摘要
高四方性的BaTiO_(3)超细粉体是下一代多层陶瓷电容器的关键材料。该文探究了砂磨介质尺寸和原料Ti O_(2)晶相对反应物活性、产物介电性能的影响,并利用砂磨固相法成功合成了高四方性Ba TiO_(3)超细粉体。分析场发射扫描电子显微镜照片和X射线光电子能谱发现,细砂磨介质粉碎原料的效率更高,机械活化作用更强。Raman光谱和X射线衍射图谱显示,在高能砂磨过程中,TiO_(2)由锐钛矿相先后转变为TiO_(2)-Ⅱ相、金红石相。分析微商热重曲线和X射线衍射,结果表明,砂磨介质更能有效降低反应温度和抑制Ba_(2)TiO_(4)的生成。此外,高分辨透射电子显微镜图像揭示了BaTiO 3的形成是Ba^(2+)向TiO_(2)晶格扩散的过程。该文相关实验结果表明,利用直径为0.1 mm的ZrO_(2)磨球对锐钛矿相TiO_(2)和BaCO_(3)混合物砂磨4 h,并在1100℃煅烧3 h后,获得了平均粒径为186 nm、四方性为1.0092且分散性良好的BaTiO_(3)粉体,该粉体在1250℃烧结的陶瓷相对密度为96.11%,居里点(137.8℃)的介电常数峰值为8677。
Ultra-fine BaTiO_(3) powder with high tetragonality is the key material for the next generation of multilayer ceramic capacitors.In this paper,effects of medium size of the sand-milling and the phase of the raw TiO_(2) on the reaction activity and dielectric properties of the product were investigated,and ultrafine BaTiO_(3) powder with high tetragonality was synthesized via the sand-milling process.Field emission scanning electron microscope images and X-ray photoelectron spectroscopy showed that the fine sand-milling media was more effective in crushing raw materials and mechanical activation.Raman spectroscopy and X-ray diffraction pattern proved that the anatase phase of TiO_(2) was transformed into TiO_(2)-Ⅱ phase and rutile phase successively during the sand-milling process.Derivative thermogravimetry and X-ray diffraction analysis proved thatfine sand-milling media was better at lowering the reaction temperature and inhibiting the formation of Ba_(2)TiO_(4).The high resolution transmission electron microscopy image revealed that the formation of BaTiO_(3) is a process by which Ba^(2+)diffuses into the TiO_(2) lattice.The anatase TiO_(2)/BaCO_(3) mixture were sand-milled for 4 h,using ZrO_(2) balls with a diameter of 0.1 mm,and calcined at 1100℃for 3 h.Then a well-dispersed BaTiO_(3) powder with an average particle size of 186 nm and tetragonality of 1.0092 was obtained.Sintered at 1250℃,the density of the ceramic derived of as-prepared powder was 96.11%,and the peak value of the dielectric constant at the Curie point(137.8℃)was 8677.
作者
司韶康
张蕾
温佳鑫
于淑会
曹秀华
付振晓
孙蓉
SI Shaokang;ZHANG Lei;WEN Jiaxin;YU Shuhui;CAO Xiuhua;FU Zhenxiao;SUN Rong(Shenzhen Institute of Advanced Electronic Materials,Shenzhen Institute of Advanced Technology,Chinese Academy of Sciences,Shenzhen 518055,China;Nano Science and Technology Institute,University of Science and Technology of China,Suzhou 215123,China;Academy for Advanced Interdisciplinary Studies,Southern University of Science and Technology,Shenzhen 518055,China;State Key Laboratory of Advanced Materials and Electronic Components,Guangdong Fenghua Advanced Technology Holding Co.,Ltd.,Zhaoqing 526060,China)
出处
《集成技术》
2022年第3期108-120,共13页
Journal of Integration Technology
基金
国家自然科学基金项目(51802142)
新型电子元器件关键材料与工艺国家重点实验室项目(FHR-JS-202011012,FHR-JS-202011013,FHR-JS-202011014)
先进电子元器件联合创新中心(FHR-JS-202103001)。
