CN104465321B - 一种制备光电薄膜的方法 - Google Patents
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Abstract
本发明公开了一种制备光电薄膜的方法,包括以下步骤:将物质A溶于溶剂X中制成AX溶液,物质B溶于溶剂Y中制成BY溶液,向旋转中的基片上加入AX溶液和BY溶液生成物质C制备光电薄膜,以此为一个沉淀周期,可以根据所需光电薄膜的厚度选择合适的沉淀周期。本发明方法简单,操作方便,所有操作是在不加热源情况下进行的,能耗低、绿色环保,所得光电薄膜纯净、致密、平整,适合工业化应用。
Description
技术领域
本发明属于光电薄膜制备技术领域,具体涉及一种制备光电薄膜的方法。
背景技术
物质在受到光照以后,往往会引发某些电性质的变化,亦称光电效应。光电效应主要有光电导效应、光生伏特效应和光电子发射效应3种。物质受光照射作用时,其电导率产生变化的现象,称为光电导效应。如果光照射到半导体的p-n结上,则在p-n结两端会出现电势差,p区为正极,n区为负极,这一电势差可以用高内阻的电压表测量出来,称为光生伏特效应。当金属或半导体受到光照射时,其表面和体内的电子因吸收光子能量而被激发,如果被激发的电子具有足够的能量,足以克服表面势垒而从表面离开,产生了光电子发射效应。前两种效应在物体内部发生,统称为内光电效应,它一般发生于半导体中。光电子发射效应产生于物体表面,又称为外光电效应,它主要发生于金属或半导体中。光电导薄膜材料包括:Ge和Si单晶及以它们为基础的掺杂体;化合物半导体有CdS,CdSe,CdTe,ZnSe,HgSe,HgTe,PbS,PbSe,InP,InAs,InSb,GaAs,GaSb等。
以硫化银为例来说明现有的光电薄膜的制备。硫化银是一种窄禁带宽度直接半导体,禁带宽度约为0.9eV,具有杰出的光电活性和很好的化学稳定性,在光伏技术领域具有光明的应用前景。河南师范大学的杨林等以硝酸银、牛血清白蛋白(BSA)和硫代乙酰胺(TAA)为原料。通过金属离子和生物大分子的螯合作用形成银离子的螯合物;该螯合物和硫代乙酰胺(TAA)释放的硫离子在多孔氧化铝模板中定位成核、逐渐组装成纳米线,然后分离清洗,得到蛋白质包覆的硫化银纳米线。许昌学院的郑直等利用磁控溅射技术在基片上溅射一层银单质,然后将其浸入硫的DMF饱和溶液中硫化,得到了片状的硫化银纳米晶光电薄膜。上海交通大学的黄鹏等通过制备银离子蛋白混合液;制备银-硫蛋白混合液;离心处理以及真空干燥处理,制成硫化银纳米颗粒。吉林大学的解仁国等将醋酸银与长链羧酸加入到非配位性有机溶剂中,再注入短链巯醇,升温至60℃-80℃,其中,醋酸银、长链羧酸和短链巯醇的摩尔比为1∶0.5∶5,非配位性有机溶剂的用量为每mol醋酸银使用25L;抽真空充氮气或惰性气体保护,升温至95℃~120℃,注入浓度为0.5mol/L硫的十八烯溶液,使注入的硫与醋酸银的摩尔比为1∶2;保持温度95℃~120℃反应10~20分钟,得到Ag2S量子点。中国科学院苏州纳米技术与纳米仿生研究所的王强斌等将包含银源和长链硫醇的混合反应体系于密闭环境中充分反应;将混合反应体系冷却后加入极性溶剂,经离心、洗涤得到疏水性近红外硫化银量子点;将疏水性近红外硫化银量子点与含巯基的亲水性试剂在有机溶剂中充分混合反应,反应混合物经离心、洗涤,获得生物相容性近红外硫化银量子点。由硫化银光电薄膜制备的例子可知,现有的光电薄膜制备方法大多需要较高的温度,并且操作复杂,能耗高。
发明内容
本发明的目的在于提供一种能在不加任何热源的情况下将光电材料制作成新型太阳能薄膜电池所需的致密纯净平整的光电薄膜的方法。
为实现上述目的,本发明采用如下技术方案:
一种制备光电薄膜的方法,包括以下步骤:将各种原料溶于溶剂中制成溶液,向旋转中的基片上分别加入各种原料的溶液即制的光电薄膜;所述各原料可以反应生成具有光电特性的物质,溶剂与基片具有亲和性。
较好的,制备光电薄膜的方法,具体包括以下步骤:(1)将物质A溶于溶剂X中制成AX溶液,物质B溶于溶剂Y中制成BY溶液,其中,物质A和物质B反应可以生成具有光电特性的物质C;
(2)向旋转中的基片上加入AX溶液和BY溶液生成物质C制备光电薄膜,以此为一个沉淀周期,可以根据所需光电薄膜的厚度选择合适的沉淀周期。
上述方法中,溶剂X或溶剂Y选择时要求物质C在溶剂X或溶剂Y中均为沉淀,溶剂X与溶剂Y互溶,溶剂X和溶剂Y与基片具有亲和性。
本发明中所述基片需经过预处理,预处理方法为:将基片依次用去离子水、无水乙醇、丙酮进行超声清洗,然后用氮气吹干。
本发明所得光电薄膜的厚度由沉淀周期、溶液浓度和基片转速来控制,本领域技术人员可以根据需要进行相应的操作。
为了使得到的光电薄膜效果更好,较好的,步骤(2)中向旋转的基片上依次滴加AX溶液、溶剂X、BY溶液和溶剂Y生成物质C制备光电薄膜,以此为一个周期。
本发明方法中,溶液和溶剂的滴加量一方面需要依据基片的大小来确定,另一方面需要同时保证有足够的溶液或溶剂在基片上生成光电薄膜的地方形成流动。
本发明中,物质A、物质B可以是纯物质也可以是混合物;溶剂X和溶剂Y可以是混合溶剂,也可以是同种溶剂;本领域技术人员可以根据实际需要进行选择。
较好的,本发明中所用基片为ITO、FTO或AZO等,利用匀胶机等实现基片的旋转,匀胶机的转速可以根据需要进行调节,使溶液可以在基片上均匀铺展即可。
本发明方法中的操作是在不加热源的情况下完成的,因此温度没有太大限制,只要低温不至于溶剂凝固或者溶质析出,高温可不至使溶剂挥发或者溶质分解变质即可。
本发明中具有光电性质的物质C为硫化银、硫化镉、硫化铅、三硫化二铟、三硫化二锑或者铜铟硫等光电材料。
本发明方法简单,操作方便,所有操作是在不加任何热源的情况下进行,能耗低、绿色环保,所得光电薄膜纯净、致密、平整,适合工业化应用。
附图说明
图1为实施例1中硫化银光电薄膜扫描电镜图;
图2为实施例2中硫化银光电薄膜扫描电镜图。
具体实施方式
下面结合实施例对本发明作进一步的说明,但本发明的保护范围并不仅限于此。
实施例1
(1)将ITO(氧化铟锡)基片(基片为长方形,规格为:1.5×2cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将ITO基片用氮气吹干备用;
(2)将硝酸银溶于去离子水乙醇混合液中得0.01mol /L的硝酸银去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.05mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1 ;
(3)将ITO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上硝酸银去离子水乙醇溶液2滴、去离子水与乙醇混合溶液2滴、硫化钠去离子水乙醇溶液2滴、去离子水与乙醇混合溶液2滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例2
(1)将ITO(氧化铟锡)(基片为长方形,规格为:1.5×2cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将ITO基片用氮气吹干备用;
(2)将硝酸铅溶于去离子水乙醇混合液中得0.01mol /L的硝酸铅去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.01mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将ITO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上硝酸铅去离子水乙醇溶液2滴、去离子水与乙醇混合溶液2滴、硫化钠去离子水乙醇溶液2滴、去离子水与乙醇混合溶液2滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例3
(1)将FTO基片(基片为长方形,规格为:6×8cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将FTO基底用氮气吹干备用;
(2)将氯化镉溶于去离子水乙醇混合液中得0.01mol /L的氯化镉去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.01mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将FTO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上氯化镉去离子水乙醇溶液3滴、去离子水与乙醇混合溶液2滴、硫化钠去离子水乙醇溶液3滴、去离子水与乙醇混合溶液2滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例4
(1)将AZO基片(基片为长方形,规格为:1.5×2cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将AZO基片用氮气吹干备用;
(2)将氯化铟溶于去离子水乙醇混合液中得0.01mol /L的氯化镉去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.015mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将AZO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上氯化铟去离子水乙醇溶液1滴、去离子水与乙醇混合溶液1滴、硫化钠去离子水乙醇溶液1滴、去离子水与乙醇混合溶液1滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例5
(1)将ITO(氧化铟锡)基片(基片为长方形,规格为:6×8cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将ITO基片用氮气吹干备用;
(2)将氯化铟溶于去离子水乙醇混合液中得0.01mol /L的氯化镉去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.015mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将ITO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上氯化铟去离子水乙醇溶液4滴、去离子水与乙醇混合溶液4滴、硫化钠去离子水乙醇溶液4滴、去离子水与乙醇混合溶液4滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例6
(1)将ITO(氧化铟锡)基片(基片为长方形,规格为:1.5×2cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将ITO基片用氮气吹干备用;
(2)将硝酸锌溶于去离子水乙醇混合液中得0.01mol /L的硝酸锌去离子水乙醇溶液;硫化钠溶于去离子水乙醇混合液中得0.005mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将ITO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴上硝酸锌去离子水乙醇溶液1滴、去离子水与乙醇混合溶液2滴、硫化钠去离子水乙醇溶液1滴、去离子水与乙醇混合溶液2滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
实施例7
(1)将FTO基片(基片为长方形,规格为:1.5×2cm)依次用去离子水、无水乙醇、丙酮进行超声清洗,然后将ITO基片用氮气吹干备用;
(2)将硫酸铜和氯化铟溶于去离子水乙醇混合液中得混合溶液,其中硫酸铜和氯化铟的摩尔浓度均为0.01mol /L;硫化钠溶于去离子水乙醇混合液中得0.025mol/L 的硫化钠去离子水乙醇溶液;其中去离子水乙醇混合液中乙醇和去离子水的体积比为4∶1;
(3)将ITO基片放到匀胶机上高速旋转,在高速旋转的基片上依次滴加混合溶液3滴、去离子水与乙醇混合溶液2滴、硫化钠去离子水乙醇溶液4滴、去离子水与乙醇混合溶液2滴,此为一个沉积周期。重复30个沉淀周期得光电薄膜,其中匀浆机转速为9000rpm。
对照方法:分子前驱体热解法:取0.0167g醋酸银和0.0152g硫脲共同放入一小药瓶中,然后向药瓶中注入0.6ml丁胺和0.04ml丙酸,用手摇匀后取混合液滴到放置在匀胶机上的ITO上,1500转每分钟旋转30秒,而后放到热台上250度加热15分钟即可。
对实施例1中的硫化银光电薄膜进行扫描得电镜扫描图1;对对照方法制备的硫化银光电薄膜进行扫描得电镜扫描图2;结果可知,对照方法制备的薄膜,表面粗糙,杂质含量高,光电性能差;本发明方法光电薄膜纯净、致密、平整、效果好,适合工业化生产。
Claims (3)
1.一种制备光电薄膜的方法,其特征在于,包括以下步骤:(1)将物质A溶于溶剂X中制成AX溶液,物质B溶于溶剂Y中制成BY溶液,其中,物质A和物质B反应生成具有光电特性的物质C,物质C在溶剂X或溶剂Y中均为沉淀;溶剂X与溶剂Y可以互溶;所述溶剂X和溶剂Y与基片具有亲和性;所述物质C为硫化银、硫化镉、硫化铅、三硫化二铟、三硫化二锑或者铜铟硫;
(2)向旋转的基片上依次滴加AX溶液、溶剂X、BY溶液和溶剂Y生成物质C制备光电薄膜,以此为一个沉淀周期。
2.如权利要求1所述的制备光电薄膜的方法,其特征在于,所述基片为ITO、FTO或AZO,并且利用匀胶机使基片旋转。
3.如权利要求1所述的制备光电薄膜的方法,其特征在于,所述基片需经过预处理,预处理方法为:将基片依次用去离子水、无水乙醇、丙酮进行超声清洗,然后用氮气吹干。
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