CN108993538B - 一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法 - Google Patents
一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法，包括：二氧化钛纳米纤维的制备；将透明溶液注入注射器中，用静电纺丝机器纺成纳米线；将纳米线转移至管式炉在空气气氛下，以5℃/min升温到500℃，保温2h，然后研磨成粉；量白色粉末分散到去离子水中，超声2h，然后加入铼酸铵，硫脲和盐酸羟胺，搅拌2h，转移至水热釜中在220℃下反应24h，最后用去离子水清洗若干次，烘干。
Description
技术领域
本发明属于光催化技术领域，具体涉及一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法。
背景技术
利用光催化技术产氢是当下被认为最理想的解决人类能源危机和环境污染问题的方法，光催化材料也是近几十年来研究的热点。TiO2作为最传统的光催化材料，主要有以下优点：1.Ti和O元素储量丰富，而且TiO2合成方法简单，廉价易得。2.有良好的物理化学稳定性，结晶性好。3.带隙位置合适，能够在理论上满足光催化分解水所需要的价、导带位置。但是TiO2这种光催化材料也有一些缺点：1.带隙太宽，对于太阳光的吸收仅限于紫外光区域。2.光生载流子复合率高，不能有效地分离从而参与到氧化还原反应中。3.表面活性位点较少，不利于催化剂表面吸附反应物质以及载流子参与到反应中。
大量文献表明，人们对于TiO2的传统改性手段主要包括掺杂和贵金属沉积这两个方面。掺杂主要就是为了减小TiO2的带隙宽度，从而提高其光谱响应范围。而贵金属沉积主要是因为贵金属通过光沉积到催化剂表面时，其吸附氢原子的吉布斯自由能几乎为零，并且为催化剂表明提供反应活性位点，从而极大地提高TiO2的光催化性能。近些年研究人员对TiO2的改性主要集中在纳米结构设计和与其他光催化材料复合这两个方面。对TiO2进行纳米结构设计是通过采用模板法或者加入表面形态调控剂，并利用其优良的结晶性制出一维线状、二维片状或者三维多孔结构，从而增大比表面积，暴露更多活性位点。与其他光催化材料复合，目的是为了通过带隙位置的匹配以及结合两种材料的优势达到协同效应。
上文中提到的对于TiO2改性的研究中，设计纳米结构并且与其他光催化材料复合是比较有效的方法。由于对TiO2进行结构设计不仅为了增大其比表面积，暴露更多活性位点，还为了在其表面负载其他的光催化材料，因此我们采用静电纺丝制成的多孔TiO2纳米纤维，这种结构的TiO2表面有很多缝隙以及缺陷而且比表面积较大，可以利用这些特征负载其他光催化材料。最近的研究表明与TiO2复合的光催化材料中，过渡族金属硫化物因其具有独特的二维片层结构和优异的光电特性而广泛关注。以MoS2为代表的过渡族金属硫化物带隙宽度适中，且少层结构的带隙位置与TiO2的带隙位置较为匹配，最重要的是这种独特的二维片层结构边缘位置会暴露大量的活性位点，会大大提高光催化材料的性能。但是大部分过渡族金属硫化物都不是直接带隙半导体，带隙宽度以及位置会随着片层的改变而改变，而且最稳定的2H相在活性位点数量和导电性方面都不如亚稳态1T相优异，因此我们仍然需要对过渡族金属硫化物进行更深的探究。在此过程中发现一种独特的过渡族金属硫化物，ReS2，这种材料是直接带隙半导体，而且稳态为1T相，理论上非常适合作为光催化材料。目前还没有报道将ReS2与TiO2两者复合作为光催化材料的文献和专利。
发明内容
为了解决单一光催化材料二氧化钛存在的问题，本发明的目的是提供一种将二氧化钛纳米纤维与片状二硫化铼复合的方法，提高二氧化钛的产氢性能，本发明的技术方案如下：
一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法，包括下列步骤：
1)二氧化钛纳米纤维的制备：以聚乙烯吡咯烷酮为粘结剂，以钛酸异丙酯为钛盐，将粘结剂溶于无水乙醇中，将钛盐溶于相同体积的无水乙醇和冰乙酸的混合溶液(1:1)中，粘结剂与钛盐的质量配比为0.45：1.5，再将两者混合均匀，得到透明溶液。
2)将透明溶液注入注射器中，用静电纺丝机器纺成纳米线；
3)将纳米线转移至管式炉在空气气氛下，以5℃/min升温到500℃，保温2h，然后研磨成粉。
3)将上述步骤得到的一定量白色粉末分散到去离子水中，超声2h，然后加入铼酸铵，硫脲和盐酸羟胺(质量比为4:5:4)，搅拌2h，转移至水热釜中在220℃下反应24h，最后用去离子水清洗若干次，烘干。
综上所述，本发明的核心是制备二氧化钛纳米纤维，再通过水热的方式得到ReS2纳米片修饰的TiO2纳米纤维复合材料。与现有的技术相比，本发明的优点在于：
(1)本发明制备的二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料充分结合了两种材料的优势，从光吸收和载流子分离能力这两个方面对材料进行改善，并且是首次将二者结合制备成复合材料，具有独创性。
(2)本发明制备的二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料，显著地提高了二氧化钛的产氢性能，并且在降解污染物方面也表现出良好的性能
(3)本发明制备设备简单，工艺简便。
(4)本发明可靠性高，可重复性强，有良好的应用前景。
附图说明
图1为本发明实施例1所制备的二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的XRD图谱。
图2为本发明实施例1所制备的二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的SEM图谱。
图3为本发明实施例1所制备的二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的TEM图谱。
具体实施方式
实施例1
将0.45g的聚乙烯吡咯烷酮溶于6ml无水乙醇中，搅拌2h，将1.5g钛酸异丙酯溶于3ml无水乙醇和3ml冰乙酸的混合溶液(1:1)中，搅拌2h，然后将上述两个溶液混在一起搅拌2h得到透明溶液，将透明溶液注入注射器中，用静电纺丝机器纺成纳米纤维，电极电压为10kV，电极距离为15cm，挤进速度为0.5ml/h，然后将纳米纤维在空气气氛中，以5℃/min升温到500℃，保温2h，得到白色粉末。将100mg白色粉末分散在30ml去离子水中，超声2h，然后加入43mg铼酸铵，42mg盐酸羟胺，54.4mg硫脲(4:5:4)，搅拌2h后转移至水热釜中，在220℃下反应24h，最后将产物用去离子水清洗三次，烘干。
实施例2
将0.45g的聚乙烯吡咯烷酮溶于6ml无水乙醇中，搅拌2h，将1.5g钛酸异丙酯溶于3ml无水乙醇和3ml冰乙酸的混合溶液(1:1)中，搅拌2h，然后将上述两个溶液混在一起搅拌2h得到透明溶液，将透明溶液注入注射器中，用静电纺丝机器纺成纳米纤维，电极电压为10kV，电极距离为15cm，挤进速度为0.5ml/h，然后将纳米纤维在空气气氛中，以5℃/min升温到500℃，保温2h，得到白色粉末。将100mg白色粉末分散在30ml去离子水中，超声2h，然后加入21.5mg铼酸铵，21mg盐酸羟胺，27.2mg硫脲(4:5:4)，搅拌2h后转移至水热釜中，在220℃下反应24h，最后将产物用去离子水清洗三次，烘干。
实施例3
将0.45g的聚乙烯吡咯烷酮溶于6ml无水乙醇中，搅拌2h，将1.5g钛酸异丙酯溶于3ml无水乙醇和3ml冰乙酸的混合溶液(1:1)中，搅拌2h，然后将上述两个溶液混在一起搅拌2h得到透明溶液，将透明溶液注入注射器中，用静电纺丝机器纺成纳米纤维，电极电压为10kV，电极距离为15cm，挤进速度为0.5ml/h，然后将纳米纤维在空气气氛中，以5℃/min升温到500℃，保温2h，得到白色粉末。将100mg白色粉末分散在30ml去离子水中，超声2h，然后加入161mg铼酸铵，125mg盐酸羟胺，205mg硫脲(4:5:4)，搅拌2h后转移至水热釜中，在220℃下反应24h，最后将产物用去离子水清洗三次，烘干。
Claims (1)
1.一种二硫化铼纳米片/二氧化钛纳米纤维复合光催化材料的制备方法，包括下列步骤：
1)二氧化钛纳米纤维的制备：以聚乙烯吡咯烷酮为粘结剂，以钛酸异丙酯为钛盐，将粘结剂溶于无水乙醇中，将钛盐溶于相同体积的无水乙醇和冰乙酸的1:1混合溶液中，粘结剂与钛盐的质量配比为0.45：1.5，再将两种溶液混合均匀，得到透明溶液；
2)将透明溶液注入注射器中，用静电纺丝机器纺成纳米线；
3）将纳米线转移至管式炉在空气气氛下，以5℃/min升温到500℃，保温2h，然后研磨成粉；
4)将上述步骤得到的一定量白色粉末分散到去离子水中，超声2h，然后加入质量比为4:5:4的铼酸铵，硫脲和盐酸羟胺，搅拌2h，转移至水热釜中在220℃下反应24h，最后用去离子水清洗若干次，烘干。
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| CN110357147B (zh) * | 2019-07-23 | 2020-08-28 | 中国科学技术大学 | 二硫化铼-二硫化锡异质纳米材料、其制备方法与应用 |
| CN111060568B (zh) * | 2019-12-18 | 2022-02-18 | 温州医科大学 | 基于二硫化铼纳米片构建三型胶原蛋白光电化学传感器的方法及应用 |
| CN111495391A (zh) * | 2020-05-22 | 2020-08-07 | 浙江大学 | 一种复合光催化剂及其制备方法与应用 |
| CN113224301A (zh) * | 2021-04-30 | 2021-08-06 | 广州大学 | 一种氧化镍复合材料及其制备方法和应用 |
| CN113634266B (zh) * | 2021-07-05 | 2023-03-21 | 宁波工程学院 | 一种ReS2超薄纳米片负载的Ta3N5空心纳米球复合材料及其应用 |
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