钨青铜结构晶体Ca_（0.28）Ba_（0.72）Nb_2O_6结构与物性机理研究
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摘要
由于钨青铜结构铌酸盐具有良好的压电、铁电和非线性光学性质,他们已经被广泛地应用于激光倍频、电光调制、光信息处理等领域。SBN晶体由于具有良好的电学和光学性质,所以已经投入广泛地应用。但由于其居里温度只有60℃,这就在很大程度上限制了其在高温下的应用。2001年德国科隆大学一个研究小组首次成功利用提拉法生长出Ca_(0.28)Ba_(0.72)Nb_2O_6(CBN-28)晶体。发现其居里温度在265℃,比SBN晶体高出近200℃。因此可以推测CBN-28晶体有着更为宽广的潜在应用前景。
对于一种新的压电铁电晶体材料来说,除了要具备良好的压电铁电特性,它的光谱特性(如透过光谱、晶格振动光谱等)、热机械特性(如热膨胀、热切削性等)和热力学特性(如热容、热扩散、热导率等)也非常重要,并且直接影响着晶体的应用。只有各方面性质综合起来都不错,晶体才能具有优良的应用价值。所以对该晶体进行物性机理研究具有重要意义。
本文对CBN-28晶体的光谱特性和热特性进行了实验结果进行了介绍,并与其他钨青铜结构铌酸盐晶体进行了比较分析。本文还对CBN-28晶体的电学特性进行了测量,并对钨青铜结构晶体的锥光干涉条纹进行了实验拍摄。主要包括以下几方面工作:
一、根据空间群理论计算并分析了CBN-28晶体的晶格振动模。利用Raman散射和红外吸收实验对晶体的晶格振动模进行验证,并取得了与理论分析一致的结果。钨青铜结构晶体的特征峰主要是八面体结构的5支光学活性振动模引起的。并对不同配置的Raman光谱和红外吸收光谱的特征峰进行了指认,发现Raman峰有展宽的情况,这主要是由于组成钨青铜结构的八面体发生畸变导致的。
二、对CBN-28晶体的热特性进行了测试。采用差示扫描量热计对CBN-28晶体的比热进行测量,测出从20℃到500℃的比热值为0.455-0.770J/g·℃。并发现在晶体相变居里点处有比热峰出现,这是晶体相变时存在相变潜热导致的结果。采用热机分析仪对CBN-28、Cu:KNSBN晶体的热膨胀曲线进行测量。在这两种晶体中均发现在居里点附近,热膨胀系数发生很大变化。采用闪光脉冲法对晶体的热扩散系数进行测量,并由此计算出晶体的热导率。
三、采用双光束型分光光度计对CBN-28晶体和其他一些钨青铜结构铌酸盐晶体的透过光谱进行测量和比较。发现非掺杂的钨青铜结构晶体的紫外吸收边一般在380nm。而掺杂离子后紫外吸收边向低频方向移动。并且对晶体对偏振光的透过特性进行了测量。
四、对CBN-28晶体的介电特性进行测量。测量了介电谱和介电损耗。发现CBN-28晶体的居里点在260℃,并且发现在低频交变电场1KHz下240℃处该晶体有较大的介电损耗。应尽量避免在这种条件下使用该晶体。
五、对钨青铜结构铌酸盐SBN和Cu:KNSBN晶体的锥光干涉现象进行了拍摄。发现SBN和Cu:KNSBN晶体都是单轴晶。并分别对光线平行于光轴入射和垂直于光轴入射的锥光干涉现象进行了分析。
As tetragonal tungsten bronze niobates have excellent piezoelectric, ferroelectric and non-linear optical characters, they have been widely used in laser frequency doubling, electro-optic modulation, optical information and other related areas. SBN crystal has very excellent electrical and optical characters, so it has been widely used. But the Curie temperature of SBN is 60℃, the application in high temperature is very limited. In 2001, CBN-28 crystal was grown by a group of Kolon University Germany for the first time. They found that the Curie temperature of CBN-28 is 265℃, which is nearly 200℃higher than SBN. It predicated that CBN-28 crystal has more potential applications.
Not only good piezoelectrical and ferroelectrical properties but also good spectral, thermomechanical, thermodynamic characters are very important to a new ferroelectrical crystal. They affect the application of a new crystal directly. So it is important to do some properties research of the crystal. In this thesis, the spectral and thermal experiments results of CBN-28 were introduced, and were compared with some other tetragonal tungsten bronze crystals. Some dielectric experiments were also introduced in this thesis. Some conoscopic interferential pictures of tetragonal tungsten bronze niobates crystals were shown. The main works of thesis are as follows:
1. Based on the space group theory, the lattice vibrational modes of CBN-28 were predicted. The modes were observed by Raman scattering and infrared absorption spectroscopy, and the results were identical to the theory. There are 3 characteristic Raman peaks and 2 characteristic infrared absorption spectroscopy peaks belonging to the internal vibrational modes of octahedral structure in tetragonal tungsten bronzea crystals. We identified the characteristic peaks in different geometry Raman scattering and infrared absorption spectroscopy. The Raman peaks relaxation of the line width is due to the distortion of octahedral ions.
2. The specific heat were measured by the differential scanning calorimetry method, which the value is 0.455-0.770J/g·℃from the temperature 20℃to 500℃. A specific heat peak at Curie temperature of CBN-28 crystal was found. Thermal expansion of CBN-28 and Cu:KNSBN were measured by thermomechanical analysis. The thermal expansion coefficients of the two crystals changed greatly at Curie temperature. Thermal diffusion coefficient was measured by flash method, and the thermal conductivity of CBN-28 was also calculated.
3. The transmission of CBN-28 crystals was measured by a UV/VIS/NIR spectrophotometer, and the transmission was compared with other tetragonal tungsten bronze crystals. The ultraviolet absorption edge of non-doped crystal was usually at 380 nm. Polarized transmission of CBN-28 was also measured.
4. Dielectric constant and dielectric loss were measured. We found the Curie temperature of CBN-28 is 260℃. There is a dielectric loss peak at the frequency of 1KHz in 240℃.
5. Some photos of conoscopic interference of tetragonal tungsten bronze structure crystals were shown in this thesis. Both SBN and Cu:KNSBN are uniaxis crystals. The phenomenons of convergent light for a uniaxis crystal with optical axis vertical and parallel to surface are also discussed in this thesis.
对于一种新的压电铁电晶体材料来说,除了要具备良好的压电铁电特性,它的光谱特性(如透过光谱、晶格振动光谱等)、热机械特性(如热膨胀、热切削性等)和热力学特性(如热容、热扩散、热导率等)也非常重要,并且直接影响着晶体的应用。只有各方面性质综合起来都不错,晶体才能具有优良的应用价值。所以对该晶体进行物性机理研究具有重要意义。
本文对CBN-28晶体的光谱特性和热特性进行了实验结果进行了介绍,并与其他钨青铜结构铌酸盐晶体进行了比较分析。本文还对CBN-28晶体的电学特性进行了测量,并对钨青铜结构晶体的锥光干涉条纹进行了实验拍摄。主要包括以下几方面工作:
一、根据空间群理论计算并分析了CBN-28晶体的晶格振动模。利用Raman散射和红外吸收实验对晶体的晶格振动模进行验证,并取得了与理论分析一致的结果。钨青铜结构晶体的特征峰主要是八面体结构的5支光学活性振动模引起的。并对不同配置的Raman光谱和红外吸收光谱的特征峰进行了指认,发现Raman峰有展宽的情况,这主要是由于组成钨青铜结构的八面体发生畸变导致的。
二、对CBN-28晶体的热特性进行了测试。采用差示扫描量热计对CBN-28晶体的比热进行测量,测出从20℃到500℃的比热值为0.455-0.770J/g·℃。并发现在晶体相变居里点处有比热峰出现,这是晶体相变时存在相变潜热导致的结果。采用热机分析仪对CBN-28、Cu:KNSBN晶体的热膨胀曲线进行测量。在这两种晶体中均发现在居里点附近,热膨胀系数发生很大变化。采用闪光脉冲法对晶体的热扩散系数进行测量,并由此计算出晶体的热导率。
三、采用双光束型分光光度计对CBN-28晶体和其他一些钨青铜结构铌酸盐晶体的透过光谱进行测量和比较。发现非掺杂的钨青铜结构晶体的紫外吸收边一般在380nm。而掺杂离子后紫外吸收边向低频方向移动。并且对晶体对偏振光的透过特性进行了测量。
四、对CBN-28晶体的介电特性进行测量。测量了介电谱和介电损耗。发现CBN-28晶体的居里点在260℃,并且发现在低频交变电场1KHz下240℃处该晶体有较大的介电损耗。应尽量避免在这种条件下使用该晶体。
五、对钨青铜结构铌酸盐SBN和Cu:KNSBN晶体的锥光干涉现象进行了拍摄。发现SBN和Cu:KNSBN晶体都是单轴晶。并分别对光线平行于光轴入射和垂直于光轴入射的锥光干涉现象进行了分析。
As tetragonal tungsten bronze niobates have excellent piezoelectric, ferroelectric and non-linear optical characters, they have been widely used in laser frequency doubling, electro-optic modulation, optical information and other related areas. SBN crystal has very excellent electrical and optical characters, so it has been widely used. But the Curie temperature of SBN is 60℃, the application in high temperature is very limited. In 2001, CBN-28 crystal was grown by a group of Kolon University Germany for the first time. They found that the Curie temperature of CBN-28 is 265℃, which is nearly 200℃higher than SBN. It predicated that CBN-28 crystal has more potential applications.
Not only good piezoelectrical and ferroelectrical properties but also good spectral, thermomechanical, thermodynamic characters are very important to a new ferroelectrical crystal. They affect the application of a new crystal directly. So it is important to do some properties research of the crystal. In this thesis, the spectral and thermal experiments results of CBN-28 were introduced, and were compared with some other tetragonal tungsten bronze crystals. Some dielectric experiments were also introduced in this thesis. Some conoscopic interferential pictures of tetragonal tungsten bronze niobates crystals were shown. The main works of thesis are as follows:
1. Based on the space group theory, the lattice vibrational modes of CBN-28 were predicted. The modes were observed by Raman scattering and infrared absorption spectroscopy, and the results were identical to the theory. There are 3 characteristic Raman peaks and 2 characteristic infrared absorption spectroscopy peaks belonging to the internal vibrational modes of octahedral structure in tetragonal tungsten bronzea crystals. We identified the characteristic peaks in different geometry Raman scattering and infrared absorption spectroscopy. The Raman peaks relaxation of the line width is due to the distortion of octahedral ions.
2. The specific heat were measured by the differential scanning calorimetry method, which the value is 0.455-0.770J/g·℃from the temperature 20℃to 500℃. A specific heat peak at Curie temperature of CBN-28 crystal was found. Thermal expansion of CBN-28 and Cu:KNSBN were measured by thermomechanical analysis. The thermal expansion coefficients of the two crystals changed greatly at Curie temperature. Thermal diffusion coefficient was measured by flash method, and the thermal conductivity of CBN-28 was also calculated.
3. The transmission of CBN-28 crystals was measured by a UV/VIS/NIR spectrophotometer, and the transmission was compared with other tetragonal tungsten bronze crystals. The ultraviolet absorption edge of non-doped crystal was usually at 380 nm. Polarized transmission of CBN-28 was also measured.
4. Dielectric constant and dielectric loss were measured. We found the Curie temperature of CBN-28 is 260℃. There is a dielectric loss peak at the frequency of 1KHz in 240℃.
5. Some photos of conoscopic interference of tetragonal tungsten bronze structure crystals were shown in this thesis. Both SBN and Cu:KNSBN are uniaxis crystals. The phenomenons of convergent light for a uniaxis crystal with optical axis vertical and parallel to surface are also discussed in this thesis.
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