摘要
本文系统研究了BaO-TiO_2-SiO_2体系中BaTiSi_2O_7相,分别制备了BaTiSi_2O_7陶瓷和Ba_2TiSi_2O_8极性玻璃陶瓷,并分析了BaTiSi_2O_7的结构与性能以及掺杂不同氧化物对Ba_2TiSi_2O_8极性玻璃陶瓷性能的影响。
采用传统氧化物混合法制备了BaTiSi_2O_7陶瓷,通过调节烧结温度,组成,利用DSC、IR、XRD、Raman、SEM等测试手段,确定了BaTiSi_2O_7陶瓷的烧结工艺制度。实验结果表明,制备BaTiSi_2O_7陶瓷需要在900℃和1000℃两次预烧, 首先生成中间相-Ba2TiSi_2O_8相,然后在1145℃烧结生产高纯BaTiSi_2O_7相。此外,BaTiSi_2O_7陶瓷对组成变化极为敏感,BaTiO_3和SiO_2比值低于1:2时,主晶相为Ba_2TiSi_2O_8相,还含有BaTiSi_2O_7相;高于1:2时,则主晶相转变为BaTiSi_2O_7相。因此,BaTiO_3和SiO_2的比例应当严格控制在1:2。通过对DSC曲线积分处理,计算出BaTiO_3和SiO2生成BaTiSi_2O_7相的活化能约为366KJ/mol。
通过IR、XRD、Raman等测试手段分析了BaTiSi_2O_7陶瓷结构,实验表明样品中含有TiO_5四方单锥结构和独立的硅氧环状结构。BaTiSi_2O_7陶瓷的介电常数在0.1K~1GHz频率范围内为10~8,介电损耗在10-4左右。
通过XRD、SEM、压电常数d33等分析了掺杂氧化物CaO和ZrO_2对Ba2TiSi_2O_8极性玻璃陶瓷性能的影响,并得出以下结论:加入氧化钙和氧化锆不会改变主晶相,但加入氧化锆将使玻璃陶瓷中出现BaZrSi_3O_9第二相;此外,加入氧化钙有利于BTS晶体的定向析出,使d33增加,相反,加入氧化锆则不利于BTS晶体的定向析出,使d33减小。
The paper studies the phase of BaTiSi_2O_7 in the system of BaO-TiO_2-SiO_2, and prepares BaTiSi_2O_7 ceramic and polar Ba2TiSi2O8 glass ceramic,analyses the structure and properties of BaTiSi_2O_7,investigates the crystalline of the polar Ba_2TiSi_2O_8 glass ceramic with additive oxide.
The paper prepares ceramic of BaTiSi_2O_7 by the method of traditional oxide mixture, gives the sintering technology of BaTiSi2O7 ceramic with the method of DSC, IR, XRD, Raman, SEM by controlling tempt rue and composition. It is concluded that it is necessary calcining at 900℃ and 1000℃ to prepare BaTiSi_2O_7 ceramic. BaTiSi_2O_7 ceramic is sensitive to variety of composition, when the proportion of BaTiO3 and SiO2 is under 1:2, the main phase is Ba2TiSi2O8, and there id BaTiSi2O7 also;When it is above1:2, the main phase is BaTiSi2O7; so the proportion of BaTiO3 and SiO2 must be strictly controlled at 1:2. Additionally, we calculate the activation energy of BaTiSi2O7 phase synthesized by BaTiO3 and SiO2 by integrating the curve of DSC, and the activation energy is about 366KJ/mol. We analyze the structure of BaTiSi2O7 ceramic by methods of IR、XRD、Raman etc, the results indicate that there is structure of TiO5 pyramids and independent ring of silica oxide. The dielectric constant of BaTiSi_2O_7 is 10~8 in the frequency of 0.1K~1GHz, and the dielectric loss is about 10-4.
We analyze the properties of polar Ba_2TiSi_2O_8 glass ceramic with additive CaO and ZrO_2 by XRD, SEM, d33 etc. And we conclude that: Additive CaO and ZrO2 can not influence the main phase, but the phase of BaZrSi_3O_9 occur; moreover, it is advantage to oriental crystallize BTS with CaO and disadvantage to crystallize BST
with ZrO2.
引文
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