CN106311216A - 一种以二维材料作为制氧助催化剂的复合光催化剂及其制备方法 - Google Patents
一种以二维材料作为制氧助催化剂的复合光催化剂及其制备方法 Download PDFInfo
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- 230000000694 effects Effects 0.000 abstract description 23
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 abstract description 13
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
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- 239000012153 distilled water Substances 0.000 description 2
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种以二维材料作为制氧助催化剂的复合光催化剂及其制备方法。以超薄二维层片状材料TiO2为助催化的WO3复合材料。TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%。利用浸渍法将二维层片材料TiO2悬浊液与WO3复合制备光催化剂TiO2纳米片/WO3。二维层片材料TiO2悬浊液的浓度为200~250ml/g,浸渍后在空气中200~500℃热处理2~6h,得到复合光催化剂TiO2纳米片/WO3。复合光催化剂应用于光催化水分解出氧半反应中。负载二维层片TiO2的WO3的出氧活性是未负载WO3活性的2倍,并且比常用助催化剂RuO2更加廉价高效。
Description
技术领域
本发明属于光催化技术领域,尤其是涉及一种以二维材料作为制氧助催化剂的复合光催化剂及其制备方法。
背景技术
直接利用光来驱动一系列重要化学反应的光催化在解决能源短缺和环境问题方面具有极大的潜力。光催化水分解是重要的人工光合成过程,而其中的水氧化过程是太阳能分解水的决速步骤和关键科学问题,它往往由于多电子转移困难以及快速的电荷重组等因素,导致水分解反应效率很低。有一些半导体本身具有一定的水分解出氧催化活性,但是催化效率和稳定性都受到局限。助催化剂可以有效促进光生载流子的分离、降低诸多反应的过电势,提高半导体本身的出氧催化活性,在光催化过程中起着举足轻重的作用。
应用于水分解出氧半反应的半导体催化剂主要有WO3,ZnO,BiVO4等,WO3由于其性能稳定,不发生光腐蚀,催化活性高被广泛应用于光催化分解水的出氧半反应中。另外,RuO2、IrO2等都是常见的水分解出氧助催化剂,但是他们的稀缺和高成本限制了大规模的应用,其水分解出氧的提升效率也依然有限。所以,开发廉价高效的助催化剂对于提高半导体本身的出氧活性有重大意义。
伴随着石墨烯等二维材料发现和发展,人们对二维材料的性质有了新的认识,其在光催化中有广阔的应用前景。TiO2单层纳米片材料研究已有20多年,液相剥离完的纳米片是一种厚度纳米级长度微米级的超薄高结晶度的二维材料,最重要的是,由于其特殊的二维结构,让他有很多不同于粉体的独特属性。低维化使材料本身带隙宽化,光学特性和电子特性都发生一定变化,在光催化领域有长远的研究价值。
本发明将这种二维层片材料作为助催化剂应用于以WO3为半导体的水分解出氧半反应中,复合后的新型光催化剂显著提高了WO3在光催化水分解中的出氧活性,其对WO3催化活性的提高作用比常用的出氧助催化剂RuO2更明显,并且TiO2相比较RuO2等助催化剂更廉价,成本更低。
发明内容
本发明提出一种以二维材料作为制氧助催化剂的复合光催化剂,即以超薄二维层片状材料TiO2为助催化的WO3复合材料,显著提高了光阳极WO3出氧反应的活性。
本发明的技术方案是:
一种以二维材料作为制氧助催化剂的复合光催化剂;以超薄二维层片状材料TiO2为助催化的WO3复合材料。
TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%。
本发明的复合光催化剂的制备方法,利用浸渍法将二维层片材料TiO2悬浊液与WO3复合制备光催化剂TiO2纳米片/WO3。
具体方法是:助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%,二维层片材料TiO2悬浊液的浓度为200~250ml/g,浸渍后在空气中200~500℃热处理2~6h,得到复合光催化剂TiO2纳米片/WO3。复合后的透射图见附图3。
所述的二维层片材料TiO2悬浊液用液相剥离法制得。用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌4~8周,最终得到TiO2纳米片悬浮液。
本发明的光催化剂应用于光催化水分解出氧半反应中。
具体说明如下:
一种以二维材料作为制氧助催化剂的复合光催化剂,应用于光催化水分解出氧半反应中。二维的助催化剂是一种超薄层片状TiO2,可以通过液相剥离法制得,呈现类石墨烯的形貌特征,具有很高的结晶度,层片材料厚度可达纳米级,长度微米级,由于特殊的二维尺寸会使带隙宽化,在光学和电学方面有独特的属性,研究表明,这种层片状TiO2可作为一种光催化领域中水分解出氧半反应的助催化剂,能够显著提高WO3的出氧活性。
所述的二维层片材料TiO2的X射线衍射图见附图1,层片材料的悬浊液XRD图一有明显的广泛衍射范围,是由于剥离的钛酸层片散射造成的,干燥后的层片材料的XRD图中有明显的(0k0)系列的布拉格衍射峰,代表着特有的层片结构。所述的二维层片材料TiO2的扫面图见附图2,可以明显看出TiO2层片材料有着类石墨烯的特殊形貌,表面存在褶皱,剥离后的层片材料很薄。
TiO2纳米片/WO3的光催化水分解产氧活性的测试:
将TiO2纳米片/WO3置于于光催化水分解反应装置中,加入0.85gAgNO3,注入270mL蒸馏水,密封,抽真空,以300W氙灯作为光源,L42滤光片滤掉紫外区域的光,只进行可见光部分的测试,光催化反应期间,每隔1h利用四通阀将反应后的气体注入气相色谱仪(岛津GC-2014)中分析光催化水分解的O2产物产量,即光催化水分解的产氧速率,所述复合光催化剂在光催化水分解的产氧效率明显高于WO3以及RuO2/WO3的产氧效率,产氧效率对比图见附图4,说明二维层状材料TiO2作为水分解出氧半反应的助催化剂有效提高了光阳极材料WO3的产氧活性。
本发明提出一种以二维材料作为制氧助催化剂的新型复合光催化剂,可应用于光催化技术领域中水分解出氧半反应。制备时将二维层片材料TiO2的悬浊液与WO3浸渍处理,合成复合光催化剂TiO2纳米片/WO3,热处理后对其进行可见光下水分解出氧活性的测试。以TiO2层片材料为制氧助催化剂的WO3出氧活性明显高于光阳极材料WO3的出氧活性,负载二维层片TiO2的WO3的出氧活性是未负载WO3活性的2倍,并且比常用助催化剂RuO2更加廉价高效。
附图说明
图1:实施例1中液相剥离法制备的TiO2层片材料的XRD图;
图2:实施例1中液相剥离法制备的TiO2层片材料的扫描电镜图;
图3:实施例4中复合光催化剂TiO2纳米片/WO3的透射电镜图;
图4:实施例7中复合光催化剂TiO2纳米片/WO3,RuO2/WO3,WO3在水分解中产氧效率对比图。
具体的实施方式
步骤方法如下:
1)二维层片材料TiO2悬浊液的制备:
用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌4~8周,最终得到TiO2纳米片悬浮液;
2)利用浸渍法制备复合光催化剂TiO2纳米片/WO3:
利用浸渍法将二维层片材料TiO2悬浊液与WO3进行复合,助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%,二维层片材料TiO2悬浊液的浓度200~250ml/g,浸渍后在空气中200~500℃热处理2~6h,得到目标复合光催化剂TiO2纳米片/WO3。
实施例1
用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌4周,最终得到TiO2纳米片悬浮液;
实施例2
用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌8周,最终得到TiO2纳米片悬浮液;
实施例3
用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌6周,最终得到TiO2纳米片悬浮液;
实施例4
利用浸渍法将二维层片材料TiO2悬浊液与WO3进行复合,助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%,二维层片材料TiO2悬浊液的浓度200ml/g,浸渍后在空气中200℃热处理2h,得到目标复合光催化剂TiO2纳米片/WO3。
实施例5
利用浸渍法将二维层片材料TiO2悬浊液与WO3进行复合,助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数0.5%,二维层片材料TiO2悬浊液的浓度250ml/g,浸渍后在空气中500℃热处理6h,得到目标复合光催化剂TiO2纳米片/WO3。
实施例6
利用浸渍法将二维层片材料TiO2悬浊液与WO3进行复合,助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数5%,二维层片材料TiO2悬浊液的浓度220ml/g,浸渍后在空气中400℃热处理4h,得到目标复合光催化剂TiO2纳米片/WO3。
实施例7
TiO2纳米片/WO3的水分解产氧活性的测试:将0.1g TiO2纳米片/WO3置于于光催化水分解反应装置中,加入0.85gAgNO3作为牺牲剂,注入270mL蒸馏水,密封,抽真空,以300W氙灯作为光源,L42滤光片滤掉紫外区域的光,只进行可见光部分的测试,光催化反应期间,每隔1h利用四通阀将反应后的气体注入气相色谱仪(岛津GC-2014)中分析光催化水分解的O2产物产量,即光催化水分解的产氧速率,附图4是复合光催化剂TiO2纳米片/WO3,RuO2/WO3以及WO3在水分解中产氧效率对比图,从图中可以看出负载二维层状材料做助催化剂的WO3的出氧活性是未负载助催化剂的WO3出氧活性的2倍左右,并且比常用的助催化剂RuO2对WO3出氧活性提升作用更明显,说明二维层状材料作为水分解出氧半反应的助催化剂有效提高了光阳极材料WO3的产氧活性。
Claims (7)
1.一种以二维材料作为制氧助催化剂的复合光催化剂;其特征是以超薄二维层片状材料TiO2为助催化的WO3复合材料。
2.如权利要求1所述的光催化剂,其特征是TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%。
3.权利要求1或2的复合光催化剂的制备方法,其特征是:利用浸渍法将二维层片材料TiO2悬浊液与WO3复合制备光催化剂TiO2纳米片/WO3。
4.如权利要求3所述的方法,其特征是助催化剂TiO2层片材料的悬浊液的负载量为WO3质量分数0.1%~5%,二维层片材料TiO2悬浊液的浓度为200~250ml/g,浸渍后在空气中200~500℃热处理2~6h,得到复合光催化剂TiO2纳米片/WO3。
5.如权利要求3所述的方法,其特征是二维层片材料TiO2悬浊液用液相剥离法制得。
6.如权利要求5所述的方法,其特征是用四丁基氢氧化铵对层片状钛酸进行溶胀剥离,搅拌4~8周,最终得到TiO2纳米片悬浮液。
7.如权利要求1所述的光催化剂应用于光催化水分解出氧半反应中。
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