CN110665528A - 一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法 - Google Patents
一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开一种2D/2D g‑C3N4/ZnIn2S4异质结复合光催化剂的制备方法。首先采用柠檬酸钠对ZnIn2S4光催化剂进行改性,寻找最佳的使用量。然后对g‑C3N4光催化剂进一步优化。通过在g‑C3N4纳米片表面原位生长一层ZnIn2S4纳米片,制备了2D/2D g‑C3N4/ZnIn2S4复合光催化剂。本发明制备方法简单,原材料易得,反应条件适中。所制备的g‑C3N4/ZnIn2S4二维复合光催化材料具有高效光催化产氢活性,产氢速率达到了3.4mmol/h/g,比单一的g‑C3N4产氢速率提高了180%。
Description
技术领域
本发明属于材料制备技术领域,具体涉及一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法。
背景技术
能源与环境,一直是备受瞩目的全球性问题。煤、石油等传统化石能源是目前全球消耗的主要能源。但一方面由于气候变化、自然灾害和一些社会原因导致能源生产增长缓慢;另一方面,人口的迅速增长以及世界经济的持续发展,特别是新兴经济体的迅速增长,导致能源消耗剧增。石油的消耗速度是自然生产石油速度的10万倍,现有的化石能源储存量已经跟不上世界经济发展的脚步。更严重的问题是,化石能源的大量消耗所引起的空气污染、水体污染、全球变暖等环境问题,直接威胁着人类的生存。因此开发绿色、安全的新能源迫在眉睫。
光催化技术就是以太阳光或模拟光源为能量来源,半导光受光能激发,作为催化剂,催化化学反应的完成,即半导体光催化材料在太阳光的激发下完成特定的氧化还原反应。根据固体能带理论,半导体的能带是不连续的,其能带分为导带(CB)和价带(VB),价带上充满电子,导带上是空的,导带底部和价带顶部之间被称为带隙或禁带宽度(Eg)。当入射光的能量大于等于带隙能量时,价带的电子(e-)吸收入射光能量,跃迁到导带,同时在价带上产生相同数量的空穴(h+),形成电子-空穴对。导带上的电子具有较强的还原性,可以作为还原剂,进行还原反应;价带上的空穴具有较强的氧化性,作为氧化剂,进行氧化反应。被吸收的能量通过激发电子跃迁被储藏在半导体中,之后,通过一系列化学反应转化成化学能。
g-C3N4在分解水方面的应用上被认为是一种理想材料,因为它具有以下优点:⑴能量带隙约为2.7eV,它的吸收光谱大约在460nm的可见光范围内,能有效利用太阳光,而且2.7eV的带隙能量足够使电子发生受激跃迁。g-C3N4的价带和导带位置的电位都在水的氧化还原电位之上,因此,光生电子被充分还原,将水还原成H2,光生空穴具有足够的氧化还原能力氧化水放出O2。g-C3N4的化学稳定性很好,在600℃下都能保证其结构的稳定。g-C3N4具有特定的微观结构,表面有一定的缺陷,缺陷位的原子可作为反应的活性位点或者金属的附着位点。而且g-C3N4这种材料成本低廉,绿色环保,可以光催化完全分解水。但是,纯g-C3N4还是存在一定的不足,它的光生载流子的复合率高,因而限制了它的光催化活性,因此,有必要对g-C3N4进行一定的改性。
ZnIn2S4具有以下优点:(1)ZnIn2S4具有典型的层状结构,因此,能有效增大比表面积,提高催化反应的效率。(2)ZnIn2S4具有优异的电学性能和光学性能,在分解水制氢中的优势明显。(3)ZnIn2S4具有较强的可见光捕获能力,能够充分利用光源。但是,ZnIn2S4吸收可见光产生的光生电子和光生空穴极易复合,致使其光催化量子效率较低。因此,纯ZnIn2S4作为分解水产氢的光催化剂还是有一定局限性的。
ZnIn2S4具有与g-C3N4匹配的带隙结构,使得制备g-C3N4/ZnIn2S4复合异质结光催化剂成为可能。利用水热法制备的ZnIn2S4/g-C3N4纳米复合材料,在g-C3N4纳米片上生长一层ZnIn2S4纳米片,提高电荷分离和迁移效率,使其具有高的光催化析氢性能。
所制备的g-C3N4/ZnIn2S4异质结就是两种不同的半导体在其相互接触的界面形成的区域。由于两种半导体中各自的费米能级电势不同,于是,在两种半导体之间的载流子就会发生移动。由于内建电场的作用异质结内部的载流子便形成了定向移动,光生电子和空穴分别向相反的方向移动,从而在很大程度上降低了载流子的复合率,同时,异质结结构还能增强光催化剂的稳定性,扩大吸光光谱范围,在很大程度上体高了光催化的效率。
本发明通过对两种纳米片材料分别改性,制备出高效的具有可见光活性的复合光催化剂。
发明内容
本发明的目的是针对上述现状,旨在提供制备一种高效光催化材料的方法;此方法简单易操作、安全可靠。
实现本发明目的的技术方案是:一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法,其特征在于,包括如下步骤:
步骤1:g-C3N4超薄纳米片的制备
(1.1)将2-10g三聚氰胺加入到100ml的坩埚中,然后在此坩埚中加入5-20g氯化铵,然后加入5-20ml水,用玻璃棒搅拌均匀,放入到60℃烘箱中烘干;
(1.2)将步骤(1.1)中的带盖坩埚放入箱式马弗炉中,以2-20℃/min的升温速率,加热到500-600℃,冷却后,在球磨机中带水球磨30-60min,然后洗涤烘干;
(1.3)将步骤(1.2)所制备的样品,放入500-700℃的管式炉中继续加热2-4小时,升温速率为2-10℃/min,所通气体为高纯氩气,气体流速为0.1-2L/min;样品冷却后,即为所得到的g-C3N4超薄纳米片;
步骤2:制备g-C3N4/ZnIn2S4超薄纳米片
(2.1)在50ml的烧杯中分别放入10-30ml去离子水、0.1-0.5g Zn(NO3)2·6H2O、0.2-0.8g In(NO3)3·4.5H2O和步骤(1.3)中所制备的g-C3N4超薄纳米片,搅拌10-30min后,超声5-10min,继续搅拌;
(2.2)在步骤(2.1)所搅拌的溶液中,加入0.1-1g柠檬酸钠,室温下继续搅拌10-30min;搅拌的溶液中加入0.2-0.8g硫代乙酰胺,室温下继续搅拌10-30min;将所制备溶液转移到50ml不锈钢反应釜中,在160-180℃中加热2-24小时;洗涤烘干后得到g-C3N4/ZnIn2S4超薄纳米片。
进一步的,所述步骤(2.1)中加入的步骤(1.3)中所制备的g-C3N4超薄纳米片用量为0.01g-0.2g。
本发明的作用机理:2D g-C3N4纳米薄片、2D ZnIn2S4纳米叶片和2D/2D异质结界面的协同作用,有助于异质结体系中形成独特的高速电荷转移纳米通道。这些2D/2D异质结内部的高速电荷转移纳米通道大大缩短了电荷迁移距离和转移时间,显著提高了电荷传输和分离效率。同时,催化剂本身的尺寸也会影响催化活性,将复合催化剂设计成纳米级,可以减少电子和空穴的复合几率,同时增大比表面积,有利于分解水反应的进行。
与现有技术相比,本发明的有益效果是:
1、所获得g-C3N4/ZnIn2S4异质结复合光催化剂,光催化产氢活性比单一的g-C3N4光催化剂提高了180%。
2、本发明所制备g-C3N4/ZnIn2S4异质结复合光催化剂方法简单易操作,具有实际的可行性,且制备的g-C3N4/ZnIn2S4光催化材料成本低,无污染。
附图说明
图1是本发明的g-C3N4/ZnIn2S4复合材料的扫描电镜图。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样在本申请所列权利要求书限定范围之内。
实施例1
步骤1:g-C3N4超薄纳米片的制备
(1.1)将2g三聚氰胺加入到100ml的坩埚中,然后在此坩埚中加入10g氯化铵,然后加入10ml水,用玻璃棒搅拌均匀,放入到60℃烘箱中烘干。
(1.2)将步骤(1.1)中的带盖坩埚放入箱式马弗炉中,以4℃/min的升温速率,加热到550℃,冷却后,在球磨机中带水球磨30min,然后洗涤烘干。
(1.3)将步骤(1.2)所制备的样品,放入620℃的管式炉中继续加热2小时,升温速率为5℃/min,所通气氛为高纯氩气,气体流速为0.1L/min;样品冷却后,即为所得到的g-C3N4超薄纳米片。
步骤2:制备g-C3N4/ZnIn2S4超薄纳米片
(2.1)在50ml的烧杯中分别放入30ml去离子水、0.3g Zn(NO3)2·6H2O、0.76g In(NO3)3·4.5H2O和0.01g的步骤(1.3)中所制备的g-C3N4超薄纳米片,搅拌30min后,超声10min,继续搅拌。
(2.2)在步骤(2.1)所搅拌的溶液中,加入0.1g柠檬酸钠,室温下继续搅拌30min;搅拌的溶液中加入0.6g硫代乙酰胺,室温下继续搅拌30min;将所制备溶液转移到50ml不锈钢反应釜中,在180℃中加热4小时;洗涤烘干后得到了g-C3N4/ZnIn2S4超薄纳米片。
实施例2
步骤1:g-C3N4超薄纳米片的制备
(1.1)将5g三聚氰胺加入到100ml的坩埚中,然后在此坩埚中加入10g氯化铵,然后加入5ml水,用玻璃棒搅拌均匀,放入到60℃烘箱中烘干。
(1.2)将步骤(1.1)中的带盖坩埚放入箱式马弗炉中,以5℃/min的升温速率,加热到550℃,冷却后,在球磨机中带水球磨60min,然后洗涤烘干。
(1.3)将步骤(1.2)所制备的样品,放入650℃的管式炉中继续加热4小时,升温速率为10℃/min,所通气氛为高纯氩气,气体流速为0.1L/min;样品冷却后,即为所得到的g-C3N4超薄纳米片。
步骤2:制备g-C3N4/ZnIn2S4超薄纳米片
(2.1)在50ml的烧杯中分别放入30ml去离子水、0.3g Zn(NO3)2·6H2O、0.76g In(NO3)3·4.5H2O和0.02g的步骤(1.3)中所制备的g-C3N4超薄纳米片,搅拌30min后,超声5min,继续搅拌。
(2.2)在步骤(2.1)所搅拌的溶液中,加入0.2g柠檬酸钠,室温下继续搅拌10-30min;搅拌的溶液中加入0.6g硫代乙酰胺,室温下继续搅拌30min;将所制备溶液转移到50ml不锈钢反应釜中,在160℃中加热24小时;洗涤烘干后得到了g-C3N4/ZnIn2S4超薄纳米片。
实施例3
步骤1:g-C3N4超薄纳米片的制备
(1.1)将2g三聚氰胺加入到100ml的坩埚中,然后在此坩埚中加入20g氯化铵,然后加入5ml水,用玻璃棒搅拌均匀,放入到60℃烘箱中烘干。
(1.2)将步骤(1.1)中的带盖坩埚放入箱式马弗炉中,以4℃/min的升温速率,加热到550℃,冷却后,在球磨机中带水球磨60min,然后洗涤烘干。
(1.3)将步骤(1.2)所制备的样品,放入620℃的管式炉中继续加热4小时,升温速率为5℃/min,所通气氛为高纯氩气,气体流速为0.1L/min;样品冷却后,即为所得到的g-C3N4超薄纳米片。
步骤2:制备g-C3N4/ZnIn2S4超薄纳米片
(2.1)在50ml的烧杯中分别放入30ml去离子水、0.3g Zn(NO3)2·6H2O、0.76g In(NO3)3·4.5H2O和0.01g的步骤(1.3)中所制备的g-C3N4超薄纳米片,搅拌30min后,超声10min,继续搅拌。
(2.2)在步骤(2.1)所搅拌的溶液中,加入0.3g柠檬酸钠,室温下继续搅拌10-30min;搅拌的溶液中加入0.6g硫代乙酰胺,室温下继续搅拌10-30min;将所制备溶液转移到50ml不锈钢反应釜中,在180℃中加热24小时;洗涤烘干后得到了g-C3N4/ZnIn2S4超薄纳米片。
本发明公开的2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法,首先采用柠檬酸钠对ZnIn2S4光催化剂进行改性,寻找最佳的使用量。然后对g-C3N4光催化剂进一步优化。通过在g-C3N4纳米片表面原位生长一层ZnIn2S4纳米片,制备了2D/2D g-C3N4/ZnIn2S4复合光催化剂。本发明制备方法简单,原材料易得,反应条件适中。所制备的g-C3N4/ZnIn2S4二维复合光催化材料对具有高效光催化产氢活性,产氢速率达到了3.4mmol/h/g,比单一的g-C3N4产氢速率提高了180%。
最后应当说明的是,以上内容仅用以说明本发明的技术方案,而非对本发明保护范围的限制,本领域的普通技术人员对本发明的技术方案进行的简单修改或者等同替换,均不脱离本发明技术方案的实质和范围。
Claims (2)
1.一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法,其特征在于,包括如下步骤:
步骤1:g-C3N4超薄纳米片的制备
(1.1)将2-10g三聚氰胺加入到100ml的坩埚中,然后在此坩埚中加入5-20g氯化铵,然后加入5-20ml水,用玻璃棒搅拌均匀,放入到60℃烘箱中烘干;
(1.2)将步骤(1.1)中的带盖坩埚放入箱式马弗炉中,以2-20℃/min的升温速率,加热到500-600℃,冷却后,在球磨机中带水球磨30-60min,然后洗涤烘干;
(1.3)将步骤(1.2)所制备的样品,放入500-700℃的管式炉中继续加热2-4小时,升温速率为2-10℃/min,所通气体为高纯氩气,气体流速为0.1-2L/min;样品冷却后,即为所得到的g-C3N4超薄纳米片;
步骤2:制备g-C3N4/ZnIn2S4超薄纳米片
(2.1)在50ml的烧杯中分别放入10-30ml去离子水、0.1-0.5g Zn(NO3)2·6H2O、0.2-0.8g In(NO3)3·4.5H2O和步骤(1.3)中所制备的g-C3N4超薄纳米片,搅拌10-30min后,超声5-10min,继续搅拌;
(2.2)在步骤(2.1)所搅拌的溶液中,加入0.1-1g柠檬酸钠,室温下继续搅拌10-30min;搅拌的溶液中加入0.2-0.8g硫代乙酰胺,室温下继续搅拌10-30min;将所制备溶液转移到50ml不锈钢反应釜中,在160-180℃中加热2-24小时;洗涤烘干后得到g-C3N4/ZnIn2S4超薄纳米片。
2.如权利1所述的一种2D/2D g-C3N4/ZnIn2S4异质结复合光催化剂的制备方法,其特征在于:所述步骤(2.1)中加入的步骤(1.3)中所制备的g-C3N4超薄纳米片用量为0.01g-0.2g。
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