CN105967721A - 一种Bi2SiO5多孔材料的制备方法 - Google Patents
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Abstract
本发明公开了一种Bi2SiO5多孔材料的制备方法，以硝酸铋和正硅酸乙酯为原料，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Bi2SiO5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Bi2SiO5多孔材料的制备方法。
背景技术
目前在Bi2O3-SiO2系统中发现和研究的化合物晶相主要包括有Bi2SiO5晶体、Bi4Si3O12晶体和Bi12SiO20晶体各相,其中前一种为亚稳化合物，后两种为稳定化合物。亚稳相Bi2SiO5不仅具有介电、热电以及非线性光学等性质,其非中心对称的晶体结构还使其有可能具有铁电性质。多孔材料以其特殊的结构特点，在克服了纳米粉体团聚的问题的同时，使材料本身具有更优越的性能。目前制备多孔材料的方法主要是利用水热法、溶胶-凝胶法、沉淀法等合成粉体后，再利用发泡剂、粘结剂等与粉体进行复配，经成形后制备出多孔块体材料，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Bi2SiO5多孔材料制备方法。
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Bi2SiO5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Bi2SiO5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1/3的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B；
(2)将分散剂加入溶液B中，再加入无水乙醇搅拌溶解，在不断搅拌下将溶液A加入其中，之后调节pH值至8～10获得溶胶C；
(3)将溶胶C于80～85℃下水浴1.5～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到Bi2SiO5多孔材料。
所述步骤(1)中，氨水的量以能溶解柠檬酸为准。
所述步骤(1)中，正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(2:1)～(1:2)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(1～1.5)。
所述步骤(2)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。
所述分散剂加入溶液B后，分散剂各组份的浓度范围均为0～0.5mol/L。
所述步骤(2)中，无水乙醇的体积是氨水体积的1/2～1。
所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为600℃～700℃。
与现有技术相比，本发明的有益效果是：本发明提供的Bi2SiO5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，使硅离子和铋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Bi2SiO5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Bi2SiO5多孔材料晶相纯，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Bi2SiO5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1/3的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝2:1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1。
(2)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。)加入溶液B中，分散剂各组份的浓度控制在0.5mol/L，加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的1/2)，在不断搅拌下将溶液A加入其中，之后调节pH值至8～10即获得溶胶C。
(3)将溶胶C于80℃下水浴1.5～3h至凝胶化。再在140℃下干燥形成干凝胶，室温下自然晾干后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粉体中进行埋烧即获得Bi2SiO5多孔材料，热处理温度为700℃。所得Bi2SiO5多孔材料中颗粒尺寸约为100nm～400nm，间隙尺寸为80nm～150nm。
实施例2
一种Bi2SiO5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1/3的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝1:2，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1.5。
(2)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。)加入溶液B中，分散剂各组份的浓度控制在0.5mol/L，加入无水乙醇搅拌溶解(无水乙醇的体积与氨水体积相等)，在不断搅拌下将溶液A加入其中，之后调节pH值至8～10即获得溶胶C。
(3)将溶胶C于85℃下水浴1.5～3h至凝胶化。再在160℃下干燥形成干凝胶，室温下自然晾干后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粉体中进行埋烧即获得Bi2SiO5多孔材料，热处理温度为600℃。所得Bi2SiO5多孔材料中颗粒尺寸约为100nm～400nm，间隙尺寸为80nm～150nm。
实施例3
一种Bi2SiO5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1/3的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝1:1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1.2。
(2)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)加入溶液B中，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.5、0.5mol/L，加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的1/2)，在不断搅拌下将溶液A加入其中，之后调节pH值至8～10即获得溶胶C。
(3)将溶胶C于85℃下水浴1.5～3h至凝胶化。再在150℃下干燥形成干凝胶，室温下自然晾干后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粉体中进行埋烧即获得Bi2SiO5多孔材料，热处理温度为650℃。所得Bi2SiO5多孔材料中颗粒尺寸约为100nm～400nm，间隙尺寸为80nm～150nm。
Claims (7)
1.一种Bi2SiO5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1/3的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B；
(2)将分散剂加入溶液B中，再加入无水乙醇搅拌溶解，在不断搅拌下将溶液A加入其中，之后调节pH值至8～10获得溶胶C；
(3)将溶胶C于80～85℃下水浴1.5～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到Bi2SiO5多孔材料。
2.根据权利要求1所述Bi2SiO5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Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(1)中，正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(2:1)～(1:2)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(1～1.5)。
4.根据权利要求1所述Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(2)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。
5.根据权利要求4所述Bi2SiO5多孔材料的制备方法，其特征在于，所述分散剂加入溶液B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4所述Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(2)中，无水乙醇的体积是氨水体积的1/2～1。
7.根据权利要求1所述Bi2SiO5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粉体中进行埋烧，温度为600℃～700℃。
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