CN105777115A - 一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法 - Google Patents

一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法 Download PDF

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CN105777115A
CN105777115A CN201610149060.9A CN201610149060A CN105777115A CN 105777115 A CN105777115 A CN 105777115A CN 201610149060 A CN201610149060 A CN 201610149060A CN 105777115 A CN105777115 A CN 105777115A
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strontium titanate
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CN105777115B (zh
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詹丽君
洑义达
左真国
陆婵娟
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JIANGSU PROV CERAMIC RESEARCH INST Co Ltd
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Abstract

本发明涉及一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，通过利用钛酸锶、钛酸钡、钛酸锆基实现使BST陶瓷材料在室温范围内实现介电特性，采用多元掺杂和协同补偿提高产品性能。结果表明：该材料具有高介低损耗高耐压特性，且该产品易于设计，节约成本。

Description

一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法
技术领域
本发明属于高压陶瓷电容器领域，特别涉及一种多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料。
背景技术
钛酸锶钡（Ba1-xSrxTiO3,简称BST）基陶瓷材料是一种铁电材料，具有高绝缘电阻，低介电损耗，通过改变材料组成和微量掺杂改性，可以将材料调整到合适范围的介电常数和居里温度，同时在一定程度上保证材料具有很好稳定的介温特性。随着现代移动通讯、LED、航空航天领域的快速发展，电子元器件日益小型化和集成化，迫切需要耐高压、容量大、损耗小、稳定性好的高性能的陶瓷电容器。
目前这类高性能陶瓷电容器所用材料主要有两种：SrTiO3系陶瓷和BaTiO3系陶瓷。SrTiO3陶瓷具有介电常数随电压变化小，介质损耗低以及抗电强度高等优点；但是室温时介电常数仅为250左右。BaTiO3居里温度在120℃左右，居里点处介电常数可达105，室温时也有较大的介电常数，但是它的损耗较大，介电常数随电压变化大。因此纯SrTiO3和BaTiO3并不能满足中高压电容器陶瓷介质材料的要求。高压电容器陶瓷的研发主要集中于添加剂对SrTiO3与BaTiO3复相陶瓷介质材料进行改性，以获得适合工业应用的高性能电容器陶瓷介质材料。
要达到上述高性能钛酸锶钡陶瓷电容器，就必须取代传统得单一各相掺杂，利用各元素之间的特性，协同作用，制备市场所需的材料。
发明内容
本发明针对现有技术的不足，提供一种具有良好介电常数、低介电损耗，能承受较高耐压，而且能便捷得生产设计产品的制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法。
为实现本发明目的，提供了以下技术方案：一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于包括以下步骤：
a.制备Bi2O3·3TiO2：以1molBi2O3、3molTiO2为标准比例，湿法球磨使其混合均匀，压滤后800~850℃保温2~3h，得到Bi2O3·3TiO2；
b．制备BaTiO3和SrTiO3：分析纯BaCO3、SrCO3分别和TiO2按照物质的量1:1比例混合均匀，湿法球磨使其混合均匀，压滤后1180~1200℃保温2~3h，制备BaTiO3和SrTiO3；
c．制备CaZrO3：分析纯CaCO3与ZrO2按照等物质的量混合均匀，在电炉内1250℃保温2h冷却得到CaZrO3；
d．根据生产设计需求制备BST陶瓷材料，（1-z）[（Ba1-x-ySrxCay）Ti1-yZryO3]·z(Bi2O3·3TiO2)，0.3≤x≤0.4，0<y<0.15，0.02<z≤0.04，加入上述BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，计总重量；
e．按质量比加入Ce2O3:0~0.5wt%，Y2O3:0~0.1wt%，Nb2O5:0.1~0.4wt%，ZnO:0~0.2wt%，然后将它们与BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，采用湿法球磨使其混合均匀，介质为去离子水；
f.造粒，成型，烧成，烧成后的陶瓷片通过磨片处理，再涂覆电极。
作为优选，造粒：将混合物料烘干后加入浓度为5w%聚乙烯醇溶液，混合均匀后喷雾造粒过60目筛；
作为优选，成型：采用干压成型，利用半自动压片机压制为圆片；
作为优选，烧成：在室温到1100℃按5℃/min，1100~最高温度按2℃/min，烧成最高温度1280-1300℃，保温2~3h；
作为优选，磨片处理的陶瓷片的磨成厚度为3.00mm，涂覆电极是在产品上下表面用丝网印刷低温欧姆银浆，烘干后，再升温至520℃，保温5min，随炉冷却。
本发明有益效果：该高性能钛酸锶钡陶瓷电容器材料：钛酸锶、锆酸钙中Ca2+、Sr2+、Zr4+使BST陶瓷材料在室温范围内实现介电特性；而Y3+、Ce3+、Nb5+、Zn2+多元协同掺杂使材料表现出高介低损耗高耐压特性。本发明的创新点在于采用多元掺杂和协同补偿，达到实现BST陶瓷电容器的高介低损耗高耐压特性。同时使我们能灵活设计出厂家提供的电容器件，方便快捷，节约成本。
附图说明
图1为介电特性与耐压示意图。
具体实施方式
下面结合实例对本发明的进一步阐述，但本发明不局限于这些实例。
以下各个实例所需原料均为分析纯原料。
实施例1:
以BaCO3、CaCO3、Bi2O3、、ZrO2、TiO2为主要原料，预先合成钛酸锶与钛酸钡等基料。
（1）以1molBi2O3、3molTiO2为标准比例，湿法球磨使其混合均匀，压滤后800℃保温2h，得到Bi2O3·3TiO2；分析纯BaCO3、SrCO3分别和TiO2按照物质的量1:1比例混合均匀，湿法球磨使其混合均匀，压滤后1180℃保温2.5h等工艺制备BaTiO3和SrTiO3；分析纯CaCO3与ZrO2按照等物质的量混合均匀，在电炉内1250℃保温2h冷却得到CaZrO3。
（2）然后根据生产设计需求制备BST陶瓷材料，（1-z）[（Ba1-x-ySrxCay）Ti1-yZryO3]·z(Bi2O3·3TiO2)，其中x=0.35，y=0.1，z=0.04，加入上述BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2。计总重量。
（3）按照上述预先称得重量，按质量比加入Ce2O30.25wt%，Y2O3:0wt%，Nb2O5:0.25wt%，ZnO:0.08wt%，然后将它们与BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，采用湿法球磨使其混合均匀，介质为去离子水。
（4）造粒：将混合物料烘干后加入浓度为5w%聚乙烯醇溶液，混合均匀后喷雾造粒过60目筛。
（5）成型：采用干压成型，利用半自动压片机压制为圆片。
（6）烧成是在室温到1100℃按5℃/min，1100~最高温度按2℃/min，烧成最高温度1280℃，保温2h。
（7）烧成后的陶瓷片通过磨片处理，再涂覆电极。陶瓷片的磨成厚度为3.00mm，电极涂覆是在产品上下表面用丝网印刷低温欧姆银浆，烘干后，再升温至520℃，保温5min，随炉冷却。
将所制得的陶瓷片进行介电特性和耐压测试，如图1。
实施例2：
以BaCO3、CaCO3、Bi2O3、、ZrO2、TiO2为主要原料，预先合成钛酸锶与钛酸钡等基料。
（1）以1molBi2O3、3molTiO2为标准比例，湿法球磨使其混合均匀，压滤后850℃保温2~3h，得到Bi2O3·3TiO2；分析纯BaCO3、SrCO3分别和TiO2按照物质的量1:1比例混合均匀，湿法球磨使其混合均匀，压滤后1200℃保温2h等工艺制备BaTiO3和SrTiO3；分析纯CaCO3与ZrO2按照等物质的量混合均匀，在电炉内1250℃保温2h冷却得到CaZrO3。
（2）然后根据生产设计需求制备BST陶瓷材料，（1-z）[（Ba1-x-ySrxCay）Ti1-yZryO3]·z(Bi2O3·3TiO2)，其中x=0.35，y=0.1，z=0.035，加入上述BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2。计总重量。
（3）按照上述预先称得重量，按质量比加入Ce2O3:0.36wt%，Y2O3:0.01wt%，Nb2O5:0.20wt%，ZnO:0.01wt%，然后将它们与BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，采用湿法球磨使其混合均匀，介质为去离子水。
（4）造粒：将混合物料烘干后加入浓度为5w%聚乙烯醇溶液，混合均匀后喷雾造粒过60目筛。
（5）成型：采用干压成型，利用半自动压片机压制为圆片。
（6）烧成是在室温到1100℃按5℃/min，1100~最高温度按2℃/min，烧成最高温度1290℃，保温2.5h。
（7）烧成后的陶瓷片通过磨片处理，再涂覆电极。陶瓷片的磨成厚度为3.00mm，电极涂覆是在产品上下表面用丝网印刷低温欧姆银浆，烘干后，再升温至520℃，保温5min，随炉冷却。
将所制得的陶瓷片进行介电特性和耐压测试，如图1。
实施例3：
以BaCO3、CaCO3、Bi2O3、、ZrO2、TiO2为主要原料，预先合成钛酸锶与钛酸钡等基料。
（1）以1molBi2O3、3molTiO2为标准比例，湿法球磨使其混合均匀，压滤后850℃保温2h，得到Bi2O3·3TiO2；分析纯BaCO3、SrCO3分别和TiO2按照物质的量1:1比例混合均匀，湿法球磨使其混合均匀，压滤后1200℃保温2h等工艺制备BaTiO3和SrTiO3；分析纯CaCO3与ZrO2按照等物质的量混合均匀，在电炉内1250℃保温2h冷却得到CaZrO3。
（2）然后根据生产设计需求制备BST陶瓷材料，（1-z）[（Ba1-x-ySrxCay）Ti1-yZryO3]·z(Bi2O3·3TiO2)，其中x=0.3，y=0.12，z=0.04，加入上述BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2。计总重量。
（3）按照上述预先称得重量，按质量比加入Ce2O3:0.2wt%，Y2O3:0.01wt%，Nb2O5:0.4wt%，ZnO:0.01wt%，然后将它们与BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，采用湿法球磨使其混合均匀，介质为去离子水。
（4）造粒：将混合物料烘干后加入浓度为5w%聚乙烯醇溶液，混合均匀后喷雾造粒过60目筛。
（5）成型：采用干压成型，利用半自动压片机压制为圆片。
（6）烧成是在室温到1100℃按5℃/min，1100~最高温度按2℃/min，烧成最高温度1290℃，保温2.5h。
（7）烧成后的陶瓷片通过磨片处理，再涂覆电极。陶瓷片的磨成厚度为3.00mm，电极涂覆是在产品上下表面用丝网印刷低温欧姆银浆，烘干后，再升温至520℃，保温5min，随炉冷却。
将所制得的陶瓷片进行介电特性和耐压测试，如图1。

Claims (5)

1.一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于包括以下步骤：
a.制备Bi2O3·3TiO2：以1molBi2O3、3molTiO2为标准比例，湿法球磨使其混合均匀，压滤后800~850℃保温2~3h，得到Bi2O3·3TiO2；
b．制备BaTiO3和SrTiO3：分析纯BaCO3、SrCO3分别和TiO2按照物质的量1:1比例混合均匀，湿法球磨使其混合均匀，压滤后1180~1200℃保温2~3h，制备BaTiO3和SrTiO3；
c．制备CaZrO3：分析纯CaCO3与ZrO2按照等物质的量混合均匀，在电炉内1250℃保温2h冷却得到CaZrO3；
d．根据生产设计需求制备BST陶瓷材料，（1-z）[（Ba1-x-ySrxCay）Ti1-yZryO3]·z(Bi2O3·3TiO2)，0.3≤x≤0.4，0<y<0.15，0.02<z≤0.04，加入上述BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，计总重量；
e．按质量比加入Ce2O3:0~0.5wt%，Y2O3:0~0.1wt%，Nb2O5:0.1~0.4wt%，ZnO:0~0.2wt%，然后将它们与BaTiO3、SrTiO3、CaZrO3和Bi2O3·3TiO2，采用湿法球磨使其混合均匀，介质为去离子水；
f.造粒，成型，烧成，烧成后的陶瓷片通过磨片处理，再涂覆电极。
2.根据权利要求1所述的一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于造粒：将混合物料烘干后加入浓度为5w%聚乙烯醇溶液，混合均匀后喷雾造粒过60目筛。
3.根据权利要求1所述的一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于成型：采用干压成型，利用半自动压片机压制为圆片。
4.根据权利要求1所述的一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于烧成：在室温到1100℃按5℃/min，1100~最高温度按2℃/min，烧成最高温度1280-1300℃，保温2~3h。
5.根据权利要求1所述的一种制备多元协同掺杂钛酸锶钡制备高性能陶瓷电容器材料的方法，其特征在于磨片处理的陶瓷片的磨成厚度为3.00mm，涂覆电极是在产品上下表面用丝网印刷低温欧姆银浆，烘干后，再升温至520℃，保温5min，随炉冷却。
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