CN106894044B - 一种azo镀膜液的电化学制备方法、一种azo导电玻璃及其制备方法 - Google Patents
一种azo镀膜液的电化学制备方法、一种azo导电玻璃及其制备方法 Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 27
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 21
- 239000011701 zinc Substances 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
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- UUZYBYIOAZTMGC-UHFFFAOYSA-M benzyl(trimethyl)azanium;bromide Chemical compound [Br-].C[N+](C)(C)CC1=CC=CC=C1 UUZYBYIOAZTMGC-UHFFFAOYSA-M 0.000 claims description 2
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims 1
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- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
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- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
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Abstract
本发明公开了一种AZO镀膜液的电化学制备方法、一种AZO导电玻璃及其制备方法,与现有技术相比,本发明提供了一种AZO镀膜液的电化学制备方法,该方法直接使用纯金属锌、铝和电能作为原材料,成本低,工艺简单,而且减少环境污染,提高产品性能。
Description
技术领域
本发明属于导电玻璃镀膜液的制备方法,具体涉及一种AZO镀膜液的电化学制备方法、一种AZO导电玻璃及其制备方法。
背景技术
TCO(Transparent conducting oxide)导电玻璃,主要包括ITO(氧化铟锡)、FTO(氟掺杂氧化锡)、AZO(铝掺杂氧化锌)等。其中,掺杂ZnO薄膜以其优良的性能吸引了人们的研究兴趣。ZnO是一种具有六方纤锌矿晶体结构的Ⅱ-Ⅵ族半导体材料,具有高质量的单晶块体材料和大的室温激子束缚能(60meV),在室温下的直接光学带隙为3.37eV,大于可见光的光子能量3.10eV,因此ZnO薄膜对可见光几乎是透明的。
AZO薄膜是在ZnO中掺杂Al形成ZnO:Al薄膜,其可以有效降低薄膜的电阻率,提高薄膜的电学性能。AZO薄膜与ITO薄膜相比,具有良好的电学和光学特性,且能源丰富、价格便宜、沉积温度低、热稳定性和化学稳定性好,可以用于制备半导体和压电薄膜,也能通过掺杂制备透明导电薄膜,因此被广泛用于太阳能电池及液晶显示器件电极的制备中。
用于制备AZO薄膜的方法主要包括脉冲激光沉积法、化学喷雾沉积法、等离子体增强化学气相沉积法、射频磁控溅射法、真空蒸发法、溶胶凝胶法。目前AZO镀膜玻璃生产方式主要采用磁控溅射法。但是磁控溅射法容易造成靶材浪费,成本高,且操作复杂。
发明内容
本发明的目的在提供一种AZO镀膜液的电化学制备方法,直接使用纯金属锌、铝和电能作为原材料,成本低,工艺简单,而且减少环境污染,提高产品性能。
本发明还提供了一种AZO导电玻璃及其制备方法,制备的导电玻璃性能优异,具有良好的热稳定性,而且,透光性好,抗酸碱能力强。
本发明提供的一种AZO镀膜液的电化学制备方法,包括以下步骤:
1)依次用纯金属锌和纯金属铝作为阳极材料、有机导电盐的有机醇溶液为电解液、以惰性电极或不锈钢作阴极,在无隔膜电解槽中通电电解,得到锌铝醇盐溶液;
2)将去离子水加入步骤1)制备的锌铝醇盐溶液,调节pH至4-6,搅拌水解反应形成AZO镀膜液。
进一步的,步骤1)中所述电解电流为直流电,电流强度为0.1-7A/dm2;电解时间为4-16h。
步骤1)中所述有机导电盐为四丁基溴化铵、四丁基氯化铵、十六烷基三甲基溴化铵、苄基三甲基溴化铵。
步骤1)中所述有机醇为无水乙醇、丙醇,异丙醇或丁醇的一种或几种的混合溶液。
步骤1)中所述的有机导电盐,其浓度为0.2-8%。
步骤1)中所述惰性电极为铅电极、碳棒或铂电极。
步骤1)中所述通电电解时,体系温度为20-30℃。
步骤1)中得到的锌铝醇盐溶液中锌和铝的摩尔比为1:0.005-0.03。
步骤2)中加入去离子水后,锌铝醇盐的浓度为0.2-0.6mol/L。
步骤2)中搅拌水解形成溶胶在20-40℃温度下进行。
步骤2)中搅拌水解时间6-24h。
步骤2)中调节pH所用的酸为甲酸、乙酸、盐酸或硝酸中的一种或几种。
一种AZO导电玻璃的制备方法,制备方法为:
将上述制备的AZO镀膜液通过旋涂、辊涂、喷涂和浸涂的方法可制备AZO导电玻璃。
一种AZO导电玻璃,采用上述方法制备得到。
与现有技术相比,本发明提供了一种AZO镀膜液的电化学制备方法,该方法直接使用用纯金属锌和纯金属铝和电能作为原材料,成本低,工艺简单,而且减少环境污染,提高产品性能。
具体实施方式
为了更好地理解本发明的内容,下面结合具体实施例作进一步说明。应理解,这些实施例仅用于对本发明进一步说明,而不用于限制本发明的范围。
实施例1
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为0.2%的四丁基溴化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,铅电极作为阴极,搅拌下以电流强度为0.1A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为0.1A/dm2直流电继续电解,共电解16h,得到锌和铝的摩尔比为1:0.005的锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌、铝醇盐的浓度为0.2mol/L,用盐酸调节pH为5,在20℃下搅拌水解24h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过辊涂的方法可制备AZO透明导电玻璃,方块电阻为15.5Ω/cm。
实施例2
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为8%的四丁基氯化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,碳棒电极作为阴极,搅拌下以电流强度为7A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为7A/dm2直流电继续电解,共电解4h,得到锌和铝的摩尔比为1:0.03的锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌铝醇盐的浓度为0.6mol/L,用盐酸调节pH为5.5,在25℃下搅拌6h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过旋涂的方法可制备AZO透明导电玻璃,方块电阻为15.8Ω/cm。
实施例3
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为0.3%的十六烷基三甲基溴化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,铂电极作为阴极,搅拌下以电流强度为0.5A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为0.5A/dm2直流电继续电解,共电解11h,得到锌和铝的摩尔比为1:0.02锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌铝醇盐的浓度为0.4mol/L,用乙酸调节pH为6,在30℃下搅拌11h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过喷涂的方法可制备AZO透明导电玻璃,方块电阻为16.5Ω/cm。
实施例4
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为1%的苄基三甲基溴化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,不锈钢作为阴极,搅拌下以电流强度为2A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为2A/dm2直流电继续电解,共电解13h,得到锌和铝的摩尔比为1:0.01锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌铝醇盐的浓度为0.5mol/L,用甲酸调节pH为4.5,在20℃下搅拌水解10h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过浸涂的方法可制备AZO透明导电玻璃,方块电阻为16.2Ω/cm。
实施例5
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为5%的苄基三甲基溴化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,铂电极作为阴极,搅拌下以电流强度为5A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为5A/dm2直流电继续电解,共电解6h,得到锌和铝的摩尔比为1:0.015的锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌铝醇盐的浓度为0.5mol/L,用乙酸调节pH为6,在25℃下搅拌水解9h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过喷涂的方法可制备AZO透明导电玻璃,方块电阻为15.9Ω/cm。
实施例6
一种AZO镀膜液的电化学制备方法,包括以下步骤:
(1)在容积为10升的无隔膜电解槽中加入含有质量浓度为5%的四丁基溴化铵的无水乙醇溶液8升,插入工业纯锌片作为阳极,不锈钢作为阴极,搅拌下以电流强度为5A/dm2直流电电解,然后将阳极换为工业纯铝片,搅拌下以电流强度为5A/dm2直流电继续电解,共电解8h,得到锌和铝的摩尔比为1:0.025的锌铝醇盐溶液。
(2)在上述反应器中加入适量的去离子水,使锌、铝醇盐的浓度为0.3mol/L,用硝酸调节pH为4,在30℃下搅拌水解16h得到一种透明的AZO溶胶镀膜液。
将步骤(2)得到的AZO溶胶镀膜液通过旋涂的方法可制备AZO透明导电玻璃,方块电阻为16.8Ω/cm。
Claims (10)
1.一种AZO镀膜液的电化学制备方法,其特征在于,所述制备方法包括以下步骤:
1)依次用纯金属锌和纯金属铝作为阳极材料、有机导电盐的有机醇溶液为电解液、以惰性电极或不锈钢作阴极,在无隔膜电解槽中通电电解,得到锌铝醇盐溶液;
2)将去离子水加入步骤1)制备的锌铝醇盐溶液,加酸调节pH 至4-6,搅拌水解反应形成AZO镀膜液;
步骤2)中调节pH所用的酸为甲酸、乙酸、盐酸或硝酸中的一种或几种。
2.根据权利要求1所述的制备方法,其特征在于,步骤1)中所述电解电流为直流电,电流强度为0.1-7A/dm2;电解时间为4-16h。
3.根据权利要求1或2所述的制备方法,其特征在于,步骤1)中所述有机醇为为无水乙醇、丙醇,异丙醇、丁醇的一种或几种的混合溶液。
4.根据权利要求1或2所述的制备方法,其特征在于,步骤1)中所述的有机导电盐,其质量浓度为0.2-10%。
5.根据权利要求1所述的制备方法,其特征在于,步骤1)中所述有机导电盐为四丁基溴化铵、四丁基氯化铵、十六烷基三甲基溴化铵或苄基三甲基溴化铵中的一种。
6.根据权利要求1或2所述的制备方法,其特征在于,步骤1)中得到的锌铝醇盐溶液中锌和铝的摩尔比为1:0.005-0.03。
7.根据权利要求1所述的制备方法,其特征在于,步骤2)中加入去离子水后,锌铝醇盐的浓度为0.2-0.6mol/L。
8.根据权利要求1所述的制备方法,其特征在于步骤2)中搅拌水解形成溶胶在20-40℃温度下进行。
9.一种AZO导电玻璃的制备方法,其特征在于,制备方法为:将权利要求1-8任一项所制备的AZO镀膜液通过旋涂、辊涂、喷涂或浸涂的方法可制备AZO导电玻璃。
10.一种AZO导电玻璃,采用权利要求9所述的方法制备得到。
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