CN105948815A - 一种多孔BaTiO3陶瓷的制备方法 - Google Patents

一种多孔BaTiO3陶瓷的制备方法 Download PDF

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CN105948815A
CN105948815A CN201610292843.2A CN201610292843A CN105948815A CN 105948815 A CN105948815 A CN 105948815A CN 201610292843 A CN201610292843 A CN 201610292843A CN 105948815 A CN105948815 A CN 105948815A
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伍媛婷
栗梦龙
王秀峰
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Shaanxi University of Science and Technology
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Abstract

本发明公开了一种多孔BaTiO3陶瓷的制备方法，以钛酸丁酯和硝酸钡为原料，无水乙醇和去离子水为溶剂，利用乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等作为分散剂合成出干凝胶粉体，再将此干凝胶粉体直接进行干压成型，形成块体材料，经热处理即可获得多孔BaTiO3陶瓷；该方法工艺简单、周期短、设备简单、成本低、所得多孔材料的孔隙尺寸及分布可控性高。

Description

一种多孔BaTiO3陶瓷的制备方法
技术领域
本发明属于材料技术领域，特别涉及一种多孔BaTiO3陶瓷的制备方法。
背景技术
钛酸钡(BaTiO3)属于典型的钙钛矿(ABO3)结构，具有优良的介电和压电性能，在压电器件、湿敏传感器和气敏传感器等多种电子元器件中具有广泛的应用。作为湿敏传感器件、气敏传感器件等敏感器件的材料，有效拉高材料与被检测介质的接触面积，可有效提高其灵敏度。如果使用纳米粉体材料，虽然纳米粉体材料具有大量的断键，比表面积大，可使接触面积增大，但也正是由于表面活性较高，颗粒间易团聚，反而降低了比表面积，这不利于敏感性材料的应用。多孔钛酸钡陶瓷材料，不仅利用细小的孔隙使材料本身保持了较高的比表面积，而且利用块体材料的优势，解决了粉体材料团聚的问题。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种多孔BaTiO3陶瓷的制备方法，具有生产工艺简单、设备要求简单、周期短的特点。
为了实现上述目的，本发明采用的技术方案是：
一种多孔BaTiO3陶瓷的制备方法，包括如下步骤：
(1)将分散剂溶于无水乙醇中得到溶液A；
(2)量取1/2的溶液A，将硝酸钡溶于其中形成溶液B备用；将钛酸丁酯溶于剩余溶液A中形成溶液C；
(3)将溶液B和溶液C混合，搅拌均匀后形成前驱体溶液，将前驱体溶液于80～85℃下水浴4～6h至凝胶化，再在140～160℃下干燥形成干凝胶，在200℃～250℃烘1～2h后，自然冷却，进行研磨过筛得到干凝胶粉体；
(4)将干凝胶粉体直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到多孔BaTiO3陶瓷。
所述步骤(1)中，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
所述溶液A中，分散剂各组份的浓度范围均为0～1.5mol/L。
所述硝酸钡和钛酸丁酯的用量满足Ba与Ti的摩尔比为1:1，且Ba离子与Ti离子之和与柠檬酸的摩尔比为1：(1.1～2.0)。
所述步骤(4)中，所述热处理是在ZnO粉体中700℃埋烧1h，之后再在1000～1400℃下烧结1～3h。
与现有技术相比，本发明的有益效果是：本发明提供的多孔BaTiO3陶瓷的制备方法中，以乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等作为分散剂直接进行络合发泡的凝胶化过程，通过控制各物质的浓度，特别是各分散剂的用量，配制出适合直接成型的干凝胶，这不仅可以减少造粒、陈腐的过程，还可使结晶过程与烧结一步完成。结合埋烧的热处理过程，利用有机物的发泡和分解燃烧过程形成多孔BaTiO3陶瓷。这种方法工艺步骤少、制备周期短、设备简单、成本低，且所得多孔BaTiO3陶瓷的孔隙尺寸及分布可控性好。
具体实施方式
下面结合实施例详细说明本发明的实施方式。
实施例1
一种多孔BaTiO3陶瓷的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成，其中聚乙二醇又包括聚乙二醇400、聚乙二醇4000和聚乙二醇6000)加入其中，搅拌溶解形成溶液A，分散剂各组份的浓度控制在1.5mol/L。
(2)量取1/2的溶液A，将醋酸钡溶于其中形成溶液B，将钛酸丁酯溶于剩余溶液A中形成溶液C，其中，Ba与Ti的摩尔比为1:1，(Ba离子+Ti离子)：柠檬酸(摩尔比)＝1：1.1。
(3)将溶液B和溶液C混合，搅拌均匀后形成前驱体溶液，将前驱体溶液于80℃下水浴4～6h至凝胶化，再在140℃下干燥形成干凝胶，在200℃烘1～2h后，自然冷却，将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中700℃进行埋烧1h，之后再在1400℃下烧结1h即获得多孔BaTiO3陶瓷。所得多孔BaTiO3陶瓷中为开孔结构，晶粒尺寸约为200nm～500nm，间隙尺寸为100nm～300nm。
实施例2
一种多孔BaTiO3陶瓷的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成)加入其中，搅拌溶解形成溶液A，分散剂各组份的浓度控制在1.5mol/L。
(2)量取1/2的溶液A，将醋酸钡溶于其中形成溶液B，将钛酸丁酯溶于剩余溶液A中形成溶液C，其中，Ba与Ti的摩尔比为1:1，(Ba离子+Ti离子)：柠檬酸(摩尔比)＝1：2。
(3)将溶液B和溶液C混合，搅拌均匀后形成前驱体溶液，将前驱体溶液于85℃下水浴4～6h至凝胶化，再在160℃下干燥形成干凝胶，在250℃烘1～2h后，自然冷却，将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中700℃进行埋烧1h，之后再在1000℃下烧结3h即获得多孔BaTiO3陶瓷。所得多孔BaTiO3陶瓷中为开孔结构，晶粒尺寸约为200nm～500nm，间隙尺寸为100nm～300nm。
实施例3
一种多孔BaTiO3陶瓷的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成)加入其中，搅拌溶解形成溶液A，分散剂各组份的浓度控制在0.01、0.1、0.7、1.0、1.2、1.5mol/L。
(2)量取1/2的溶液A，将醋酸钡溶于其中形成溶液B，将钛酸丁酯溶于剩余溶液A中形成溶液C，其中，Ba与Ti的摩尔比为1:1，(Ba离子+Ti离子)：柠檬酸(摩尔比)＝1：1.5。
(3)将溶液B和溶液C混合，搅拌均匀后形成前驱体溶液，将前驱体溶液于80℃水浴4～6h至凝胶化，再在150℃下干燥形成干凝胶，在220℃烘1～2h后，自然冷却，将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中700℃进行埋烧1h，之后再在1200℃下烧结2h即获得多孔BaTiO3陶瓷。所得多孔BaTiO3陶瓷中为开孔结构，晶粒尺寸约为200nm～500nm，间隙尺寸为100nm～300nm。

Claims (5)

1.一种多孔BaTiO3陶瓷的制备方法，其特征在于，包括如下步骤：
(1)将分散剂溶于无水乙醇中得到溶液A；
(2)量取1/2的溶液A，将硝酸钡溶于其中形成溶液B备用；将钛酸丁酯溶于剩余溶液A中形成溶液C；
(3)将溶液B和溶液C混合，搅拌均匀后形成前驱体溶液，将前驱体溶液于80～85℃下水浴4～6h至凝胶化，再在140～160℃下干燥形成干凝胶，在200℃～250℃烘1～2h后，自然冷却，进行研磨过筛得到干凝胶粉体；
(4)将干凝胶粉体直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到多孔BaTiO3陶瓷。
2.根据权利要求1所述多孔BaTiO3陶瓷的制备方法，其特征在于，所述步骤(1)中，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
3.根据权利要求2所述多孔BaTiO3陶瓷的制备方法，其特征在于，所述溶液A中，分散剂各组份的浓度范围均为0～1.5mol/L。
4.根据权利要求2所述多孔BaTiO3陶瓷的制备方法，其特征在于，所述硝酸钡和钛酸丁酯的用量满足Ba与Ti的摩尔比为1:1，且Ba离子与Ti离子之和与柠檬酸的摩尔比为1：(1.1～2.0)。
5.根据权利要求1所述多孔BaTiO3陶瓷的制备方法，其特征在于，所述步骤(4)中，所述热处理是在ZnO粉体中700℃埋烧1h，之后再在1000～1400℃下烧结1～3h。
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CN101100309A (zh) * 2007-06-29 2008-01-09 西北大学 钛酸钡纳米粉体及其陶瓷的制备方法
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CN101041587A (zh) * 2007-03-29 2007-09-26 贵州大学 一种钛酸钡电子功能陶瓷及其制备方法
CN101100309A (zh) * 2007-06-29 2008-01-09 西北大学 钛酸钡纳米粉体及其陶瓷的制备方法
CN101633520A (zh) * 2009-08-25 2010-01-27 陕西科技大学 钛酸钡纳米粉的制备方法

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