CN107988615B - 一种氮化碳修饰ZnO/CdS光阳极材料的制备及应用 - Google Patents
一种氮化碳修饰ZnO/CdS光阳极材料的制备及应用 Download PDFInfo
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Abstract
本发明公开了一种氮化碳修饰ZnO/CdS光阳极材料的制备方法，及其在光电解水中的应用。该方法采用一步水热法制备氮化碳(g‑C3N4)修饰的ZnO膜，离子吸附法制备CdS纳米颗粒，经过热处理，得到g‑C3N4修饰的ZnO/CdS光阳极，提高其光电流。由于该方法采用了一步水热法制备g‑C3N4/ZnO膜，且常温下进行离子吸附CdS，反应容易控制，且吸附效果较好。通过该方法制备的g‑C3N4修饰的ZnO/CdS光阳极，其光电转化性能相比纯ZnO提高近30倍。
Description
技术领域
本发明属于光阳极修饰技术领域，特别涉及氮化碳修饰ZnO/CdS光阳极的方法。
背景技术
为了满足对能源和环境问题日益增长的需求，太阳能光解水制备氢气作为一种高效且干净的产氢方式受到了极大的关注。目前主要的生产氢气的方式是天然气的蒸汽转化，但是这将消耗大量资源，并且产生二氧化碳废气，因此利用半导体纳米结构器件进行光解水制备氢气具有一定优势。在光电化学(PEC) 电池中，为了清洁和实用的氢气生产，需要廉价，高效和稳定的半导体光电分解水来制备大量氢气。氧化锌(ZnO)作为常温下具有宽带隙(～3.3eV)的n 型氧化物半导体被深入研究，由于其独特的电化学特性，高电子迁移率，低成本和无毒性，广泛应用于电子器件，太阳能电池，传感器等领域。然而，ZnO 的宽带隙和光生载流子的快速重组，导致光吸收较弱和光电转换效率低，阻碍了ZnO在光电催化中的应用。
为了解决ZnO对太阳光的有限吸收，采用了不同的方法对半导体ZnO进行改善，增加其在可见光区域的吸收。如复合贵金属纳米颗粒(Au Ag)；掺杂金属或非金属离子，Hanhong Chen等人用金属有机气相沉积法制备Ga掺杂的 ZnO(GZO)薄膜，Ga的掺杂成功的提高了材料的单色光光电转换效率。Lijuan Luo等人制备了非金属F掺杂的ZnO棱形阵列，掺杂后ZnO的电子寿命增加，电子传输电阻降低，光电转换效率增大。Lanlan Lu等人研究一系列稀土元素(La, Ce,Nd,Sm和Gd)对ZnO光电性能的影响，发现稀土能钝化ZnO阳极的表面态，其中Gd的掺杂成功的提高了电池的光电转换效率；负载助催化剂MoS2或新型催化剂(BiOBr,BiOI,g-C3N4)；沉淀带隙窄的量子点,如CdS、CdSe、PbS等。在这其中,CdS因其具有与ZnO相似的晶格和较窄的带隙，可以吸收更多的可见光。另一方面,可以很容易通过化学沉积方法得到CdS，用作于各种光阳极的表面改性，从而提高光电性能。由于CdS容易氧化，大部分的复合光阳极需要在 400-600℃的马弗炉中，氮气或者氩气氛围下退火处理。然而，ZnO/CdS仍然存在着电子空穴对复合，且光电催化效率低的问题，这就限制了总体光电制氢效率。
因此，需要寻找一种简单易操作的修饰ZnO光阳极的方法来提高ZnO的光电性能。
发明内容
本发明目的在于提供一种氮化碳修饰ZnO/CdS光阳极材料的方法，提高作为光阳极材料的ZnO膜的光电性能。
为达上述目的，本发明采用如下技术方案：
一步水热合成及离子吸附的方法，使ZnO膜复合C3N4及CdS，提高其光电性能，包括以下步骤：
步骤1)水热合成g-C3N4/ZnO薄膜可以采用掺杂氟的二氧化锡导电玻璃(FTO)，以硝酸锌的水溶液为反应溶液,调节pH，搅拌均匀，在一定温度下水热合成，并经过热处理得到g-C3N4/ZnO薄膜。
步骤2)离子吸附CdS采用硝酸镉的乙醇溶液和硫化钠的甲醇溶液，将 g-C3N4/ZnO薄膜的导电玻璃分别浸泡在上述两种溶液中各30s，若干循环后，得到g-C3N4/ZnO/CdS光阳极薄膜材料，并对其进行热处理。
进一步的，硝酸锌溶液的浓度为0.04mol/L。
进一步的，g-C3N4溶液的浓度为2mg/ml。
进一步的，水热合成温度为80℃。
进一步的，离子吸附CdS的循环次数为2-10次。
与现有技术相比，本发明的效果及优点是：
(1)一步水热法合成g-C3N4/ZnO膜，操作简便且易于大量制备；
(2)常温下进行吸附，得到g-C3N4/ZnO/CdS的复合膜，较高提高了ZnO 膜的光电流，操作简便并降低了能源消。
由上述优点可见，本发明对提高作为光阳极材料的ZnO膜的光电性能有重要意义。
附图说明
图1实施例 1中，ZnO复合g-C3N4及CdS前后的光电流图。
具体实施方式
以下通过具体实施例结合附图详细说明本发明的技术及特点，但这些实施例并非用以限定本发明的保护范围。
一步水热合成及离子吸附的方法，使ZnO膜复合C3N4及CdS，提高其光电性能，包括以下步骤：
步骤1)水热合成g-C3N4/ZnO薄膜可以采用掺杂氟的二氧化导电玻璃(FTO)，以硝酸锌的水溶液为反应溶液,调节pH，搅拌均匀，在一定温度下水热合成，并经过热处理得到g-C3N4/ZnO薄膜。
步骤2)离子吸附CdS采用硝酸镉的乙醇溶液和硫化钠的甲醇溶液，将 g-C3N4/ZnO薄膜的导电玻璃分别浸泡在上述两种溶液中各30s，若干循环后，得到g-C3N4/ZnO/CdS光阳极薄膜材料，并对其进行热处理。
进一步的，硝酸锌溶液的浓度为0.04mol/L。
进一步的，g-C3N4溶液的浓度为2mg/ml。
进一步的，水热合成温度为80℃。
进一步的，离子吸附CdS的循环次数为5次。
Claims (5)
1.一种g-C3N4修饰ZnO/CdS光阳极材料的方法，其特征在于，采用一步水热法，使水热合成ZnO膜的过程中负载g-C3N4，常温下进行离子吸附CdS，提高其光电性能，其特征在于，包括以下步骤：
步骤1)水热合成g-C3N4/ZnO薄膜采用掺杂氟的二氧化锡导电玻璃(FTO)，以硝酸锌的水溶液为反应溶液， 调节pH，搅拌均匀，在一定温度下水热合成，并经过热处理得到g-C3N4/ZnO薄膜；
步骤2)离子吸附CdS采用硝酸镉的乙醇溶液和硫化钠的甲醇溶液，将g-C3N4/ZnO薄膜的导电玻璃分别浸泡在上述两种溶液中各30s，若干循环后，得到g-C3N4/ZnO/CdS光阳极薄膜材料，并对其进行热处理。
2.如权利要求1所述的g-C3N4修饰ZnO/CdS光阳极材料的方法，其特征在于：硝酸锌溶液的浓度为0.04mol/L。
3.如权利要求1所述的g-C3N4修饰ZnO/CdS光阳极材料的方法，其特征在于：g-C3N4溶液的浓度为2mg/mL 。
4.如权利要求1所述的g-C3N4修饰ZnO/CdS光阳极材料的方法，其特征在于：水热合成温度为80℃。
5.如权利要求1所述的g-C3N4修饰ZnO/CdS光阳极材料的方法，其特征在于：离子吸附CdS的循环次数为2-10次。
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