CN116099555A - 一种ZnO基三元Z型结构光催化剂的制备方法及用途 - Google Patents
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Abstract
本发明涉及一种ZnO基三元Z型结构光催化剂的制备方法,包括,种子层制备‑生长ZnO纳米棒阵列‑磁控溅射Bi纳米粒子‑ZnO/Bi/CdTe双壳层复合物的构建‑有机污染物的光催化降解。本发明方法结合了Bi纳米粒子的可见光及近红外光高响应的优势,有效扩展了ZnO/CdTe的光响应范围。该方法选用透光率高、导电性好的氧化铟锡导电玻璃作为基底,所制备的复合材料具有比单纯的ZnO、ZnO/CdTe更高的光降解性能,在太阳光下对对硝基苯酚的降解效率高达89.65%。
Description
技术领域
本发明涉及光催化剂的合成方法,特别涉及一种ZnO基三元Z型结构光催化剂的制备方法及用途。
背景技术
对硝基苯酚作为燃料、医药、农药等精细化工产品生产的重要中间体,是工业和农业生产废水中常见的一种有机污染物,具有高毒性和难降解的特性。因此,迫切需要开发一种有效的方法来消除废水中的对硝基苯酚。光催化技术借助纳米材料在光照下表面能受激活化的特性,利用光能有效地氧化分解有机物污染物,使其完全矿化为水和无机离子,且光催化剂本身无毒无害,无二次污染,是一种具有广阔应用前景的绿色环境治理技术。
近年来,光敏纳米材料因其良好的吸光性和优越的导电性能收到研究者的广泛关注。ZnO作为一种n型半导体材料,室温下其禁带宽度为3.20eV,具有毒性低、价格便宜、容易获得等优点,被极大地应用于光催化领域。但是,未经修饰的ZnO仅局限于紫外区域的激发,这阻碍了从光到电的有效转换,光催化反应量子效率比较低。为了扩大ZnO对可见光的吸收范围,CdTe作为一种直接跃迁型能带结构且有很高的光吸收系数的纳米材料,可有效吸收波长小于850nm的入射太阳光,与ZnO复合能够有效提高光电转换效率和信号的输出。然而ZnO/CdTe仅对可见光区域具有很小的吸收,因此其应用仍然受到限制。
发明内容
发明目的:本发明提供一种ZnO基三元Z型结构光催化剂的制备方法。
本发明另一目的是提供所述ZnO基三元Z型结构光催化剂的用途。
本发明方法引入具有独特的贵金属(Ag和Au)性质的Bi纳米粒子,将其包覆于纳米阵列的中间作为载流子传输介质,将光源吸收扩展到近红外区,极大促进电子-空穴对的分离效率,进而得到更高的光催化活性。
技术方案:本发明所述ZnO基三元Z型结构光催化剂的制备方法,包括如下步骤:
(1)氧化铟锡导电玻璃基底的清洗及ZnO种子层的制备;
(2)水热法合成ZnO纳米棒阵列;
(3)磁控溅射法依次包覆Bi纳米粒子和CdTe纳米壳层,构建ZnO/Bi/CdTe三元体系复合材料。
进一步地,步骤(1)的制备方法为:将氧化铟锡导电玻璃裁剪,依次放入丙酮、无水乙醇、超纯水超声处理,干燥后放置于含有ZnO靶材的磁控溅射系统中生长种子层。
进一步地,溅射时间为10~30min,氧气和氩气的流量分别是5~15sccm和50~100sccm,工作气压为2~5Pa。
进一步地,步骤(2)合成方法为:取二水醋酸锌和六次甲基四胺溶于超纯水中,充分溶解,得到ZnO前驱体溶液,然后将溅射有ZnO种子层的氧化铟锡浸泡在该溶液中,反应后,清洗样品,干燥。
进一步地,步骤(3)将步骤(2)中制备好的ZnO基导电玻璃置于氩气流量50~100sccm,工作气压2~5Pa的条件下先后磁控溅射Bi和CdTe纳米粒子壳层。
进一步地,所述溅射功率分别为10~30W和40~80W,溅射时间分别为2~8min和2~10min,成功构建Z型结构光催化剂。
ZnO基三元Z型结构光催化剂在光降解硝基苯酚中的用途。
进一步地,光降解硝基苯酚的方法是将制备好的ZnO/Bi/CdTe导电玻璃插入对硝基苯酚溶液中,施加电压,对硝基苯酚进行降解。
有益效果:本发明与现有技术相比,具有如下优势:
(1)本发明在传统的ZnO纳米棒阵列表面包覆了CdTe纳米壳层,有效的扩大了对光的吸收和基底材料的导电性;
(2)同时引入Bi纳米粒子作为载流子传输中间介质,将对光的吸收有效扩展到近红外区域,利用其类贵金属特性极大地降低了电子-空穴的复合速率,提高了光催化反应量子效率;
(3)利用电化学工作站施加一定电压进一步提高了复合材料的光电转化效率,促进了对有机污染物的光催化降解。
附图说明
图1为本发明制备的ZnO/Bi/CdTe纳米棒核壳阵列扫描电子显微镜图;
图2为本发明制备的光催化剂的紫外-可见光吸收谱图;
图3为本发明制备的ZnO基三元Z型结构光催化剂对有机污染物对硝基苯酚的光降解性能。
具体实施方式
本实施例1的光催化降解对硝基苯酚的ZnO基三元Z型结构光催化剂的制备及应用,包括如下步骤:
(1)氧化铟锡导电玻璃基底的清洗及ZnO种子层的制备:将氧化铟锡导电玻璃裁剪成1cm×2cm尺寸,依次放入丙酮、无水乙醇、超纯水超声处理10min,在40℃烘箱干燥30min后放置于含有ZnO靶材的磁控溅射系统中生长种子层,溅射时间为20min,氧气和氩气的流量分别是5sccm和55sccm,工作气压为2Pa。
(2)水热法合成ZnO纳米棒阵列:首先称取0.7902g二水醋酸锌和0.5047g六次甲基四胺溶于90mL超纯水中,搅拌20min使其充分溶解,得到ZnO前驱体溶液,然后将溅射有ZnO种子层的氧化铟锡浸泡在此溶液中,90℃反应6h,取出样品,超纯水冲洗干净后放入烘箱干燥。
(3)磁控溅射法依次包覆Bi纳米粒子和CdTe纳米壳层,构建ZnO/Bi/CdTe三元体系复合材料:将制备好的ZnO基导电玻璃置于氩气流量55sccm,工作气压2Pa的条件下先后磁控溅射Bi和CdTe纳米粒子壳层,溅射功率分别为20W和60W,溅射时间分别为4min和5min,成功构建Z型结构光催化剂。如图1所示,外层Bi和CdTe纳米粒子均匀的包覆在ZnO纳米棒的表面,形成复合纳米阵列结构。后续对此复合基底进行光吸收的表征,如图2所示,纯ZnO的光吸收范围在紫外区,在Bi和CdTe纳米粒子包覆以后其吸收范围扩展至可见区以及近红外区。
(4)将构建的Z型结构光催化剂与三电极电化学工作站连接,实现有机污染物对硝基苯酚的光降解:将制备好的ZnO/Bi/CdTe导电玻璃插入浓度为1.0mmol/L的对硝基苯酚溶液中,通过电化学工作站施加一定电压提高复合材料的光电转换效率,最终实现对硝基苯酚的有效降解。
(5)结果观察:通过紫外-可见吸收光谱观测对硝基苯酚在318nm处的光强度随光催化时间的变化,如图3所示,随着降解时间的增加,其吸收光谱强度逐渐降低,结果为光降解效率高达89.65%。
本实施例2的光催化降解对硝基苯酚的ZnO基三元Z型结构光催化剂的制备及应用,包括如下步骤:
(1)氧化铟锡导电玻璃基底的清洗及ZnO种子层的制备:将氧化铟锡导电玻璃裁剪成1cm×2cm尺寸,依次放入丙酮、无水乙醇、超纯水超声处理10min,在40℃烘箱干燥30min后放置于含有ZnO靶材的磁控溅射系统中生长种子层,溅射时间为10min,氧气和氩气的流量分别是15sccm和100sccm,工作气压为5Pa。
(2)水热法合成ZnO纳米棒阵列:首先称取0.7902g二水醋酸锌和0.5047g六次甲基四胺溶于90mL超纯水中,搅拌20min使其充分溶解,得到ZnO前驱体溶液,然后将溅射有ZnO种子层的氧化铟锡浸泡在此溶液中,90℃反应6h,取出样品,超纯水冲洗干净后放入烘箱干燥。
(3)磁控溅射法依次包覆Bi纳米粒子和CdTe纳米壳层,构建ZnO/Bi/CdTe三元体系复合材料:将制备好的ZnO基导电玻璃置于氩气流量100sccm,工作气压5Pa的条件下先后磁控溅射Bi和CdTe纳米粒子壳层,溅射功率分别为10W和40W,溅射时间分别为8min和10min,成功构建Z型结构光催化剂,。
(4)将构建的Z型结构光催化剂与三电极电化学工作站连接,实现有机污染物对硝基苯酚的光降解:将制备好的ZnO/Bi/CdTe导电玻璃插入浓度为1.0mmol/L的对硝基苯酚溶液中,通过电化学工作站施加一定电压提高复合材料的光电转换效率,最终实现对硝基苯酚的有效降解,光降解效率高达87.32%。
本实施例3的光催化降解对硝基苯酚的ZnO基三元Z型结构光催化剂的制备及应用,包括如下步骤:
(1)氧化铟锡导电玻璃基底的清洗及ZnO种子层的制备:将氧化铟锡导电玻璃裁剪成1cm×2cm尺寸,依次放入丙酮、无水乙醇、超纯水超声处理10min,在40℃烘箱干燥30min后放置于含有ZnO靶材的磁控溅射系统中生长种子层,溅射时间为30min,氧气和氩气的流量分别是15sccm和100sccm,工作气压为5Pa。
(2)水热法合成ZnO纳米棒阵列:首先称取0.7902g二水醋酸锌和0.5047g六次甲基四胺溶于90mL超纯水中,搅拌20min使其充分溶解,得到ZnO前驱体溶液,然后将溅射有ZnO种子层的氧化铟锡浸泡在此溶液中,90℃反应6h,取出样品,超纯水冲洗干净后放入烘箱干燥。
(3)磁控溅射法依次包覆Bi纳米粒子和CdTe纳米壳层,构建ZnO/Bi/CdTe三元体系复合材料:将制备好的ZnO基导电玻璃置于氩气流量100sccm,工作气压5Pa的条件下先后磁控溅射Bi和CdTe纳米粒子壳层,溅射功率分别为30W和80W,溅射时间分别为2min和2min,成功构建Z型结构光催化剂。
(4)将构建的Z型结构光催化剂与三电极电化学工作站连接,实现有机污染物对硝基苯酚的光降解:将制备好的ZnO/Bi/CdTe导电玻璃插入浓度为1.0mmol/L的对硝基苯酚溶液中,通过电化学工作站施加一定电压提高复合材料的光电转换效率,最终实现对硝基苯酚的有效降解,光降解效率高达86.84%。
Claims (8)
1.一种ZnO基三元Z型结构光催化剂的制备方法,其特征在于,包括以下步骤:
(1)氧化铟锡导电玻璃基底的清洗及ZnO种子层的制备;
(2)水热法合成ZnO纳米棒阵列;
(3)依次包覆Bi纳米粒子和CdTe纳米壳层,构建ZnO/Bi/CdTe三元体系复合材料,获得所述的Z型结构光催化剂。
2.根据权利要求1所述的ZnO基三元Z型结构光催化剂的制备方法,其特征在于:步骤(1)的制备方法为:将氧化铟锡导电玻璃裁剪,依次放入丙酮、无水乙醇、超纯水超声处理,干燥后放置于含有ZnO靶材的磁控溅射系统中生长种子层。
3.根据权利要求2所述的ZnO基三元Z型结构光催化剂的制备方法,其特征在于:溅射时间为10~30min,氧气和氩气的流量分别是5~15sccm和50~100sccm,工作气压为2~5Pa。
4.根据权利要求1所述的ZnO基三元Z型结构光催化剂的制备方法,其特征在于:步骤(2)合成方法为:取二水醋酸锌和六次甲基四胺溶于超纯水中,充分溶解,得到ZnO前驱体溶液,然后将溅射有ZnO种子层的氧化铟锡浸泡在该溶液中,反应后,清洗样品,干燥。
5.根据权利要求1所述的ZnO基三元Z型结构光催化剂的制备方法,其特征在于:步骤(3)将步骤(2)中制备好的ZnO基导电玻璃置于氩气流量50~100sccm,工作气压2~5Pa的条件下先后磁控溅射Bi和CdTe纳米粒子壳层。
6.根据权利要求5所述的ZnO基三元Z型结构光催化剂的制备方法,其特征在于:所述溅射功率分别为10~30W和40~80W,溅射时间分别为2~8min和2~10min,成功构建Z型结构光催化剂。
7.权利要求1-6任一项制备得到的ZnO基三元Z型结构光催化剂在光降解硝基苯酚中的用途。
8.根据权利要求7所述的用途,其特征在于:光降解硝基苯酚的方法是将制备好的ZnO/Bi/CdTe导电玻璃插入对硝基苯酚溶液中,施加电压,对硝基苯酚进行降解。
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