Ca. For infrared properties of these samples, Fourierf transformation infrared spectrometer is applied to measure the infrared absorption spectrum of power samples obtained in different sintering temperature. We found the distortion of octahedral structure and the frequency decrease with the increasing sintering temperature. For bulk sample, synchrotron radiation infrared spectrograph is used for intermediate infrared (4500～370cm-1) and far infrared (700～20cm-1) at the interval of 10K from room temperature to the temperature of liquid nitrogen. The whole refraction curve at the range of intermediate and far infrared is fitted by appropriated software. Conductivity and permittivity can be obtained from the refraction spectrum data by means of Kramers-Kroning analysis. All these analysis about infrared spectrum show that the manganese La1-xCaxMnO3 (x=0.5,0.67,0.75) samples have phase transformation temperature, and the change of micro structures, electrical and magnetic properties according to the magnetic and electrical transport mechanism.
引文
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