CN105499596A - 在电沉积CdSe薄膜上自发生长Au纳米微粒的方法 - Google Patents
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Abstract
本发明公开了一种在电沉积CdSe薄膜上自发生长Au纳米微粒的方法。利用二价镉盐和二氧化硒(SeO2)混合溶液,先利用电沉积的方法将CdSe沉积在电极表面,形成一种载体薄膜,把电极浸入Au纳米颗粒生长液中,再在恒温水浴锅中生长1~3h,最后取出电极,电极上就自发地生长上Au纳米微粒。本发明方法制备步骤简单,所沉积的复合膜附着力强,效率高,成本低廉,非常适宜大规模生产。
Description
技术领域
本发明属于纳米材料及电化学领域,特别涉及一种在电沉积CdSe薄膜上自发生长Au纳米微粒的方法。
背景技术
硒化镉(CdSe)是n型直接能隙的半导体材料,其禁带宽度为1.8eV左右,是一种化学性质较稳定的半导体材料,具有独特的光电转换特性,经常被用来改进宽带隙半导体以提高它们的可见光吸收的能力和光催化活性,在光催化氧化技术针对环境污染的治理和光电催化(PEC)分解水应用广泛而备受关注,但是它本身存在一个很明显的缺点,光生电子与空穴复合将会使得光电催化的活性并不高,所以必须提高催化剂的活性,其中最常用的是进行贵金属(Au,Ag,Pd等)沉积,贵金属的活性很高,经过贵金属沉淀修饰之后得催化剂可以改变其体系中的电子分布,从而提高光电催化性能。目前制备硒化镉(CdSe)薄膜的常用方法有电沉积法、分子束外延法、水热法、溶胶-凝胶法、化学浴沉积法等。其中电沉积法优点最突出,生产设备简单,反应条件要求低,膜的厚度可控,适合大规模生产。利用化学水域自发生长贵金属(Au,Ag,Pd等),方法简单,相比于其他生长方法,其最大优点就是无需另外添加还原剂,而其他方法制备步骤繁琐,使用溶剂多,效率较低,成本高,很难大规模工业化生产。
发明内容
本发明的目的是提供一种在电沉积CdSe薄膜上自发生长Au纳米微粒的方法。
本发明的原理和思路:利用电聚合的方法将CdSe沉积在电极表面,形成一种载体薄膜,把电极浸入Au纳米颗粒生长液中,再在恒温水浴锅中生长1~3h,最后取出电极,电极上就自发地生长上Au纳米微粒。
具体步骤为:
(1)将电极分别经分析纯丙酮、分析纯乙醇和二次水各超声清洗3min,在空气中干燥后用万能表测量出导电一面,备用,即为基体电极。
(2)量取6mL浓度为0.05~0.15mol/L的二价镉盐溶液置于洁净的小烧杯中,并在磁力搅拌下分六次分别加入1mL浓度为0.01~0.1mol/L的SeO2水溶液,制得电沉积CdSe薄膜底液。
(3)在步骤(2)制得的电沉积CdSe薄膜底液中构建三电极体系,其中,步骤(1)制得的基体电极作为工作电极,Ag/AgCl作为参比电极,Pt作为辅助电极,采用循环伏安法进行电沉积,扫描范围为-1.1~0V,扫描速度为0.05V/s,扫描段数为20~40段,扫描结束后,基体电极表面就沉积出CdSe薄膜,制得薄膜基片。
(4)量取9.52mL二次水,300μLPBS溶液,100μL质量浓度为1%的氯金酸水溶液和80μL浓度为0.2mol/L的十六烷基三甲基氯化铵水溶液,混合制得生长液,然后把步骤(3)制得的薄膜基片斜放入生长液中,置于45℃水浴锅中恒温条件下反应1~3h,薄膜基片上自发生长出Au纳米微粒。
所述电极为掺杂氟的二氧化锡透明导电玻璃电极或铟锡氧化物电极。
所述二价镉盐为CdCl2、Cd(NO3)2和CdSO4中的一种或多种。
所述PBS溶液是浓度为0.2mol/L,pH值为6.0的NaH2PO4-Na2HPO4缓冲溶液。
本发明方法制备过程简单,薄膜附着力强,生长效率高,成本低,易于大规模推广。
附图说明
图1为本发明实施例1制备的最终产物的X射线衍射图。
图2为本发明实施例1中电沉积制备的CdSe薄膜的扫描电镜图。
图3为本发明实施例1中在电沉积CdSe薄膜上生长Au的产物的扫描电镜图。
具体实施方式
以下将结合说明书附图和具体实施例对本发明做进一步详细说明。
实施例1:
(1)将电极分别经分析纯丙酮、分析纯乙醇和二次水各超声清洗3min,在空气中干燥后用万能表测量出导电一面,备用,即为基体电极。
(2)量取6mL浓度为0.05mol/L的二价镉盐溶液置于洁净的小烧杯中,并在磁力搅拌下分六次分别加入1mL浓度为0.01mol/L的SeO2水溶液,制得电沉积CdSe薄膜底液。
(3)在步骤(2)制得的电沉积CdSe薄膜底液中构建三电极体系,其中,步骤(1)制得的基体电极作为工作电极,Ag/AgCl作为参比电极,Pt作为辅助电极,采用循环伏安法进行电沉积,扫描范围为-1.1~0V,扫描速度为0.05V/s,扫描段数为20段,扫描结束后,基体电极表面就沉积出CdSe薄膜,制得薄膜基片。
(4)量取9.52mL二次水,300μLPBS溶液,100μL质量浓度为1%的氯金酸水溶液和80μL浓度为0.2mol/L的十六烷基三甲基氯化铵水溶液,混合制得生长液,然后把步骤(3)制得的薄膜基片斜放入生长液中,置于45℃水浴锅中恒温条件下反应1h,薄膜基片上自发生长出Au纳米微粒。
所述电极为掺杂氟的二氧化锡透明导电玻璃电极。
所述二价镉盐为CdCl2。
所述PBS溶液是浓度为0.2mol/L,pH值为6.0的NaH2PO4-Na2HPO4缓冲溶液。
将本实施例制得的最终产物进行X射线衍射测试,结果见图1,基体电极上所获得的产物为Au,CdSe。将本实施例中电沉积出的CdSe进行扫描电镜测试,结果见图2,能够清晰看到CdSe沉积物的颗粒形貌。将本实施例中在电沉积CdSe薄膜上生长Au的产物进行扫描电镜测试,结果见图3,能够清晰辨析到Au纳米微粒附着在CdSe的颗粒上。
实施例2:
(1)将电极分别经分析纯丙酮、分析纯乙醇和二次水各超声清洗3min,在空气中干燥后用万能表测量出导电一面,备用,即为基体电极。
(2)量取6mL浓度为0.1mol/L的二价镉盐溶液置于洁净的小烧杯中,并在磁力搅拌下分六次分别加入1mL浓度为0.05mol/L的SeO2水溶液,制得电沉积CdSe薄膜底液。
(3)在步骤(2)制得的电沉积CdSe薄膜底液中构建三电极体系,其中,步骤(1)制得的基体电极作为工作电极,Ag/AgCl作为参比电极,Pt作为辅助电极,采用循环伏安法进行电沉积,扫描范围为-1.1~0V,扫描速度为0.05V/s,扫描段数为30段,扫描结束后,基体电极表面就沉积出CdSe薄膜,制得薄膜基片。
(4)量取9.52mL二次水,300μLPBS溶液,100μL质量浓度为1%的氯金酸水溶液和80μL浓度为0.2mol/L的十六烷基三甲基氯化铵水溶液,混合制得生长液,然后把步骤(3)制得的薄膜基片斜放入生长液中,置于45℃水浴锅中恒温条件下反应2h,薄膜基片上自发生长出Au纳米微粒。
所述电极为掺杂氟的二氧化锡透明导电玻璃电极。
所述二价镉盐为Cd(NO3)2。
所述PBS溶液是浓度为0.2mol/L,pH值为6.0的NaH2PO4-Na2HPO4缓冲溶液。
实施例3:
(1)将电极分别经分析纯丙酮、分析纯乙醇和二次水各超声清洗3min,在空气中干燥后用万能表测量出导电一面,备用,即为基体电极。
(2)量取6mL浓度为0.15mol/L的二价镉盐溶液置于洁净的小烧杯中,并在磁力搅拌下分六次分别加入1mL浓度为0.1mol/L的SeO2水溶液,制得电沉积CdSe薄膜底液。
(3)在步骤(2)制得的电沉积CdSe薄膜底液中构建三电极体系,其中,步骤(1)制得的基体电极作为工作电极,Ag/AgCl作为参比电极,Pt作为辅助电极,采用循环伏安法进行电沉积,扫描范围为-1.1~0V,扫描速度为0.05V/s,扫描段数为40段,扫描结束后,基体电极表面就沉积出CdSe薄膜,制得薄膜基片。
(4)量取9.52mL二次水,300μLPBS溶液,100μL质量浓度为1%的氯金酸水溶液和80μL浓度为0.2mol/L的十六烷基三甲基氯化铵水溶液,混合制得生长液,然后把步骤(3)制得的薄膜基片斜放入生长液中,置于45℃水浴锅中恒温条件下反应3h,薄膜基片上自发生长出Au纳米微粒。
所述电极为掺杂氟的二氧化锡透明导电玻璃电极。
所述二价镉盐为CdSO4。
所述PBS溶液是浓度为0.2mol/L,pH值为6.0的NaH2PO4-Na2HPO4缓冲溶液。
以上仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,与本发明构思无实质性差异的各种工艺方案均在本发明的保护范围内。
Claims (1)
1.一种在电沉积CdSe薄膜上自发生长Au纳米微粒的方法,其特征在于具体步骤为:
(1)将电极分别经分析纯丙酮、分析纯乙醇和二次水各超声清洗3min,在空气中干燥后用万能表测量出导电一面,备用,即为基体电极;
(2)量取6mL浓度为0.05~0.15mol/L的二价镉盐溶液置于洁净的小烧杯中,并在磁力搅拌下分六次分别加入1mL浓度为0.01~0.1mol/L的SeO2水溶液,制得电沉积CdSe薄膜底液;
(3)在步骤(2)制得的电沉积CdSe薄膜底液中构建三电极体系,其中,步骤(1)制得的基体电极作为工作电极,Ag/AgCl作为参比电极,Pt作为辅助电极,采用循环伏安法进行电沉积,扫描范围为-1.1~0V,扫描速度为0.05V/s,扫描段数为20~40段,扫描结束后,基体电极表面就沉积出CdSe薄膜,制得薄膜基片;
(4)量取9.52mL二次水,300μLPBS溶液,100μL质量浓度为1%的氯金酸水溶液和80μL浓度为0.2mol/L的十六烷基三甲基氯化铵水溶液,混合制得生长液,然后把步骤(3)制得的薄膜基片斜放入生长液中,置于45℃水浴锅中恒温条件下反应1~3h,薄膜基片上自发生长出Au纳米微粒;
所述电极为掺杂氟的二氧化锡透明导电玻璃电极或铟锡氧化物电极;
所述二价镉盐为CdCl2、Cd(NO3)2和CdSO4中的一种或多种;
所述PBS溶液是浓度为0.2mol/L,pH值为6.0的NaH2PO4-Na2HPO4缓冲溶液。
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