CN108636426A - 三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法 - Google Patents
三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法 Download PDFInfo
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Abstract
本发明涉及一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法,复合材料为二硫化钼/石墨烯。其结构为层状二硫化钼垂直均匀分布在齿状石墨烯纳米片表面,形成三维有序取向材料。这种新颖的结构能够促进光生电子的转移,而且具有较大的表面积,同时三维有序朝向阵列二硫化钼暴露较多的活性位点,增强光子的吸收并且优化电荷传输,另外制备过程简单,成本低,可以直接生长在普通透明玻璃上,直接作为光催化电极材料,能够进一步推进光催化制备氢气技术的应用。
Description
技术领域
本发明属于催化领域,涉及一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法。
背景技术
氢能源作为一种可再生清洁能源,能够缓解能源短缺的压力以及环境污染问题,具有巨大的应用潜力。光催化制备氢气技术也因此备受关注。目前二硫化钼/石墨烯复合材料在光催化制备氢气领域中受到了广泛的研究。例如,二硫化钼纳米花/石墨烯复合材料,超薄二硫化钼/石墨烯纳米片复合材料(Ma C B,Qi X,Chen B,et al.MoS2 nanoflower-decorated reduced graphene oxide paper for high-performance hydrogenevolution reaction.[J].Nanoscale,2014,6(11):5624.Deng Z H,Li L,Ding W,etal.Synthesized ultrathin MoS2nanosheets perpendicular to graphene forcatalysis of hydrogen evolution reaction.[J].Chemical Communications,2015,51(10):1893-6)首先,制备石墨烯纳米片的方法多种多样,例如还原氧化石墨烯、液相剥离、CVD等。在这些技术中,CVD技术具有独特的优势,能够有效的控制石墨烯纳米片在金属基片上均匀生长,但是此过程需要昂贵的金属基板,额外的传输也可能阻碍石墨烯器件的性能,因此寻找一种合适的廉价的基板也成为了一个研究关注点。另外随着纳米技术的不断发展,研制出了不同形貌的纳米二硫化钼,其中较为典型的纳米二硫化钼形貌为纳米球和纳米片,相对于二硫化钼纳米球,二硫化钼纳米片具有较大尺寸的表面,能够提供更多的活性位点,更具有催化优势。然而由于二硫化钼/石墨烯结构设计的不合理性导致电子传输受限,光生载流子复合严重,而且暴露的产氢催化活性位点较少,产氢催化效率不高。(BeheraS K,Deb P,Ghosh A.Mechanistic Study on Electrocatalytic Hydrogen Evolution byHigh Efficiency Graphene/MoS2Heterostructure[J].Chemistryselect,2017,2(13):3657-3667.Chen K,Wan X,Jingxiu W,et al.Electrical Properties of MoS2-WS2Heterostructures Synthesized with Two-Step Lateral Epitaxial Strategy[J].AcsNano,2015,9(10):9868.)。因此,杂化结构设计的不合理,也制约了二硫化钼/石墨烯复合材料的在光催化领域的发展和应用;设计优化的合理的二硫化钼/石墨烯复合材料杂化结构成为了一个研究热点。
发明内容
要解决的技术问题
为了避免现有技术的不足之处,本发明提出一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法。该材料主要由二硫化钼和石墨烯复合形成,其结构为层状二硫化钼垂直均匀分布在齿状石墨烯纳米片表面,形成三维有序取向材料。这种材料结构新颖,比表面积大,产氢活性位点多,能够高效光催化分解水产氢。
技术方案
一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料,其特征在于:结构为层状二硫化钼垂直均匀分布在齿状石墨烯纳米片表面,形成三维有序取向材料。
一种制备所述三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料的方法,其特征在于步骤如下:
步骤1、三维石墨烯的制备:经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比为1-2的水和乙醇混合液为前驱体溶液,以0.8-1.0毫升/分钟的速度且压力控制在50-100Pa将前驱体溶液注入PECVD系统,1100-1200℃、50-100Pa环境下生长2-6h,自然冷却至室温,即得到三维石墨烯;
步骤2、三维有序朝向二硫化钼/石墨烯复合材料的制备:通过热蒸发仪蒸发速度控制在在三维石墨烯基片上沉积15-25nm厚的三氧化钼薄膜;然后放在管式炉加热中心区域,将硫粉置于管式炉的上游;管式炉的压力设置为200-400Pa,通入氩气保持管内气氛,氩气流速控制在100-120s.c.c.m;在20-30min内将加热中心加热至550-650℃,硫粉保持在220℃以上,反应10-15min,自然冷却,即得三维有序取向二硫化钼/石墨烯复合材料。
表征:取质量50mg的三维有序朝向二硫化钼/石墨烯材料复合材料,分散在50ml去离子水中。用光催化设备进行光催化制备氢气的测试。光催化制备氢气的测试条件是:光源为氙灯,用电流控制氙灯光源强度,电流为15A。每隔30min进行取样检测。一共取样8次。
有益效果
本发明提出的一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料及制备方法,复合材料为二硫化钼/石墨烯。其结构为层状二硫化钼垂直均匀分布在齿状石墨烯纳米片表面,形成三维有序取向材料。这种新颖的结构能够促进光生电子的转移,而且具有较大的表面积,同时三维有序朝向阵列二硫化钼暴露较多的活性位点,增强光子的吸收并且优化电荷传输,另外制备过程简单,成本低,可以直接生长在普通透明玻璃上,直接作为光催化电极材料,能够进一步推进光催化制备氢气技术的应用。
与二硫化钼/石墨烯简单杂化的复合材料制氢催化剂相比,本发明提供的三维有序朝向二硫化钼/石墨烯复合材料具有新颖的结构,这种三维有序取向结构能够有效地促进光生电子的转移,而且具有较大的表面积,同时三维阵列二硫化钼暴露较多的催化产氢活性位点,增强光子的吸收并且优化电荷传输,另外制备过程简便,成本低,可以直接生长在普通透明玻璃上,做光催化分解水的电极,能够进一步推进光催化制备氢气技术的应用。
附图说明
图1是三维有序取向二硫化钼/石墨烯材料的扫描电镜图。其中500nm是尺寸标尺。
图2是三维有序取向二硫化钼/石墨烯材料的透射电镜图。其中20nm以及2nm是尺寸标尺。
图3是三维有序取向二硫化钼/石墨烯材料光催化产氢测试图
具体实施方式
现结合实施例、附图对本发明作进一步描述:
实施例一:
经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比例1:1.5的水和乙醇混合液为前驱体溶液,以0.8毫升/分钟的速度且压力控制在50Pa将前驱体溶液注入PECVD系统,1100℃、50Pa环境下,生长4h,自然冷却至室温,即可得到三维石墨烯。通过热蒸发仪蒸发速度控制在在上述得到的三维石墨烯基片上沉积15nm厚的氧化钼薄膜。然后将基片放在管式炉加热中心区域,将硫粉置于管式炉的上游。管式炉的压力设置为200Pa,通入氩气保持管内气氛,氩气流速控制在100s.c.c.m。在20min内将加热中心迅速加热至650℃,硫粉前驱体保持在220℃以上,反应15min,自然冷却,可得的三维有序取向二硫化钼/石墨烯复合材料。
表征:取质量50mg的三维有序取向二硫化钼/石墨烯纳米材料,分散在50ml去离子水中。用光催化设备进行光催化制备氢气的测试。光催化制备氢气的测试条件是:光源为氙灯,用电流控制氙灯光源强度,电流为15A。每隔30min进行取样检测。一共取样8次,经过3次循环。结果显示该材料最大产氢量为4324.1微摩尔/克。
实施例二:
经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比例1:1的水和乙醇混合液为前驱体溶液,以0.8毫升/分钟的速度且压力控制在60Pa将前驱体溶液注入PECVD系统,1140℃、60Pa环境下,生长2h,自然冷却至室温,即可得到三维石墨烯。通过热蒸发仪蒸发速度控制在在上述得到的三维石墨烯基片上沉积15nm厚的氧化钼薄膜。然后将基片放在管式炉加热中心区域,将硫粉置于管式炉的上游。管式炉的压力设置为200Pa,通入氩气保持管内气氛,氩气流速控制在100s.c.c.m。在25min内将加热中心迅速加热至550℃,硫粉前驱体保持在220℃以上,反应12min,自然冷却,可得的三维有序取向二硫化钼/石墨烯复合材料。
表征:取质量50mg的三维有序取向二硫化钼/石墨烯纳米材料,分散在50ml去离子水中。用光催化设备进行光催化制备氢气的测试。光催化制备氢气的测试条件是:光源为氙灯,用电流控制氙灯光源强度,电流为15A。每隔30min进行取样检测。一共取样8次,经过3次循环。结果显示该材料最大产氢量为4465.4微摩尔/克。
实施例三:
经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比例1:2的水和乙醇混合液为前驱体溶液,以0.9毫升/分钟的速度且压力控制在80Pa将前驱体溶液注入PECVD系统,1180℃、70Pa环境下,生长6h,自然冷却至室温,即可得到三维石墨烯。通过热蒸发仪蒸发速度控制在在上述得到的三维石墨烯基片上沉积20nm厚的氧化钼薄膜。然后将基片放在管式炉加热中心区域,将硫粉置于管式炉的上游。管式炉的压力设置为200Pa,通入氩气保持管内气氛,氩气流速控制在100s.c.c.m。在30min内将加热中心迅速加热至600℃,硫粉前驱体保持在220℃以上,反应10min,自然冷却,可得的三维有序取向二硫化钼/石墨烯复合材料。
表征:取质量50mg的三维有序取向二硫化钼/石墨烯纳米材料,分散在50ml去离子水中。用光催化设备进行光催化制备氢气的测试。光催化制备氢气的测试条件是:光源为氙灯,用电流控制氙灯光源强度,电流为15A。每隔30min进行取样检测。一共取样8次,经过3次循环。结果显示该材料最大产氢量为4032.5微摩尔/克。
实施例四:
经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比例1:1的水和乙醇混合液为前驱体溶液,以1.0毫升/分钟的速度且压力控制在100Pa将前驱体溶液注入PECVD系统,1200℃、100Pa环境下,生长3h,自然冷却至室温,即可得到三维石墨烯。通过热蒸发仪蒸发速度控制在在上述得到的三维石墨烯基片上沉积25nm厚的氧化钼薄膜。然后将基片放在管式炉加热中心区域,将硫粉置于管式炉的上游。管式炉的压力设置为200Pa,通入氩气保持管内气氛,氩气流速控制在100s.c.c.m。在30min内将加热中心迅速加热至650℃,硫粉前驱体保持在220℃以上,反应10min,自然冷却,可得的三维有序取向二硫化钼/石墨烯复合材料。
表征:取质量50mg的三维有序取向二硫化钼/石墨烯纳米材料,分散在50ml去离子水中。用光催化设备进行光催化制备氢气的测试。光催化制备氢气的测试条件是:光源为氙灯,用电流控制氙灯光源强度,电流为15A。每隔30min进行取样检测。一共取样8次,经过3次循环。结果显示该材料最大产氢量为3975.8微摩尔/克。
Claims (2)
1.一种三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料,其特征在于:结构为层状二硫化钼垂直均匀分布在齿状石墨烯纳米片表面,形成三维有序取向材料。
2.一种制备权利要求1所述三维有序取向二硫化钼/石墨烯高效光催化制氢复合纳米材料的方法,其特征在于步骤如下:
步骤1、三维石墨烯的制备:经超声波清洗以及紫外线清洗后的玻璃装入等离子体增强化学气相沉积装置,取体积比为1-2的水和乙醇混合液为前驱体溶液,以0.8-1.0毫升/分钟的速度且压力控制在50-100Pa将前驱体溶液注入PECVD系统,1100-1200℃、50-100Pa环境下生长2-6h,自然冷却至室温,即得到三维石墨烯;
步骤2、三维有序朝向二硫化钼/石墨烯复合材料的制备:通过热蒸发仪蒸发速度控制在在三维石墨烯基片上沉积15-25nm厚的三氧化钼薄膜;然后放在管式炉加热中心区域,将硫粉置于管式炉的上游;管式炉的压力设置为200-400Pa,通入氩气保持管内气氛,氩气流速控制在100-120s.c.c.m;在20-30min内将加热中心加热至550-650℃,硫粉保持在220℃以上,反应10-15min,自然冷却,即得三维有序取向二硫化钼/石墨烯复合材料。
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