低温烧结热稳定BaTiO_3基陶瓷介质材料研究
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摘要
本文主要研究以BaTiO3基陶瓷介质材料为基础，通过掺杂改性、添加玻璃和不同的制备工艺实现高热稳定性、高介电性能、低温烧结的目标，制造出了满足电子工业协会(Electronic Industries Association,EIA)标准的X7R、X8R、X8R-BX、X9R以及具有超宽温度范围(-55℃到230℃)稳定性的陶瓷介质材料。并且运用现代微观分析手段XRD、SEM等，对其内在机理进行了分析。主要的研究内容及结果如下：
1.我们在BaTiO3基陶瓷材料中，添加5wt%ZnO-B2O3、改变制备工艺，成功的降低了烧结温度，实现低温烧结(烧结温度850℃~930℃)，性能参数如下：室温介电常数ε25oC≥2500,介电损耗tanδ≤1.0%,-55℃到125℃范围内最大电容量变化率不超过±10%。另外，对BaTiO3基陶瓷材料进行改性，添加CaTiO3等添加剂，进行了钽电容器替代产品的探索性研究，并且成功制备了具有正温度特性的BaTiO3基陶瓷介质材料。
2.我们分别讨论了Ho2O3、Er2O3、MnCO3、Bi2O3等添加剂对于BaTiO3陶瓷系统介电性能以及居里峰移动的影响。通过改变制备工艺，在910℃下，成功的制备了满足要求的X8R陶瓷材料，主要性能参数如下：室温介电常数ε25℃>2250,介电损耗tanδ <1.5%,-55℃到150℃范围内最大电容量变化率不超过±13%，满足EIA X8R标准。另外，我们进行了直流偏压特性的研究，成功制备了满足EIAX8R-BX的陶瓷介质材料。
3.我们研究了(BixNa1-x)TiO3(0.4≤x≤0.7)以及xBaTiO3-Bi0.5Na0.5TiO3(x=7,8,9,10,11)的制备工艺和介电性能。并且以此为基础，添加Nb2O5、SrTiO3等添加剂，尝试不同的制备工艺，最终在960℃和1100℃下获得了满足要求的X9R陶瓷介质材料，主要性能参数如下：(a)960℃烧结,室温介电常数ε25oC>1100,介电损耗tanδ <1.0%,-55℃到200℃范围内最大电容量变化率不超过±15%;(b)1100℃烧结,室温介电常数ε25oC>1200,介电损耗tanδ <1.5%,-55℃到200℃范围内最大电容量变化率不超过±15%。另外，我们又获得一种具有超宽温度范围(-55℃到230℃)稳定性的陶瓷介质材料，主要性能参数如下：室温介电常数ε25oC>1000,介电损耗tanδ <1.5%,-55℃到230℃范围内最大电容量变化率不超过±8%。
The preparation of BaTiO3-based ceramics, which had temperature-stable andperfect dielectric properties, sintered at low temperature and doped some glass andoxides were researched in this dissertation.The dielectric properties of the systemssatisfied EIA X7R、X8R、X8R-BX、X9R specifications,even more some werebetter from-55℃to230℃.The principles and mechanism of them was revealed bymodern methods such as XRD, SEM and so on. The main contents and results were asfollows:
1.With adding5wt%ZnO-B2O3and process Optimization,the sintering temperaturewas reduced successfully.The sample sintered at the temperature from850℃to930℃had better dielectric properties,which were as follows: ε25℃≥2500, tanδ≤1.0%,ΔC/C≤±10%in the region of-55~125℃at room temperature. Finally,by addingadditives such as CaTiO3, a new BaTiO3-based ceramic materials wasmanufactured,which had a positive temperature characteristic and can substitute fortantalum capacitors in the certain circumstances. The modified BaTiO3-based ceramicmaterials, adding additives such as CaTiO3exploratory study of of tantalumcapacitors alternative products, and successfully prepared BaTiO3-based ceramicdielectric material having a positive temperature characteristic under certaincircumstance.
2.The effects of Ho2O3,Er2O3,MnCO3,Bi2O3to the dielectric properties and theCurie peak shifted of the system was discussed. By optimization of the process,wefabricated the X8R ceramic materials, of which dielectric properties were asfollows:ε25℃≥2250, tanδ≤1.5%, ΔC/C≤±13%in the region of-55~150℃at roomtemperature. In addition, its characteristics in the DC bias were studied,which metEIA X8R-BX standard.
3.The preparation process and dielectric properties of (BixNa1-x)TiO3(0.4≤x≤0.7)and xBaTiO3-Bi0.5Na0.5TiO3(x=7,8,9,10,11) were studied. With adding additive suchas Nb2O5,SrTiO3, the BaTiO3-based ceramics met EIA X9R specifications wereobtained at eiher960℃or1100℃. Those dielectric properties were as follows:(a)thesample sintered at960℃,ε25℃>1100, tanδ <1.0%, ΔC/C≤±15%in the region of -55~200℃at room temperature;(b) the sample sintered at1100℃, ε25℃>1200,tanδ<1.5%, ΔC/C≤±15%in the region of-55~200℃at room temperature.Furthermore, we also obtained good temperature-stable ceramics at the wide range oftemperature from-55℃to230℃,of which performance were as follows:ε25℃>1000,tanδ <1.5%, ΔC/C≤±15%in the region of-55~230℃at room temperature.
1.我们在BaTiO3基陶瓷材料中，添加5wt%ZnO-B2O3、改变制备工艺，成功的降低了烧结温度，实现低温烧结(烧结温度850℃~930℃)，性能参数如下：室温介电常数ε25oC≥2500,介电损耗tanδ≤1.0%,-55℃到125℃范围内最大电容量变化率不超过±10%。另外，对BaTiO3基陶瓷材料进行改性，添加CaTiO3等添加剂，进行了钽电容器替代产品的探索性研究，并且成功制备了具有正温度特性的BaTiO3基陶瓷介质材料。
2.我们分别讨论了Ho2O3、Er2O3、MnCO3、Bi2O3等添加剂对于BaTiO3陶瓷系统介电性能以及居里峰移动的影响。通过改变制备工艺，在910℃下，成功的制备了满足要求的X8R陶瓷材料，主要性能参数如下：室温介电常数ε25℃>2250,介电损耗tanδ <1.5%,-55℃到150℃范围内最大电容量变化率不超过±13%，满足EIA X8R标准。另外，我们进行了直流偏压特性的研究，成功制备了满足EIAX8R-BX的陶瓷介质材料。
3.我们研究了(BixNa1-x)TiO3(0.4≤x≤0.7)以及xBaTiO3-Bi0.5Na0.5TiO3(x=7,8,9,10,11)的制备工艺和介电性能。并且以此为基础，添加Nb2O5、SrTiO3等添加剂，尝试不同的制备工艺，最终在960℃和1100℃下获得了满足要求的X9R陶瓷介质材料，主要性能参数如下：(a)960℃烧结,室温介电常数ε25oC>1100,介电损耗tanδ <1.0%,-55℃到200℃范围内最大电容量变化率不超过±15%;(b)1100℃烧结,室温介电常数ε25oC>1200,介电损耗tanδ <1.5%,-55℃到200℃范围内最大电容量变化率不超过±15%。另外，我们又获得一种具有超宽温度范围(-55℃到230℃)稳定性的陶瓷介质材料，主要性能参数如下：室温介电常数ε25oC>1000,介电损耗tanδ <1.5%,-55℃到230℃范围内最大电容量变化率不超过±8%。
The preparation of BaTiO3-based ceramics, which had temperature-stable andperfect dielectric properties, sintered at low temperature and doped some glass andoxides were researched in this dissertation.The dielectric properties of the systemssatisfied EIA X7R、X8R、X8R-BX、X9R specifications,even more some werebetter from-55℃to230℃.The principles and mechanism of them was revealed bymodern methods such as XRD, SEM and so on. The main contents and results were asfollows:
1.With adding5wt%ZnO-B2O3and process Optimization,the sintering temperaturewas reduced successfully.The sample sintered at the temperature from850℃to930℃had better dielectric properties,which were as follows: ε25℃≥2500, tanδ≤1.0%,ΔC/C≤±10%in the region of-55~125℃at room temperature. Finally,by addingadditives such as CaTiO3, a new BaTiO3-based ceramic materials wasmanufactured,which had a positive temperature characteristic and can substitute fortantalum capacitors in the certain circumstances. The modified BaTiO3-based ceramicmaterials, adding additives such as CaTiO3exploratory study of of tantalumcapacitors alternative products, and successfully prepared BaTiO3-based ceramicdielectric material having a positive temperature characteristic under certaincircumstance.
2.The effects of Ho2O3,Er2O3,MnCO3,Bi2O3to the dielectric properties and theCurie peak shifted of the system was discussed. By optimization of the process,wefabricated the X8R ceramic materials, of which dielectric properties were asfollows:ε25℃≥2250, tanδ≤1.5%, ΔC/C≤±13%in the region of-55~150℃at roomtemperature. In addition, its characteristics in the DC bias were studied,which metEIA X8R-BX standard.
3.The preparation process and dielectric properties of (BixNa1-x)TiO3(0.4≤x≤0.7)and xBaTiO3-Bi0.5Na0.5TiO3(x=7,8,9,10,11) were studied. With adding additive suchas Nb2O5,SrTiO3, the BaTiO3-based ceramics met EIA X9R specifications wereobtained at eiher960℃or1100℃. Those dielectric properties were as follows:(a)thesample sintered at960℃,ε25℃>1100, tanδ <1.0%, ΔC/C≤±15%in the region of -55~200℃at room temperature;(b) the sample sintered at1100℃, ε25℃>1200,tanδ<1.5%, ΔC/C≤±15%in the region of-55~200℃at room temperature.Furthermore, we also obtained good temperature-stable ceramics at the wide range oftemperature from-55℃to230℃,of which performance were as follows:ε25℃>1000,tanδ <1.5%, ΔC/C≤±15%in the region of-55~230℃at room temperature.
引文
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