CN108977848B - 一种Cu2O基多层光电阴极薄膜材料的制备方法 - Google Patents

一种Cu2O基多层光电阴极薄膜材料的制备方法 Download PDF

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CN108977848B
CN108977848B CN201810903289.6A CN201810903289A CN108977848B CN 108977848 B CN108977848 B CN 108977848B CN 201810903289 A CN201810903289 A CN 201810903289A CN 108977848 B CN108977848 B CN 108977848B
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马艺
张婉
尹志广
王子豪
王奕岚
王增林
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Shaanxi Normal University
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Abstract

本发明公开了一种Cu2O基多层光电阴极薄膜材料的制备方法，通过电化学沉积Cu2O后的FTO导电玻璃上先磁控溅射沉积一层金属或金属的氧化物纳米层，然后用含S2‑的水溶液浸渍并退火，或先将沉积Cu2O后的FTO导电玻璃用含S2‑的水溶液浸渍并退火，再磁控溅射沉积一层金属或金属的氧化物纳米层，最终得到Cu2O基多层光电阴极薄膜材料。本发明的制备过程简单，原材料价格低廉，降低了生产成本，同时提高了Cu2O的光电催化活性和稳定性，在光电催化分解水领域具有潜在的应用。

Description

一种Cu2O基多层光电阴极薄膜材料的制备方法
技术领域
本发明属于光电催化分解水技术领域，具体涉及一种Cu2O基光电阴极薄膜材料的制备方法。
背景技术
近几年来，越来越严峻的环境问题使得人们迫切的寻找新型的清洁可在生能源来替代传统的化石燃料。太阳能是目前最理想的替代能源，在众多的太阳能利用方式中，光电催化水分解技术因为将太阳能和氢能有效的进行了结合，因此是目前的研究热点。
Cu2O的禁带宽度约为2.2eV，可直接被可见光激发，其原料为无毒、储量丰富且价格低廉的Cu，因此Cu2O被广泛应用于光电催化领域，同时Cu2O也存在比较明显的缺点，由于其还原电位低于氢离子的还原电位，因此在水溶液中很容易被还原成Cu，并且光生载流子的复合率比较高，所以如何提高Cu2O的催化活性和稳定性是亟待解决的问题。
发明内容
本发明的目的是提供一种高催化活性和高稳定性的Cu2O基多层光电阴极薄膜材料的制备方法。
针对上述目的，本发明所采用的技术方案由下述步骤组成：
1、在清洗干净的FTO导电玻璃上离子溅射沉积一层Au纳米层，然后电化学沉积一层Cu2O。
2、在沉积Cu2O后的FTO导电玻璃上先磁控溅射沉积一层金属或金属的氧化物纳米层，然后浸渍于含S2-的水溶液中，浸渍完后退火，得到Cu2O基多层光电阴极薄膜材料；或先将沉积Cu2O后的FTO导电玻璃浸渍于含S2-的水溶液中，浸渍完后退火，然后再磁控溅射沉积一层金属或金属的氧化物纳米层，得到Cu2O基多层光电阴极薄膜材料。
上述步骤1中，电化学沉积Cu2O的参比电极选用Ag/AgCl(饱和KCl)，铂片为对电极，沉积Au纳米层的FTO导电玻璃为工作电极，电解质溶液是含0.2～0.5 mol/L硫酸铜和1～6mol/L乳酸的水溶液，且该水溶液通过氢氧化钠调节pH为8～ 14，优选电解质溶液是含0.3～0.4mol/L硫酸铜和3～4mol/L乳酸的水溶液，且该水溶液通过氢氧化钠调节pH为12～13；采用恒电位电化学沉积Cu2O，所施加的电压为-0.3～-0.8V，在25～60℃的条件下沉积200～1000s。
上述步骤2中，所述的金属为Mn、Ni、Co或F，金属或金属的氧化物纳米层的厚度为5～20nm，磁控溅射沉积金属或金属的氧化物纳米层的Ar压力为1～5 mTorr，沉积功率为10～50W，沉积时间为20s～5min；所述含S2-的水溶液为硫化钠、硫脲、硫化铵中任意一种或两种以上的水溶液，其中S2-浓度为1mmol/L～ 0.1mol/L，浸渍时间控制在20s～5min；所述退火温度为200～300℃，退火时间为 1～3h。
本发明通过在Cu2O表面沉积一层金属或金属的氧化物来提高催化活性，通过将电极浸渍于含S2-的溶液中，利用离子交换的方法生成一层Cu2S，由于Cu2S的导带电位相对于Cu2O更正，有利用光生电子从Cu2O层迁移至Cu2S层，促进了光生电子和空穴的分离，提高了Cu2O的稳定性。
附图说明
图1是Cu2O、Cu2S/Cu2O、Ni/Cu2O-2min、Ni/Cu2S/Cu2O-2min、Cu2S/Ni/Cu2O-2 min的XRD图。
图2是Cu2O、Cu2S/Cu2O、Ni/Cu2O-2min、Ni/Cu2S/Cu2O-2min、Cu2S/Ni/Cu2O-2 min的光电极I-V性能曲线。
图3是Cu2O、Cu2S/Cu2O、Ni/Cu2O-2min、Ni/Cu2S/Cu2O-2min、Cu2S/Ni/Cu2O-2 min的光电极稳定性曲线。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施例。
实施例1
1、将FTO导电玻璃切割成1cm×1.5cm的基片后，以导电面朝上的方式以60°斜靠于聚四氟乙烯的凹槽内，用丙酮超声清洗15min后，再用乙醇超声清洗15min，最后用水超声清洗15min，转移至烘箱内烘干。然后通过离子溅射的方式，在FTO 导电玻璃的导电面沉积一层Au纳米层，时间控制在80s。再利用三电极体系进行恒电位电化学沉积Cu2O，参比电极选用Ag/AgCl(饱和KCl)，铂片为对电极，沉积Au纳米层的FTO导电玻璃为工作电极，电解质溶液是含0.3mol/L硫酸铜和3 mol/L乳酸的水溶液，且该水溶液通过氢氧化钠调节pH为12，所施加的电压为-0.6 V，在50℃的条件下沉积500s。
2、以高纯Ni靶为靶材，采用磁控溅射沉积法在沉积Cu2O后的FTO导电玻璃上沉积一层Ni纳米层，沉积条件为：Ar压力1.5mTorr、沉积功率20W、沉积时间20s。然后将沉积Ni纳米层后的FTO导电玻璃浸渍于50mmol/L硫化钠水溶液中，时间控制在90s，浸渍完后于200℃退火2小时，得到Cu2O基多层光电阴极薄膜材料，记为Cu2S/Ni/Cu2O-20s。
实施例2
本实施例的步骤2中，沉积时间为1min，其他步骤与实施例1相同，得到Cu2O 基多层光电阴极薄膜材料，记为Cu2S/Ni/Cu2O-1min。
实施例3
本实施例的步骤2中，沉积时间为2min，其他步骤与实施例1相同，得到Cu2O 基多层光电阴极薄膜材料，记为Cu2S/Ni/Cu2O-2min。
实施例4
本实施例的步骤2中，沉积时间为2.5min，其他步骤与实施例1相同，得到 Cu2O基多层光电阴极薄膜材料，记为Cu2S/Ni/Cu2O-2.5min。
实施例5
本实施例的步骤1与实施例1相同。在步骤2中，先将沉积Cu2O后的FTO导电玻璃浸渍于50mmol/L硫化钠水溶液中，时间控制在90s，浸渍完后于200℃退火 2小时，然后以高纯Ni靶为靶材，采用磁控溅射沉积法沉积一层Ni纳米层，沉积条件为：Ar压力1.5mTorr、沉积功率20W、沉积时间20s，得到Cu2O基多层光电阴极薄膜材料，记为Ni/Cu2S/Cu2O-20s。
实施例6
本实施例的步骤2中，沉积时间为1min，其他步骤与实施例5相同，得到Cu2O 基多层光电阴极薄膜材料，记为Ni/Cu2S/Cu2O-1min。
实施例7
本实施例的步骤2中，沉积时间为2min，其他步骤与实施例5相同，得到Cu2O 基多层光电阴极薄膜材料，记为Ni/Cu2S/Cu2O-2min。
实施例8
本实施例的步骤2中，沉积时间为2.5min，其他步骤与实施例5相同，得到 Cu2O基多层光电阴极薄膜材料，记为Ni/Cu2S/Cu2O-2.5min。
实施例9
在实施例1～8中，所用的镍靶用钴靶替换，其他步骤与相应实施例相同。
发明人对实施例1～8中得到的Cu2O基多层光电阴极薄膜进行了XRD以及光电性能的测定，结果见图1～3。图1为不同电极的XRD图谱，除去FTO的衬底峰，所有的衍射峰均为Cu2O相，说明Cu2S和Ni的担载量很少或是以无定型态存在。图2为单独Cu2O光电阴极与Cu2O基多层光电阴极的LSV曲线，从图中可以看出在电压为-0.8V时，单独Cu2O的电流密度为-1.89mA/cm2，Cu2S/Cu2O的电流密度为-1.99mA/cm2，Ni/Cu2O-2min的电流密度为-2.38mA/cm2，Ni/Cu2S/Cu2O-2min 的电流密度为-3.29mA/cm2，Cu2S/Ni/Cu2O-2min的电流密度为-3.37mA/cm2，可以看出，每担载一层催化剂后对催化活性均有提高。图3是对一系列电极进行了稳定性测试，从图中可以看出单独Cu2O起始时的电流密度为-1.02mA/cm2，500s后变为-0.127mA/cm2，衰减量为87.5％，Cu2S/Cu2O起始时的电流密度为-1.03mA/cm2， 500s后变为-0.55mA/cm2，衰减量为46.6％，Ni/Cu2O-2min起始时的电流密度为-1.36 mA/cm2，500s后变为-0.46mA/cm2，衰减量为66.5％，Ni/Cu2S/Cu2O-2min起始时的电流密度为-2.01mA/cm2，500s后变为-1.02mA/cm2，衰减量为49.3％，可以看出 Cu2S层的加入对稳定性的提高有很大的改善，原因是Cu2S的导带电位相对于Cu2O 更正，有利用光生电子从Cu2O层迁移至Cu2S层，促进了光生电子和空穴的分离，提高了Cu2O的稳定性。

Claims (7)

1.一种Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于该方法由下述步骤组成：
（1）在清洗干净的FTO导电玻璃上离子溅射沉积一层Au纳米层，然后电化学沉积一层Cu2O；
（2）在沉积Cu2O后的FTO导电玻璃上先磁控溅射沉积一层厚度为5～20 nm金属或金属的氧化物纳米层，然后浸渍于含S2-的水溶液中，浸渍完后退火，得到Cu2O基多层光电阴极薄膜材料；
上述的金属为Mn、Ni、Co或Fe。
2.根据权利要求1所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：步骤（2）中，所述磁控溅射沉积金属或金属的氧化物纳米层的Ar压力为1～5 mTorr，沉积功率为10～50 W，沉积时间为20 s～5 min。
3.根据权利要求1所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：步骤（2）中，所述含S2-的水溶液为硫化钠、硫脲、硫化铵中任意一种或两种以上的水溶液，其中S2-浓度为1 mmol/L～0.1 mol/L，浸渍时间控制在20 s～5 min。
4.根据权利要求1所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：步骤（2）中，所述退火温度为200～300℃，退火时间为1～3h。
5.根据权利要求1～4任意一项所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：步骤（1）中，电化学沉积Cu2O的参比电极选用Ag/AgCl/饱和KCl，铂片为对电极，沉积Au纳米层的FTO导电玻璃为工作电极，电解质溶液是含0.2～0.5 mol/L硫酸铜和1～6mol/L乳酸的水溶液，且该水溶液通过氢氧化钠调节pH为8～14。
6.根据权利要求5所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：电解质溶液是含0.3～0.4 mol/L硫酸铜和3～4 mol/L乳酸的水溶液，且该水溶液通过氢氧化钠调节pH为12～13。
7.根据权利要求5所述的Cu2O基多层光电阴极薄膜材料的制备方法，其特征在于：采用恒电位电化学沉积Cu2O，所施加的电压为-0.3～-0.8 V，在25～60 ℃的条件下沉积200～1000 s。
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