CN107029755A - 一种异质结光催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种Ag2S/SnS2异质结光催化剂及其制备方法。首先通过水热法合成SnS2纳米片，再在含有SnS2纳米片的水溶液中加入银离子，使其与二硫化锡发生离子交换反应，得到Ag2S/SnS2异质结复合光催化剂。Ag2S纳米颗粒与SnS2纳米片的结合明显地增强了它们的光电性能与光催化性能，Ag2S(8wt％)/SnS2复合物，光生电密度是的SnS22倍。异质结光催化降解甲基橙的活性显然优于Ag2S和SnS2纳米片。该方法操作简便、条件温和、产率高，所制备的SnS2超薄纳米片具有很高的光催化活性。
Description
技术领域
本发明所属技术领域为光催化、光电化学材料技术领域，特别涉及二硫化锡异质结光催化剂开发及制备方法。
背景技术
SnS2作为一种具有良好光电性的半导体材料，其直接禁带宽度为1.91～2.4eV，而且二维层状的SnS2具有光学性质各向异性和优越的化学稳定性。二维SnS2纳米片因其层间距比较大且有晶格空位，SnS2还被用作光催化剂，分解有机污染物或废水中的重金属离子等，主要是因为高吸光性、无毒、抗氧化性与化学稳定性高。虽然具有窄带隙能的SnS2可以高效利用可见光，光催化活性高，被视为一种极具应用潜力的光催化剂；但是，SnS2的光催化活性依然不够高，且自身易发生分解。另外，光催化反应后，SnS2的再次重复收集比较困难。构建含有SnS2的异质结复合半导体材料，是一种有效提高SnS2光催化活性的途径，便于解决其重复使用性的问题。
硫化银是一种窄带隙的直接半导体，而且其带隙值约为0.9～1.1eV，吸光系数特别高，被应用于太阳能电池、光电导元件、光电设备的光敏薄膜、光敏涂料和红外探测器等。特别地，Ag2S因其带隙比较窄而具有非常宽的吸收光谱，使其成为一种高效的半导体光催化剂材料。所以本专利中将Ag2S作为助催化剂与SnS2构建异质结催化剂，以提高SnS2的光催化活性及稳定性。希望其突出的性能可以在光催化领域有实际的应用，有效解决现在社会环境污染问题。
发明内容
本发明的目的是提供一种Ag2S/SnS2异质结光催化剂及其制备方法，该方法操作简便、条件温和、产率高，所制备的SnS2超薄纳米片具有很高的光催化活性。
具体步骤为：
(1)将0.1～10mmol四氯化锡和0.2～20mmol硫源加入到40mL的蒸馏水中，四氯化锡：硫源摩尔比为1：2，混合均匀后加入到容积为50mL的聚四氟乙烯反应釜中,110～180℃条件下反应0.5～5天，自然冷却至室温后分别用蒸馏水和无水乙醇各离心清洗2～3次，60℃真空干燥，得到SnS2纳米片；
(2)将步骤(1)合成的制的0.5g SnS2纳米片，投入500mL的烧杯中，量取300mL蒸馏水加入烧杯中，超声分散3小时，形成均匀的黄色分散液；随后量取0.01mol/L的Na2S溶液1～10mL加入烧杯中，搅拌10分钟后，再量取0.1mol/L的银盐溶液0.3～20mL，慢慢地逐滴加入烧杯中，30分钟滴加完，仍然搅拌3小时，最后30℃恒温2小时，得到褐色沉淀物，即为Ag2S/SnS2异质结光催化剂。；
所述硫源为硫代乙酰胺(TAA)、硫粉、硫化钠、硫化钾、硫化铵、硫脲和硫代硫酸钠中的一种。
所述的银盐为硝酸银、硫酸银、醋酸银、氟化银、苯甲酸银中的一种
所述化学试剂纯度均为化学纯以上纯度。
本发明Ag2S/SnS2复合物展示出了优异的吸光性能和很强的光电化学响应，光生电流密度为是纯SnS2的2倍；同时其光催化活性显著增强，尤其是，Ag2S(8wt％)/SnS2复合物样品光催化降解甲基橙平均速度0.0440mg/min，20min甲基橙分解率达到99.9％。经过5次循环重复稳定性实验后，仍然保持很高的活性，具有很强的稳定性。因此，Ag2S/SnS2作为一种可见光响应材料，在环境污染如降解染料、光催化处理污水，太阳能电池等方面具有很大的应用潜能。
附图说明
图1为本发明实施例1制备的不同组成粉末XRD谱。
图2为本发明实施例1制备(a,b)SnS2纳米片的TEM图，(c,d)Ag2S/SnS2复合物的TEM图。
图3为本发明实施例1制备的SnS2纳米片、Ag2S和Ag2S/SnS2复合物的光生电流曲线。。
图4为本发明实施例1制备的(a)不同粉末样品光催化降解甲基橙，(b)样品粉末光催化降解甲基橙的动力学线性拟合曲线。
具体实施方式
实施例1：
(1)将4mmol四氯化锡和8mmol硫代乙酰胺加入到40mL的蒸馏水中，，混合均匀后加入到容积为50mL的聚四氟乙烯反应釜中,180℃条件下反应24小时，自然冷却至室温后分别用蒸馏水和无水乙醇各离心清洗2～3次，60℃真空干燥，得到SnS2纳米片；
(2)将步骤(1)合成的制的0.5g SnS2纳米片，投入500mL的烧杯中，量取300mL蒸馏水加入烧杯中，超声分散3小时，形成均匀的黄色分散液；随后量取0.01mol/L的Na2S溶液3mL加入烧杯中，搅拌10分钟后，再量取0.1mol/L的硝酸银溶液4mL，慢慢地逐滴加入烧杯中，30分钟滴加完，仍然搅拌3小时，最后30℃恒温2小时，得到褐色沉淀物，即为Ag2S/SnS2异质结光催化剂。
所制备的SnS2薄纳米片分散液，通过旋涂法在ITO表面做成光电极，制备电极作为工作电极(面积为1cm2)，辅助电极为铂电极，饱和甘汞电极(SCE)作为参比电极，0.5mol/LNa2SO4为支持电解质溶液，在太阳光模拟器(一个太阳的光强)下测试光电化学性能，从图3可以看出Ag2S/SnS2异质结的光电流高于SnS2、Ag2S的光电流。
实施例2：
(1)将2mmol四氯化锡和4mmol硫化钠加入到40mL的蒸馏水中，，混合均匀后加入到容积为50mL的聚四氟乙烯反应釜中,180℃条件下反应24小时，自然冷却至室温后分别用蒸馏水和无水乙醇各离心清洗2～3次，60℃真空干燥，得到SnS2纳米片；
(2)将步骤(1)合成的制的0.5g SnS2纳米片，投入500mL的烧杯中，量取300mL蒸馏水加入烧杯中，超声分散3小时，形成均匀的黄色分散液；随后量取0.01mol/L的Na2S溶液3mL加入烧杯中，搅拌10分钟后，再量取0.1mol/L的醋酸银溶液1mL，慢慢地逐滴加入烧杯中，30分钟滴加完，仍然搅拌3小时，最后30℃恒温2小时，得到褐色沉淀物，即为Ag2S/SnS2异质结光催化剂。
实施例3：
(1)将10mmol四氯化锡和20mmol硫脲加入到40mL的蒸馏水中，，混合均匀后加入到容积为50mL的聚四氟乙烯反应釜中,180℃条件下反应24小时，自然冷却至室温后分别用蒸馏水和无水乙醇各离心清洗2～3次，60℃真空干燥，得到SnS2纳米片；
(2)将步骤(1)合成的制的0.5g SnS2纳米片，投入500mL的烧杯中，量取300mL蒸馏水加入烧杯中，超声分散3小时，形成均匀的黄色分散液；随后量取0.01mol/L的Na2S溶液3mL加入烧杯中，搅拌10分钟后，再量取0.1mol/L的苯甲酸银银溶液4mL，慢慢地逐滴加入烧杯中，30分钟滴加完，仍然搅拌3小时，最后30℃恒温2小时，得到褐色沉淀物，即为Ag2S/SnS2异质结光催化剂。
以上实施例所述化学试剂纯度均为化学纯。
Claims (3)
1.一种Ag2S/SnS2异质结光催化剂,摩尔比组成为SnS2 85～99.5％，Ag2S0.5～15％。
2.一种Ag2S/SnS2异质结光催化剂的制备方法，其特征在于具体步骤为：
(1)将0.1～10mmol四氯化锡和0.2～20mmol硫源加入到40mL的蒸馏水中，四氯化锡：硫源摩尔比为1：2，混合均匀后加入到容积为50mL的聚四氟乙烯反应釜中,110～180℃条件下反应0.5～5天，自然冷却至室温后分别用蒸馏水和无水乙醇各离心清洗2～3次，60℃真空干燥，得到SnS2纳米片；
(2)将步骤(1)合成的制的0.5g SnS2纳米片，投入500mL的烧杯中，量取300mL蒸馏水加入烧杯中，超声分散3小时，形成均匀的黄色分散液；随后量取0.01mol/L的Na2S溶液1～10mL加入烧杯中，搅拌10分钟后，再量取0.1mol/L的银盐溶液0.3～20mL，慢慢地逐滴加入烧杯中，30分钟滴加完，仍然搅拌3小时，最后30℃恒温2小时，得到褐色沉淀物，即为Ag2S/SnS2异质结光催化剂。
所述化学试剂纯度均为化学纯以上纯度。
3.根据权利要求1所述的一种制备SnS2超薄纳米片的方法，其特征在于：步骤(1)中硫源为硫代乙酰胺(TAA)、硫粉、硫化钠、硫化钾、硫化铵、硫脲、硫代硫酸钠中的一种。
步骤(2)中银盐为硝酸银、硫酸银、醋酸银、氟化银、苯甲酸银中的一种。
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