CN110252342B - 一种硫化锌-硫化铟异质结材料及其制备方法和应用 - Google Patents
一种硫化锌-硫化铟异质结材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种硫化锌‑硫化铟异质结材料及其制备方法和应用,属于无机材料技术领域,该材料按如下方法制备:将硝酸铟和ZIF‑8分别加入乙醇溶液中,然后将含硝酸铟的乙醇溶液加入含ZIF‑8的乙醇溶液中,混匀后通过溶剂热法在100‑180℃下反应1‑6h,经抽滤、洗涤、干燥后获得中间产物,最后将所述中间产物与硫粉混匀后置于管式炉中,以1‑10℃/min的速率升温至400‑600℃后保温1‑6h,即可。该材料为具有丰富界面的纳米异质结,呈纳米棒状,其尺寸仅为数十纳米,能够高效降解有机污染物。其制备工艺简单,易操作,适合扩大化生产。
Description
技术领域
本发明属于无机材料技术领域,具体涉及一种硫化锌-硫化铟异质结材料及其制备方法和应用。
背景技术
近年来,通过光催化技术降解有机污染物是目前环境领域的一项重要课题,而光催化剂的空穴(h+)和光生电子(e-)复合率较高导致催化剂量子效率低。目前,科研界用于改善光催化剂光生载流子复合率高这一问题,最常用的一种方法是形成异质结结构。然而,在实际应用的过程中发现异质结的两相总是易于脱结,从而导致异质结的稳定性、光催化活性和重复利用性不乐观。因此,构建优异的异质结在提高催化剂催化活性方面发挥着至关重要的作用。目前光催化异质结材料具有很好的应用前景,但制备具有纳米尺寸且具有稳定异质结结构的光催化异质结材料还存在困难。
发明内容
有鉴于此,本发明的目的之一在于提供一种硫化锌-硫化铟异质结材料的制备方法;目的之二在于提供一种硫化锌-硫化铟异质结材料;目的之三在于提供该硫化锌-硫化铟异质结材料在光催化降解有机污染物中的应用。
为达到上述目的,本发明提供如下技术方案:
1、一种硫化锌-硫化铟异质结材料的制备方法,所述方法如下:
将硝酸铟和ZIF-8分别加入乙醇溶液中,然后将含硝酸铟的乙醇溶液加入含ZIF-8的乙醇溶液中,混匀后通过溶剂热法在100-180℃下反应1-6h,经抽滤、洗涤、干燥后获得中间产物,最后将所述中间产物与硫粉混匀后置于管式炉中,以1-10℃/min的速率升温至400-600℃后保温1-6h,即可。
优选的,所述硝酸铟与ZIF-8的质量比为5-18:1。
优选的,所述乙醇溶液的体积分数为90%以上。
优选的,所述洗涤具体为以乙醇溶液洗涤。
优选的,所述干燥具体为在50-100℃下真空干燥6h以上。
优选的,所述中间产物与硫粉的质量比小于等于1:3。
2、由所述的方法制备的硫化锌-硫化铟异质结材料。
3、所述的硫化锌-硫化铟异质结材料在光催化降解有机污染物中的应用。
优选的,所述有机污染物为甲基橙、乙基紫、盐酸四环素或双酚A中的至少一种。
本发明的有益效果在于:本发明提供了一种硫化锌-硫化铟异质结材料及其制备方法和应用,通过本发明中的方法制备的硫化锌-硫化铟异质结材料为具有丰富界面的纳米异质结,该材料呈纳米棒状,其尺寸仅为数十纳米,能够高效降解有机污染物。该材料具有一维纳米异质结构,克服了现有技术中在合成异质结材料过程中通过聚合连接不同的材料,或由一种组分包覆另一种组分,而导致载体向光催化剂表面迁移距离长,电荷-载体分离效率低的缺陷,能够保证快速和长距离的电子输运,提高电荷分离效率,从而能够高效降解有机污染物。该材料制备工艺简单,易操作,适合扩大化生产。
本发明的其他优点、目标和特征在某种程度上将在随后的说明书中进行阐述,并且在某种程度上,基于对下文的考察研究对本领域技术人员而言将是显而易见的,或者可以从本发明的实践中得到教导。本发明的目标和其他优点可以通过下面的说明书来实现和获得。
附图说明
为了使本发明的目的、技术方案和优点更加清楚,下面将结合附图对本发明作优选的详细描述,其中:
图1为实施例1中制备的硫化锌-硫化铟异质结材料的XRD图;
图2为实施例1中制备的硫化锌-硫化铟异质结材料的FESEM图;
图3为实施例1中制备的硫化锌-硫化铟异质结材料的TEM图;
图4为实施例2中制备的硫化锌-硫化铟异质结材料的XRD图;
图5为实施例2中制备的硫化锌-硫化铟异质结材料的FESEM图;
图6为实施例2中制备的硫化锌-硫化铟异质结材料的TEM图;
图7为实施例3中制备的硫化锌-硫化铟异质结材料的XRD图;
图8为实施例3中制备的硫化锌-硫化铟异质结材料的FESEM图;
图9为实施例3中制备的硫化锌-硫化铟异质结材料的TEM图;
图10为实施例1中制备的硫化锌-硫化铟异质结材料对甲基橙的光催化降解能力测试结果图;
图11为实施例1中制备的硫化锌-硫化铟异质结材料对乙基紫的光催化降解能力测试结果图;
图12为实施例1中制备的硫化锌-硫化铟异质结材料对盐酸四环素的光催化降解能力测试结果图;
图13为实施例1中制备的硫化锌-硫化铟异质结材料对双酚A的光催化降解能力测试结果图;
图14为实施例1中制备的硫化锌-硫化铟异质结材料的光电流测试结果图;
图15为实施例2中制备的硫化锌-硫化铟异质结材料的光电流测试结果图;
图16为实施例3中制备的硫化锌-硫化铟异质结材料的光电流测试结果图。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式,本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用,本说明书中的各项细节也可以基于不同观点与应用,在没有背离本发明的精神下进行各种修饰或改变。
实施例1
制备硫化锌-硫化铟异质结材料
将1200mg硝酸铟和100mg ZIF-8分别加入20mL体积分数为99.5%的乙醇溶液中,然后将含有硝酸铟的乙醇溶液加入含有ZIF-8的乙醇溶液中,混匀后通过溶剂热法在120℃下反应6h,经抽滤后以体积分数为99.5%的乙醇溶液进行洗涤,接着在60℃下真空干燥12h后获得中间产物,最后按中间产物与硫粉的质量比为1:3,将中间产物与硫粉混匀后置于管式炉中,以2℃/min的速率升温至500℃后保温2h,制得硫化锌-硫化铟异质结材料。
图1为实施例1中制备的硫化锌-硫化铟异质结材料的XRD图,由图1可知,该硫化锌-硫化铟异质结材料的晶体结构结构有序,与标准卡片相对应。
图2实施例1中制备的硫化锌-硫化铟异质结材料的FESEM图,由图2可知,该硫化锌-硫化铟异质结材料呈纳米棒状,尺寸为数十纳米,且分散均匀。
图3实施例1中制备的硫化锌-硫化铟异质结材料的TEM图,由图3可知,该硫化锌-硫化铟异质结材料为具有丰富界面的纳米异质结。
实施例2
制备硫化锌-硫化铟异质结材料
将500mg硝酸铟和100mg ZIF-8分别加入20mL体积分数为95%的乙醇溶液中,然后将含有硝酸铟的乙醇溶液加入含有ZIF-8的乙醇溶液中,混匀后通过溶剂热法在180℃下反应1h,经抽滤后以体积分数为95%的乙醇溶液进行洗涤,接着在100℃下真空干燥6h后获得中间产物,最后按中间产物与硫粉的质量比为1:5,将中间产物与硫粉混匀后置于管式炉中,以10℃/min的速率升温至600℃后保温1h,制得硫化锌-硫化铟异质结材料。
图4为实施例2中制备的硫化锌-硫化铟异质结材料的XRD图,由图4可知,该硫化锌-硫化铟异质结材料的晶体结构结构有序,与合成的单独硫化铟和硫化锌的晶体结构相对应。
图5实施例2中制备的硫化锌-硫化铟异质结材料的FESEM图,由图5可知,该硫化锌-硫化铟异质结材料呈纳米棒状,尺寸为数十纳米,且分散均匀。
图6实施例2中制备的硫化锌-硫化铟异质结材料的TEM图,由图6可知,该硫化锌-硫化铟异质结材料为具有丰富界面的纳米异质结。
实施例3
制备硫化锌-硫化铟异质结材料
将1800mg硝酸铟和100mg ZIF-8分别加入20mL体积分数为98%的乙醇溶液中,然后将含有硝酸铟的乙醇溶液加入含有ZIF-8的乙醇溶液中,混匀后通过溶剂热法在100℃下反应3h,经抽滤后以体积分数为98%的乙醇溶液进行洗涤,接着在50℃下真空干燥15h后获得中间产物,最后按中间产物与硫粉的质量比为1:10,将中间产物与硫粉混匀后置于管式炉中,以5℃/min的速率升温至400℃后保温6h,制得硫化锌-硫化铟异质结材料。
图7为实施例3中制备的硫化锌-硫化铟异质结材料的XRD图,由图7可知,该硫化锌-硫化铟异质结材料的晶体结构结构有序,与合成的单独硫化铟和硫化锌的晶体结构相对应。
图8实施例3中制备的硫化锌-硫化铟异质结材料的FESEM图,由图8可知,该硫化锌-硫化铟异质结材料呈纳米棒状,尺寸为数十纳米,且分散均匀。
图9实施例3中制备的硫化锌-硫化铟异质结材料的TEM图,由图9可知,该硫化锌-硫化铟异质结材料为具有丰富界面的纳米异质结。
实施例4
测试实施例1中制备的硫化锌-硫化铟异质结材料对甲基橙的光催化降解能力
取50mg实施例1中制备的硫化锌-硫化铟异质结材料、50mg ZnS和50mg In2S3分别分散于50mL浓度为10ppm的甲基橙溶液中,黑暗吸附平衡30min后在可见光下进行降解测试,测试如图10所示,由图10可知,与单纯ZnS和In2S3相比,实施例1中制备的硫化锌-硫化铟异质结材料在15min内吸附和降解了更多的甲基橙。
实施例5
测试实施例1中制备的硫化锌-硫化铟异质结材料对乙基紫的光催化降解能力
取50mg实施例1中制备的硫化锌-硫化铟异质结材料、50mg ZnS和50mg In2S3分别分散于100mL浓度为10ppm的乙基紫溶液中,黑暗吸附平衡30min后在可见光下进行降解测试,测试如图11所示,由图11可知,与单纯ZnS和In2S3相比,实施例1中制备的硫化锌-硫化铟异质结材料在30min内吸附和降解了更多的乙基紫。
实施例6
测试实施例1中制备的硫化锌-硫化铟异质结材料对盐酸四环素的光催化降解能力
取50mg实施例1中制备的硫化锌-硫化铟异质结材料分散于50mL浓度为20ppm的盐酸四环素溶液中,黑暗吸附平衡30min后在可见光下进行降解测试,测试如图12所示,由图12可知,实施例1中制备的硫化锌-硫化铟异质结材料在20min内降解了74%的盐酸四环素。
实施例7
测试实施例1中制备的硫化锌-硫化铟异质结材料对双酚A的光催化降解能力
取50mg实施例1中制备的硫化锌-硫化铟异质结材料分散于50mL浓度为18ppm的双酚A溶液中,黑暗吸附平衡30min后在可见光下进行降解测试,测试如图13所示,由图13可知,实施例1中制备的硫化锌-硫化铟异质结材料在20min内降解了73%的双酚A。
实施例8
测试实施例1中制备的硫化锌-硫化铟异质结材料的光电流
按V乙醇溶液:VNafion溶液=20:1将质量分数为5%的Nafion溶液加入乙醇溶液(V水:V乙醇=1:1)中,获得混合液,将2mg实施例1中制备的硫化锌-硫化铟异质结材料、2mg ZnS和2mgIn2S3分别分散与1mL上述混合液中超声,各取5μL滴加到直径为3mm的环盘电极上,干燥后,在0.1M的Na2SO4溶液中,使用电化学工作站测试光电流,测试结果如图14所示,由图14可知,与单纯ZnS和In2S3相比,实施例1中制备的硫化锌-硫化铟异质结材料的光电流明显增大,证明其具有更好的光催化能力。
实施例9
测试实施例2中制备的硫化锌-硫化铟异质结材料的光电流
测试方法参照实施例8,测试结果如图15所示,由图15可知,与单纯ZnS和In2S3相比,实施例2中制备的硫化锌-硫化铟异质结材料的光电流明显增大,证明其具有更好的光催化能力。
实施例10
测试实施例3中制备的硫化锌-硫化铟异质结材料的光电流
测试方法参照实施例8,测试结果如图16所示,由图16可知,与单纯ZnS和In2S3相比,实施例3中制备的硫化锌-硫化铟异质结材料的光电流明显增大,证明其具有更好的光催化能力。
最后说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本技术方案的宗旨和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (7)
1.一种硫化锌-硫化铟异质结材料的制备方法,其特征在于,所述方法如下:
将硝酸铟和ZIF-8分别加入乙醇溶液中,然后将含硝酸铟的乙醇溶液加入含ZIF-8的乙醇溶液中,混匀后通过溶剂热法在100-180℃下反应1-6h,经抽滤、洗涤、干燥后获得中间产物,最后将所述中间产物与硫粉混匀后置于管式炉中,以1-10℃/min的速率升温至400-600℃后保温1-6h,即可;
所述硝酸铟与ZIF-8的质量比为5-18:1,所述中间产物与硫粉的质量比小于等于1:3。
2.如权利要求1所述的方法,其特征在于,所述乙醇溶液的体积分数为90%以上。
3.如权利要求1所述的方法,其特征在于,所述洗涤具体为以乙醇溶液洗涤。
4.如权利要求1所述的方法,其特征在于,所述干燥具体为在50-100℃下真空干燥6h以上。
5.由权利要求1-4任一项所述的方法制备的硫化锌-硫化铟异质结材料。
6.权利要求5所述的硫化锌-硫化铟异质结材料在光催化降解有机污染物中的应用。
7.如权利要求6所述的应用,其特征在于,所述有机污染物为甲基橙、乙基紫、盐酸四环素或双酚A中的至少一种。
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