CN105967746A - 一种多孔Bi2SiO5块材的制备方法 - Google Patents

一种多孔Bi2SiO5块材的制备方法 Download PDF

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CN105967746A
CN105967746A CN201610292683.1A CN201610292683A CN105967746A CN 105967746 A CN105967746 A CN 105967746A CN 201610292683 A CN201610292683 A CN 201610292683A CN 105967746 A CN105967746 A CN 105967746A
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伍媛婷
栗梦龙
鲁建
王莉丽
高辉
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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Bi2SiO5块材的制备方法,利用多种分散剂的复配,使硅离子和铋离子与有机物形成络合大分子结构,各物质均匀地存在于干凝胶中,结合合理的复配浓度,使干凝胶具有合适的粘度,将干凝胶直接压制成型后,经热处理即可获得多孔Bi2SiO5块材;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Bi2SiO5块材的制备方法
技术领域
本发明属于材料技术领域,特别涉及一种多孔Bi2SiO5块材的制备方法。
背景技术
Bi2SiO5是Bi2O3-SiO2二元系统中的一个亚稳定的化合物,其主要具有介电、热电以及非线性光学等性质。正因为Bi2SiO5为亚稳相物质,其结晶温度与Bi12SiO20稳定晶相的结晶温度点较接近,且其结晶过程中还存在中间相Bi2O3的影响,因此合成纯相Bi2SiO5较为困难。目前制备多孔材料的方法主要是利用湿法(如水热法、溶胶-凝胶法等)合成粉体材料后,再在粉体中混入复配的有机物(如发泡剂),经制成形、热处理后获得多孔块体材料。这种方法不仅周期长,所得多孔材料中的孔隙分布也不够均匀,针对这个问题,本专利提出了一种周期短、工艺简单而成本低的一步制备法。应用这种方法,不仅大大缩短了制备周期,而且可使铋离子和硅离子均匀存在于体系中以利于获得纯相Bi2SiO5
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Bi2SiO5块材的制备方法,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Bi2SiO5块材的制备方法,包括如下步骤:
(1)将分散剂溶于无水乙醇中搅拌溶解得到溶液A;
(2)量取1/3的溶液A,将正硅酸乙酯溶于其中形成溶液B;将硝酸铋溶于剩余溶液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2~5h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多孔Bi2SiO5块材。
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0~0.5mol/L。
所述正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(1:2)~(3:1),且Si离子与Bi离子之和与柠檬酸的摩尔比为1:(0.6~1.0)。
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:本发明提供的多孔Bi2SiO5块材的制备方法中,既不含有造粒及陈腐的过程,也不存在预结晶的过程,不需要在造粒和压片时加入额外的发泡剂等物质,是利用湿法过程直接将分散剂(如乙二胺四乙酸、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)与反应物形成大分子络合结构,通过控制各物质的浓度,特别是各分散剂的用量,干燥后的粉体具有一定的粘度,可进行直接压制成型。此制备方法不仅制备工艺过程少、设备简单,而且结合了湿法过程,使铋离子和硅离子可以均匀地存在于络合大分子中,从而完成均匀的结晶过程,微孔的形成过程是均匀的,因此所得多孔Bi2SiO5块材的孔隙尺寸及分布可控性较好。
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Bi2SiO5块材的制备方法,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0.5mol/L。
(2)量取1/3的溶液A,将正硅酸乙酯溶于其中形成溶液B备用;将硝酸铋溶于剩余溶液A中形成溶液C,其中,Si:Bi(摩尔比)=1:2,Si离子与Bi离子之和:柠檬酸(摩尔比)=1:0.6。
(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2~5h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多孔Bi2SiO5块材,热处理温度为600℃。所得多孔Bi2SiO5块材中为开孔结构,晶粒尺寸约为50nm~260nm,间隙尺寸为50nm~150nm。
实施例2
一种多孔Bi2SiO5块材的制备方法,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0.5mol/L。
(2)量取1/3的溶液A,将正硅酸乙酯溶于其中形成溶液B备用;将硝酸铋溶于剩余溶液A中形成溶液C,其中,Si:Bi(摩尔比)=3:1的比例,Si离子与Bi离子之和:柠檬酸(摩尔比)=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85℃下水浴2~5h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多孔Bi2SiO5块材,热处理温度为700℃。所得多孔Bi2SiO5块材中为开孔结构,晶粒尺寸约为50nm~260nm,间隙尺寸为50nm~150nm。
实施例3
一种多孔Bi2SiO5块材的制备方法,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、0.1、0.5、0.5、0.5mol/L。
(2)量取1/3的溶液A,将正硅酸乙酯溶于其中形成溶液B备用;将硝酸铋溶于剩余溶液A中形成溶液C,其中,Si:Bi(摩尔比)=1:1的比例,Si离子与Bi离子之和:柠檬酸(摩尔比)=1:0.8。
(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2~5h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多孔Bi2SiO5块材,热处理温度为700℃。所得多孔Bi2SiO5块材中为开孔结构,晶粒尺寸约为50nm~260nm,间隙尺寸为50nm~150nm。

Claims (5)

1.一种多孔Bi2SiO5块材的制备方法,其特征在于,包括如下步骤:
(1)将分散剂溶于无水乙醇中搅拌溶解得到溶液A;
(2)量取1/3的溶液A,将正硅酸乙酯溶于其中形成溶液B;将硝酸铋溶于剩余溶液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2~5h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多孔Bi2SiO5块材。
2.根据权利要求1所述多孔Bi2SiO5块材的制备方法,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Bi2SiO5块材的制备方法,其特征在于,所述溶液A中,分散剂各组份的浓度范围均为0~0.5mol/L。
4.根据权利要求2所述多孔Bi2SiO5块材的制备方法,其特征在于,所述正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(1:2)~(3:1),且Si离子与Bi离子之和与柠檬酸的摩尔比为1:(0.6~1.0)。
5.根据权利要求1所述多孔Bi2SiO5块材的制备方法,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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