CN110176389A - 一种制备金-硫化银-磷酸铅异质结纳米薄膜的方法 - Google Patents

一种制备金-硫化银-磷酸铅异质结纳米薄膜的方法 Download PDF

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CN110176389A
CN110176389A CN201910431722.5A CN201910431722A CN110176389A CN 110176389 A CN110176389 A CN 110176389A CN 201910431722 A CN201910431722 A CN 201910431722A CN 110176389 A CN110176389 A CN 110176389A
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潘宏程
李向葵
陈雯
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Guilin University of Technology
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Abstract

本发明公开了一种制备金‑硫化银‑磷酸铅异质结纳米薄膜的方法。其方法步骤：先利用循环伏安法将PbS沉积在电极表面，然后将电极置于Ag2S的生长液中，于于60℃恒温水浴锅中反应24h后，电极表面即可同时生长出Ag2S‑Pb3(PO4)2异质结纳米薄膜。随后将Ag2S‑Pb3(PO4)2异质结纳米薄膜置于置于HAuCl4的溶液中，于60℃恒温水浴锅中反应6h，电极表面即可生成Au‑Ag2S‑Pb3(PO4)2异质结纳米薄膜。本发明方法成本制备过程简单，且制得的Au‑Ag2S‑Pb3(PO4)2异质结纳米薄膜附着力强，薄膜中金具有纳米尺寸，具有一定的生物分析应用价值。

Description

一种制备金-硫化银-磷酸铅异质结纳米薄膜的方法
技术领域
本发明纳米薄膜材料领域及电化学领域，特别涉及一种制备Au-Ag2S-Pb3(PO4)2异质结纳米薄膜的方法。
背景技术
“异质结”是指两种或两种以上半导体相接触所形成的界面区域。随着科学技术的发展，半导体材料和纳米技术的结合越来越密切，纳米异质结具有纳米材料的表面效应、量子尺寸效应、宏观量子隧道效应和介电限域效应等性质，与传统固体材料相比具有很多优点。
Ag2S是一种n型质结禁带半导体材料，Ag2S具有良好的光电和热电效应，因而被广泛地应用于发光材料、红外光谱检测器和光纤维通讯等领域。Au纳米材料具有生物亲和性和相容性好的特点，被广泛应用于生物传感领域，然而传统的Au纳米材料制备条件较为苛刻，合成过程繁琐，因而寻找简便快捷的Au纳米材料合成方法有助于生物分析领域的研究进展。同时，将Ag2S和Au纳米材料相结合的复合材料，不仅能保留半导体的优异光电性能，还能提升材料的生物分析性能，扩大异质结材料的应用范围。
发明内容
本发明的目的是提供一种制备Au-Ag2S-Pb3(PO4)2异质结纳米薄膜的方法。
具体步骤为：
(1)将事先裁好的ITO导电玻璃电极，分别经由分析纯丙酮、分析纯乙醇和二次水超声清洗5min，干燥后用万能表测出导电面待用。
(2)依次量取1mL浓度为0.2mol/L Pb(NO3)2、1mL浓度为0.2mol/L EDTA、3.5mL浓度为0.3mol/L Na2S2O3和4mL浓度为1.25mol/L Na2SO4溶液置于20mL烧杯中均匀混合，制得电沉积PbS薄膜的底液。
(3)在步骤(2)中制得的电沉积PbS薄膜的底液中建立三电极体系，其中，工作电极为步骤(1)中制得的导电玻璃电极，对电极为Pt电极，参比电极为Ag/AgCl电极，用循环伏安法进行电沉积，电位扫描范围为-1.0V～0V，扫描速度为0.05V/s，扫描段数为40～120。电沉积结束后，将电极取出并用二次水冲洗干净，空气烘干后即可得到PbS薄膜。
(4)将步骤(3)制得的PbS薄膜置于250℃管式炉，氮气氛围中加热1h，待管式炉等却后将PbS薄膜取出。
(5)于20mL的玻璃瓶中依次加入700μL浓度为0.02mol/L的Na2HPO4溶液，80μL浓度为0.01mol/L的AgNO3溶液，100μL质量分数为1％的十二烷基苯磺酸钠溶液，7mL二次水，制得生长Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的PbS薄膜正面朝上放入生长溶液中，于60℃恒温水浴中反应24h后取出PbS薄膜，以二次水冲洗干净，烘干即可得到Ag2S-Pb3(PO4)2薄膜。
(6)于20mL的玻璃瓶中依次加入300μL浓度为0.2mol/L、pH为6的HAc-NaAc缓冲溶液，15μL～100μL质量分数为1％的氯金酸溶液，80μL浓度为0.2mol/L的十六烷基三甲基氯化铵溶液，7mL二次水，制得生长Au-Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的Ag2S-Pb3(PO4)2薄膜置正面朝上放入该生长液中，于60℃恒温水浴反应0.5h～24h后取出，以二次水冲洗干净，烘干即可得到Au-Ag2S-Pb3(PO4)2纳米异质结薄膜。
所述步骤(1)中的ITO导电玻璃为掺杂氧化铟锡的玻璃电极。
本发明方法的优点如下：
(1)本发明方法制得的Au-Ag2S-Pb3(PO4)2纳米异质结薄膜综合了无机材料、半导体材料和纳米材料的优良特性，在光电化学、生物分析以及环保等领域中展现出广阔的应用前景。
(2)本发明方法制备过程简单，试剂消耗量小，成本低，易于大规模生产。
附图说明
图1是本发明实施例1制备的Au-Ag2S-Pb3(PO4)2纳米异质结薄膜的扫描电子显微镜照片(SEM)。
图2是本发明实施例1制备的Au-Ag2S-Pb3(PO4)2纳米异质结薄膜的X射线衍射图谱。
具体实施方式
实施例1
本实施例用于说明本发明制备的Au-Ag2S-Pb3(PO4)2纳米异质结薄膜的合成方法及形貌、组成分析。
(1)将事先裁好的1cm×3cm的ITO导电玻璃电极，分别经由分析纯丙酮、分析纯乙醇和二次水超声清洗5min，干燥后用万能表测出导电面待用。
(2)依次量取1mL浓度为0.2mol/L Pb(NO3)2溶液、1mL浓度为0.2mol/L EDTA溶液、3.5mL浓度为0.3mol/L Na2S2O3溶液和4mL 1.25mol/L Na2SO4溶液置于20mL烧杯中均匀混合，制得电沉积PbS薄膜的底液。
(3)在步骤(2)中制得的电沉积PbS薄膜的底液中建立三电极体系，其中，工作电极为步骤(1)中制得的导电玻璃电极，对电极为Pt电极，参比电极为Ag/AgCl电极，用循环伏安法进行电沉积，电位扫描范围为-1.0V～0V，扫描速度为0.05V/s，扫描段数为100。电沉积结束后，将电极取出并用二次水冲洗干净，空气烘干后即可得到PbS薄膜。
(4)将步骤(3)制得的PbS薄膜置于250℃管式炉，氮气氛围中加热1h，待管式炉等却后将PbS薄膜取出。
(5)于20mL的玻璃瓶中依次加入700μL浓度为0.02mol/L的Na2HPO4溶液，80μL浓度为0.01mol/L的AgNO3溶液，100μL质量分数为1％的十二烷基苯磺酸钠溶液，7mL二次水，制得生长Ag2S-Pb3(PO4)2薄膜的生长液。将步骤(4)中制得的PbS薄膜正面朝上放入生长溶液中，于60℃恒温水浴中反应24h后取出PbS薄膜，以二次水冲洗干净，烘干即可得到Ag2S-Pb3(PO4)2薄膜。
(6)于20mL的玻璃瓶中依次加入300μL浓度为0.2mol/L、pH为6的HAc-NaAc缓冲溶液，25μL质量分数为1％的氯金酸溶液，80μL浓度为0.2mol/L的十六烷基三甲基氯化铵溶液，7mL二次水，制得生长Au-Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的Ag2S-Pb3(PO4)2薄膜置正面朝上放入该生长液中，于60℃恒温水浴反应3h后取出，以二次水冲洗干净，烘干即可得到Au-Ag2S-Pb3(PO4)2纳米异质结薄膜。
图1为本实施例中所得Au-Ag2Se-Pb3(PO4)2纳米异质结薄膜的扫描电子纤维镜(SEM)照片，由图1可见Au-Ag2S-Pb3(PO4)2纳米异质结薄膜微观上呈现出由粗细均匀的棒状形成的网状结构。
图2为本实施例中所得Au-Ag2Se-Pb3(PO4)2纳米异质结薄膜的X射线衍射(XRD)图谱，由图2可见该薄膜中含有Au、Ag2S和Pb3(PO4)2。
实施例2
(1)将事先裁好的1cm×3cm的ITO导电玻璃电极，分别经由分析纯丙酮、分析纯乙醇和二次水超声清洗5min，干燥后用万能表测出导电面待用。
(2)依次量取1mL浓度为0.2mol/L Pb(NO3)2溶液、1mL浓度为0.2mol/L EDTA溶液、3.5mL浓度为0.3mol/L Na2S2O3溶液和4mL浓度为1.25mol/L Na2SO4溶液置于20mL烧杯中均匀混合，制得电沉积PbS薄膜的底液。
(3)在步骤(2)中制得的电沉积PbS薄膜的底液中建立三电极体系，其中，工作电极为步骤(1)中制得的导电玻璃电极，对电极为Pt电极，参比电极为Ag/AgCl电极，用循环伏安法进行电沉积，电位扫描范围为-1.0V～0V，扫描速度为0.05V/s，扫描段数为40。电沉积结束后，将电极取出并用二次水冲洗干净，空气烘干后即可得到PbS薄膜。
(4)将步骤(3)制得的PbS薄膜置于250℃管式炉，氮气氛围中加热1h，待管式炉等却后将PbS薄膜取出。
(5)于20mL的玻璃瓶中依次加入700μL浓度为0.02mol/L的Na2HPO4溶液，80μL浓度为0.01mol/L的AgNO3溶液，100μL质量分数为1％的十二烷基苯磺酸钠溶液，7mL二次水，制得生长Ag2S-Pb3(PO4)2薄膜的生长液。将步骤(4)中制得的PbS薄膜正面朝上放入生长溶液中，于60℃恒温水浴中反应24h后取出PbS薄膜，以二次水冲洗干净，烘干即可得到Ag2S-Pb3(PO4)2薄膜。
(6)于20mL的玻璃瓶中依次加入300μL浓度为0.2mol/L、pH为6的HAc-NaAc缓冲溶液，25μL质量分数为1％的氯金酸溶液，80μL浓度为0.2mol/L的十六烷基三甲基氯化铵溶液，7mL二次水，制得生长Au-Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的Ag2S-Pb3(PO4)2薄膜置正面朝上放入该生长液中，于60℃恒温水浴反应0.5h后取出，以二次水冲洗干净，烘干即可得到Au-Ag2S-Pb3(PO4)2纳米异质结薄膜。
实施例3
(1)将事先裁好的1cm×3cm的ITO导电玻璃电极，分别经由分析纯丙酮、分析纯乙醇和二次水超声清洗5min，干燥后用万能表测出导电面待用。
(2)依次量取1mL浓度为0.2mol/L Pb(NO3)2溶液、1mL浓度为0.2mol/L EDTA溶液、3.5mL浓度为0.3mol/L Na2S2O3溶液和4mL浓度为1.25mol/L Na2SO4溶液置于20mL烧杯中均匀混合，制得电沉积PbS薄膜的底液。
(3)在步骤(2)中制得的电沉积PbS薄膜的底液中建立三电极体系，其中，工作电极为步骤(1)中制得的导电玻璃电极，对电极为Pt电极，参比电极为Ag/AgCl电极，用循环伏安法进行电沉积，电位扫描范围为-1.0V～0V，扫描速度为0.05V/s，扫描段数为120，电沉积结束后，将电极取出并用二次水冲洗干净，空气烘干后即可得到PbS薄膜。
(4)将步骤(3)制得的PbS薄膜置于250℃管式炉，氮气氛围中加热1h，待管式炉等却后将PbS薄膜取出。
(5)于20mL的玻璃瓶中依次加入700μL浓度为0.02mol/L的Na2HPO4溶液，80μL浓度为0.01mol/L的AgNO3溶液，100μL质量分数为1％的十二烷基苯磺酸钠溶液，7mL二次水，制得生长Ag2S-Pb3(PO4)2薄膜的生长液。将步骤(4)中制得的PbS薄膜正面朝上放入生长溶液中，于60℃恒温水浴中反应24h后取出PbS薄膜，以二次水冲洗干净，烘干即可得到Ag2S-Pb3(PO4)2薄膜。
(6)于20mL的玻璃瓶中依次加入300μL浓度为0.2mol/L、pH为6的HAc-NaAc缓冲溶液，25μL质量分数为1％的氯金酸溶液，80μL浓度为0.2mol/L的十六烷基三甲基氯化铵溶液，7mL二次水，制得生长Au-Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的Ag2S-Pb3(PO4)2薄膜置正面朝上放入该生长液中，于60℃恒温水浴反应24h后取出，以二次水冲洗干净，烘干即可得到Au-Ag2S-Pb3(PO4)2纳米异质结薄膜。
以上仅是本发明的优选实施例，本发明的保护范围并不仅局限于上述实施例。

Claims (2)

1.一种制备金-硫化银-磷酸铅异质结纳米薄膜的方法，其特征在于具体步骤为：
(1)将事先裁好的ITO导电玻璃电极，分别经由分析纯丙酮、分析纯乙醇和二次水超声清洗5min，干燥后用万能表测出导电面待用；
(2)依次量取1mL浓度为0.2mol/L Pb(NO3)2、1mL浓度为0.2mol/L EDTA、3.5mL浓度为0.3mol/L Na2S2O3和4mL浓度为1.25mol/L Na2SO4溶液置于20mL烧杯中均匀混合，制得电沉积PbS薄膜的底液；
(3)在步骤(2)中制得的电沉积PbS薄膜的底液中建立三电极体系，其中，工作电极为步骤(1)中制得的导电玻璃电极，对电极为Pt电极，参比电极为Ag/AgCl电极，用循环伏安法进行电沉积，电位扫描范围为-1.0V～0V，扫描速度为0.05V/s，扫描段数为40～120，电沉积结束后，将电极取出并用二次水冲洗干净，空气烘干后即可得到PbS薄膜；
(4)将步骤(3)制得的PbS薄膜置于250℃管式炉，氮气氛围中加热1h，待管式炉等却后将PbS薄膜取出；
(5)于20mL的玻璃瓶中依次加入700μL浓度为0.02mol/L的Na2HPO4溶液，80μL浓度为0.01mol/L的AgNO3溶液，100μL质量分数为1％的十二烷基苯磺酸钠溶液，7mL二次水，制得生长Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的PbS薄膜正面朝上放入生长溶液中，于60℃恒温水浴中反应24h后取出PbS薄膜，以二次水冲洗干净，烘干即可得到Ag2S-Pb3(PO4)2薄膜；
(6)于20mL的玻璃瓶中依次加入300μL浓度为0.2mol/L、pH为6的HAc-NaAc缓冲溶液，15μL～100μL质量分数为1％的氯金酸溶液，80μL浓度为0.2mol/L的十六烷基三甲基氯化铵溶液，7mL二次水，制得生长Au-Ag2S-Pb3(PO4)2薄膜的生长液，将步骤(4)中制得的Ag2S-Pb3(PO4)2薄膜置正面朝上放入该生长液中，于60℃恒温水浴反应0.5h～24h后取出，以二次水冲洗干净，烘干即可得到Au-Ag2S-Pb3(PO4)2纳米异质结薄膜。
2.根据权利要求1所述的制备方法，其特征在于所述步骤(1)中的ITO导电玻璃为掺杂氧化铟锡的玻璃电极。
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