CN105967720A - 一种BaTiO3多孔材料的制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
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- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
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- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
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- 229910021529 ammonia Inorganic materials 0.000 claims 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
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- 235000011114 ammonium hydroxide Nutrition 0.000 description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 11
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- 229910052719 titanium Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种BaTiO3多孔材料的制备方法，以钛酸丁酯和硝酸钡为原料，无水乙醇和去离子水为溶剂，利用分散剂使离子均匀存在于干凝胶粉体中，经直接压制成型和热处理，即可获得BaTiO3多孔材料；这方法不仅利用了络合作用使复合更均匀，还有效缩短制备周期，具有工艺设备简单和成本低的优点。
Description
技术领域
本发明属于材料技术领域，特别涉及一种BaTiO3多孔材料的制备方法。
背景技术
BaTiO3是一种重要的铁电材料，其具有较高的介电常数，在小体积、大容量的电子器件中有着广泛的应用，BaTiO3多孔材料以其结构的优势，增大了材料的比表面积，更有利于其在电容器、光电材料等方面的应用。目前制备BaTiO3多孔材料的方法主要是利用水热法、溶胶-凝胶法、凝胶-沉淀法等合成BaTiO3粉体后，再利用发泡剂等与BaTiO3粉体进行复配，经成形后制备出BaTiO3多孔块体材料，这些方法的制备周期长且复杂，本专利即针对目前制备BaTiO3多孔材料制备方法的弊端，发明了一种制备周期短而有效的制备方法。
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BaTiO3多孔材料的制备方法，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BaTiO3多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中得到柠檬酸溶液，量取1/2的柠檬酸溶液，将硝酸钡溶于其中形成溶液A备用；将钛酸丁酯溶于剩余柠檬酸溶液中形成溶液B；
(2)将溶液A和溶液B混合，搅拌均匀后加入分散剂，再加入无水乙醇搅拌溶解，之后调节pH值至7～10获得溶胶C；
(3)将溶胶C于80～85℃下水浴4～5h至凝胶化，再在140～160℃下干燥形成干凝胶，在200℃～250℃烘1h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BaTiO3多孔材料。
所述步骤(1)中，氨水的量以能溶解柠檬酸为准。
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：(0.5～1)。
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和溶液B中加入分散剂后，分散剂各组份的浓度范围均为0～0.5mol/L。
所述无水乙醇的体积是氨水体积的2～3倍。
所述步骤(4)中，所述热处理是在ZnO粉体中700℃埋烧1h，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BaTiO3多孔材料的制备方法中，合理利用乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇400、聚乙二醇4000、聚乙二醇6000等作为分散剂，使钡离子和钛离子均匀分布于凝胶中，控制分散剂的各类和用量，使干凝胶呈现一定粘性的粉末状，使干凝胶可用于直接压制成型，结合埋烧和适当的热处理制度，利用有机物的发泡和分解燃烧过程形成BaTiO3多孔材料。这种方法可以减少造粒、陈腐等制备工艺过程，使工艺步骤少、制备周期缩短，所利用有机物的络合和分散效应，使BaTiO3多孔材料中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BaTiO3多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将硝酸钡溶于其中形成溶液A备用；将钛酸丁酯溶于剩余柠檬酸溶液中形成溶液B，其中，Ba：Ti(摩尔比)符合化学计量比1:1，且Ba离子与Ti离子之和与柠檬酸的摩尔比为＝1：0.5。
(2)混合溶液A和溶液B，搅拌均匀后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，分散剂各组份的浓度控制在0.5mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的2倍)，调节pH值至7～10即获得溶胶C。
(3)将溶胶C于80℃下水浴4～5h至凝胶化。再在140℃下干燥形成干凝胶，在200℃烘1h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1～3h即获得BaTiO3多孔材料。所得BaTiO3多孔材料中为开孔结构，晶粒尺寸约为100nm～300nm，间隙尺寸为50nm～200nm。
实施例2
一种BaTiO3多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将硝酸钡溶于其中形成溶液A备用；将钛酸丁酯溶于剩余柠檬酸溶液中形成溶液B，其中，Ba：Ti(摩尔比)符合化学计量比1:1，且Ba离子与Ti离子之和与柠檬酸的摩尔比为＝1：1。
(2)混合溶液A和溶液B，搅拌均匀后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，分散剂各组份的浓度控制在0.5mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的3倍)，调节pH值至7～10即获得溶胶C。
(3)将溶胶C于80℃下水浴4～5h至凝胶化。再在140℃下干燥形成干凝胶，在250℃烘1h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1～3h即获得BaTiO3多孔材料。所得BaTiO3多孔材料中为开孔结构，晶粒尺寸约为100nm～300nm，间隙尺寸为50nm～200nm。
实施例3
一种BaTiO3多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将硝酸钡溶于其中形成溶液A备用；将钛酸丁酯溶于剩余柠檬酸溶液中形成溶液B，其中，Ba：Ti(摩尔比)符合化学计量比1:1，且Ba离子与Ti离子之和与柠檬酸的摩尔比为＝1：0.8。
(2)混合溶液A和溶液B，搅拌均匀后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，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.7、0.8mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的3倍)，调节pH值至7～10即获得溶胶C。
(3)将溶胶C于85℃下水浴4～5h至凝胶化。再在150℃下干燥形成干凝胶，在250℃烘1h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1～3h即获得BaTiO3多孔材料。所得BaTiO3多孔材料中为开孔结构，晶粒尺寸约为100nm～300nm，间隙尺寸为50nm～200nm。
Claims (7)
1.一种BaTiO3多孔材料的制备方法，其特征在于，包括如下步骤：
(1)将柠檬酸溶于氨水中得到柠檬酸溶液，量取1/2的柠檬酸溶液，将硝酸钡溶于其中形成溶液A备用；将钛酸丁酯溶于剩余柠檬酸溶液中形成溶液B；
(2)将溶液A和溶液B混合，搅拌均匀后加入分散剂，再加入无水乙醇搅拌溶解，之后调节pH值至7～10获得溶胶C；
(3)将溶胶C于80～85℃下水浴4～5h至凝胶化，再在140～160℃下干燥形成干凝胶，在200℃～250℃烘1h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BaTiO3多孔材料。
2.根据权利要求1所述BaTiO3多孔材料的制备方法，其特征在于，所述步骤(1)中，氨水的量以能溶解柠檬酸为准。
3.根据权利要求1所述BaTiO3多孔材料的制备方法，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：(0.5～1)。
4.根据权利要求1所述BaTiO3多孔材料的制备方法，其特征在于，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。
5.根据权利要求4所述BaTiO3多孔材料的制备方法，其特征在于，所述溶液A和溶液B中加入分散剂后，分散剂各组份的浓度范围均为0～0.5mol/L。
6.根据权利要求1所述BaTiO3多孔材料的制备方法，其特征在于，所述无水乙醇的体积是氨水体积的2～3倍。
7.根据权利要求1所述BaTiO3多孔材料的制备方法，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，再在1000℃～1400℃下烧结1～3h。
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