CN110841626A - 一种氧化钨/氧化铋网-片复合材料及制备方法与用途 - Google Patents
一种氧化钨/氧化铋网-片复合材料及制备方法与用途 Download PDFInfo
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Abstract
本发明涉及一种氧化钨/氧化铋网‑片复合材料及制备方法与用途，属于材料制备和光催化技术领域。本发明通过采用原位合成的方法制备了具有化学键异质结的Bi2O3/WO3光催化剂。该样品的合成是在反应进行到一半时终止，形成复合型光催化剂。该复合型光催化剂原料廉价，且合成方法简单，所制备的复合型光催化剂具有稳定的理化性质，无毒等优点。其光催化还原CO2活性高，生产过程绿色环保，既达到环境友好，又为可持续发展生产新能源提供了新思路，有望工业化生产。
Description
技术领域
本发明涉及一种氧化钨/氧化铋网-片复合材料及制备方法与用途，属于材料制备和光催化技术领域。
背景技术
利用可再生太阳能实现CO2光催化还原是缓解温室效应、燃料短缺等问题的重要手段。光催化还原CO2可以给我们带来巨大的环境保护和资源再生效益。目前，TiO2、g-C3N4、ZnO等已被广泛报道。但它们大多具有光生载流子复合率高、可见光无响应等缺点。因此，开发一种可见光响应、光生载流子复合率低的光催化剂具有重要意义。
不同半导体的界面通过化学键连接可以促进电荷的快速分离，定义为异质结，异质结的影响是来自原子薄界面的内置电场。已有研究表明，异质结会降低光生电子空穴的复合率。与传统的异质结材料相比，由不同超薄2D材料组成的化学键原位异质结引起了广泛的兴趣。Bi2WO6是由[BiO]+-[WO4]2--[BiO]+组成的一种典型的Aurivillius相氧化物，[BiO]+单分子层与[WO4]2-单分子层通过化学键紧密连接。同时，不同的单分子层容易通过范德华力堆叠在一起，降低了反应位点数量，并且载流子复合率增加，导致活性降低。在此基础上，迫切需要开发出有着更多催化活性中心和化学键原位异质结的光催化剂，以达到高活性和高稳定性的目的。然而，目前对于具备这些特点的光催化剂的研究仍然缺乏。
迄今为止，一些研究已经采用强化学键阻止单层膜堆积。为了阻止[BiO]+单层膜堆积在一起，已有研究通过将表面活性剂CTAB附着在[BiO]+单层膜表面，使得[BiO]+单层膜表面存在大量的CTA+，[BiO]+单层膜表面的CTA+可以阻止[BiO]+单层膜之间的堆积，形成具有超薄结构的Bi2WO6纳米片。然而，在Bi2WO6三明治分子层结构纳米片中，当可见光激发时两侧[BiO]+单层膜电子会转移到中间WO4 2-单层膜上，具有较高的光生载流子分离率。而[BiO]+-WO4 2--[BiO]+的两侧[BiO]+单分子层都具有相同的库仑力，该库仑力来自于中间的WO4 2-单分子层的吸引力。{[BiO]+-WO4 2-}与{WO4 2--[BiO]+}之间的相互作用削弱了W原子的引力，导致光生载流子迁移速率较慢，载流子易复合。此外，CO2还原反应位点仅分布在Bi2WO6中间WO4 2-层边缘位置，还原性能较差。本研究的目的是制备非对称结构光催化剂，该催化剂能暴露出大量的活性位点，并且不同超薄单分子层之间直接由化学键相连接，以形成联系紧密利于电荷传输的原位异质结。
通过采用原位合成的方法制备了具有化学键异质结的Bi2O3/WO3光催化剂。该样品的合成是在反应进行到一半时终止，形成复合型光催化剂。该复合型光催化剂原料廉价，且合成方法简单，所制备的复合型光催化剂具有稳定的理化性质，无毒等优点。其光催化还原CO2活性高，生产过程绿色环保，既达到环境友好，又为可持续发展生产新能源提供了新思路，有望工业化生产。
发明内容
本发明目的是提供一种简易的一步水热法合成二维网筛WO3/Bi2O3纳米片复合半导体材料的方法。
本发明通过以下技术实现：
通过在形成稳定的三明治结构Bi2WO6二维超薄纳米片的水热反应过程中，将反应终止，在反应中间过渡状态形成了WO3/Bi2O3复合型光催化剂。并且通过加入阳离子表面活性剂CTAB，形成了具有超薄结构的二维WO3网筛和Bi2O3纳米片。
本发明通过以下步骤实现：
合成WO3/Bi2O3：称取硝酸铋、钨酸钠和十六烷基三甲基溴化铵溶于去离子水中，搅拌器搅拌后，将混合溶液倒入聚四氟乙烯的反应釜中，将反应釜置于烘箱中，180℃进行24小时水热反应将会得到三明治结构的Bi2WO6二维超薄纳米片，若在反应进行到12小时终止水热反应，将会得到中间过渡态产物WO3/Bi2O3复合型光催化剂，反应完成后，用去离子水和无水乙醇对样品进行离心洗涤。最后，对样品进行干燥。
铋钨原子化学计量比为2：1。
十六烷基三甲基溴化铵为定量加入，加入量为0.025g。
所述搅拌器搅拌时间为30min。
利用X射线衍射仪(XRD)、透射电子显微镜(TEM)以及高分辨透射电子显微镜(HRTEM)对产物进行形貌结构分析，通过氙灯照射还原二氧化碳进行光催化活性实验，通过CEAULIGHT GC-7920气相色谱保留时间确定还原产物种类，用实测峰面积与标准峰面积进行对比来确定还原二氧化碳效率，以评估其光催化还原二氧化碳性能。
与现有技术相比，所制备二维超薄结构Bi2O3纳米片和WO3纳米网筛，其表面均暴露出大量的协同不饱和Bi原子和W原子作为活性位点。Bi2O3表面的CTA+阻止Bi2O3单层膜之间的堆叠，形成超薄结构的Bi2O3纳米片。与对称三明治结构Bi2WO6相比，WO3/Bi2O3的非对称结构不存在Bi2O3单层之间的电荷竞争，可以获得高效快速的光生载流子分离效率。该光催化剂不仅具有双活性中心(协同不饱的Bi原子和大量暴露的W原子)，而且具有较强的化学键原位异质结，与机械复合型光催化剂有着本质区别。双位点之间可以形成协同效应，提高氧化还原能力。同时，原位合成的异质结具有高效的电子空穴分离率。总的来说，本实验为研究多金属氧化物的中间过渡态体系，形成具有多位点高活性的复合金属氧化物半导体光催化剂提供了参考和指导。
附图说明
图1为所制备WO3/Bi2O3复合材料的XRD衍射谱图。从图中可以看出该复合型光催化剂的衍射峰对应于单体WO3(JCPDS NO.83-0951)和Bi2O3(JCPDSNO.71-0147)的特征峰。可以看出该复合型纳米光催化材料已成功制备且复合样品结晶度高、无杂质。
图2为所制备WO3/Bi2O3复合材料的透射电镜照片和高分辨透射电子显微镜照片，(a,b,c)为WO3/Bi2O3样品的不同尺度下的透射电子显微镜照片，由图可以看出该复合型光催化剂成功制备，且网筛和片之间紧密连接；(d,e,f)为WO3/Bi2O3高分辨透射电子显微镜照片，图中有着清晰可见的WO3和Bi2O3晶格条纹，表明该复合型光催化剂的成功制备。
图3为所制备WO3/Bi2O3复合材料的XPS能谱，进一步分析样品的元素组成和化学状态。(a)单体Bi2O3的Bi 4f结合能分别为158.1eV和163.5eV，而WBC-12h和WBC-24h的特征峰分别位于159.1eV和164.5eV。Bi的结合能增大的原因是Bi原子与表面Br原子结合，且WBC-12h和WBC-24h(Bi2WO6)具有相同的结合能。(b)W 4f5/2和W 4f7/2的肩峰(37.6eV和35.4eV)出现在更高的结合能，且WBC-12h和WBC-24h具有相同的结合能。由于WBC-12h和WBC-24h具有相同的W和Bi结合能，说明WBC-12h与Bi2WO6具有相同的非均相界面(化学键界面)。因此，成功制备了具有化学键原位异质结的WO3/Bi2O3复合型光催化剂。
图4为光催化CO2还原活性图，(a)单体WO3和单体Bi2O3以及复合型光催化剂WO3/Bi2O3的CO产率图；(b)单体WO3和单体Bi2O3以及复合型光催化剂WO3/Bi2O3的CO生成速率图。该WO3/Bi2O3复合型光催化剂在反应两小时后CO生成率高达35μmol·g-1,CO生成速率高达16.65μmol·g-1·h-1,光催化活性为单体WO3和Bi2O3催化剂的10倍。
具体实施方式
实施例1 WO3纳米光催化材料的制备
称取0.5g二水合钨酸钠和0.3g一水合柠檬酸于烧杯中，加入30mL去离子水搅拌至完全溶解，逐滴加入6mol L-1的盐酸溶液调节溶液的pH值至1，继续搅拌1h直至得到黄色悬浊液，然后将所得悬浊液转移到50mL反应釜中,放入烘箱中，120℃水热反应12h；待自然冷却至室温后，用去离子水和无水乙醇分别洗3次，离心分离后在60℃下干燥。取出，用研钵研磨至粉末状后，转入半封闭的坩埚中，然后转移到程序升温管式炉中500℃煅烧2h。
实施例2 Bi2O3纳米光催化材料的制备
1.46g Bi(NO3)3·5H2O加入到51mL乙醇和25.5mL乙二醇中，搅拌1h，将混合液倒入80mL反应釜中，160℃反应5h，将样品离心，去离子水和乙醇分别洗涤3次，60℃干燥12h得粉末样品。
实施例3 WO3/Bi2O3复合纳米光催化材料的制备
0.1649g Na2WO4·2H2O,0.4650g Bi(NO3)3·5H2O,0.025g CTAB溶于40mL去离子水中。搅拌30min后，将混合溶液倒入80mL反应釜中，180℃加热12h，反应完成后，用去离子水和无水乙醇对得到的样品进行离心洗涤3次。最后，样品在60℃干燥12h得粉末样品。
实施例4 WO3/Bi2O3复合材料的光催化CO2还原实验
(1)在150mL自制耐热玻璃反应器中进行光催化CO2还原实验。将30mg试样加入适量去离子水中分散均匀，60℃烘干。
(2)在反应器槽中加入0.084g NaHCO3。氮气氛围下鼓泡15min后，注入0.3mLH2SO4(2mol L-1)与NaHCO3反应，释放CO2和H2O。用300W氙灯照射，安装上截止滤光片(λ>400nm)。
(3)用气相色谱仪(CEAULIGHT GC-7920)对产物进行检测，每隔半小时抽样注入气相色谱中进行检测，并用标准气体混合物进行标定。用保留时间测定各组分，用峰面积外标法计算各组分浓度。该WO3/Bi2O3复合型光催化剂在反应两小时后CO生成率高达35μmol·g-1,单位时间内产生CO的速率为16.65μmol·g-1·h-1,活性为单体WO3和Bi2O3的10倍。
Claims (5)
1.一种氧化钨/氧化铋网-片复合材料，其特征在于，所述复合材料由二维超薄结构Bi2O3纳米片和WO3纳米网筛组成，WO3纳米网筛和Bi2O3纳米片之间由化学键相连接，形成利于电荷传输的原位异质结。
2.如权利要求1所述的一种氧化钨/氧化铋网-片复合材料的制备方法，其特征在于，具体步骤如下：称取硝酸铋、钨酸钠和十六烷基三甲基溴化铵溶于去离子水中，搅拌器搅拌后，将混合溶液倒入聚四氟乙烯的反应釜中，将反应釜置于烘箱中，180℃进行水热反应，水热反应进行到12小时终止水热反应，得到中间过渡态产物WO3/Bi2O3复合型光催化剂，用去离子水和无水乙醇对样品进行离心洗涤，最后，对样品进行干燥得到氧化钨/氧化铋网-片复合材料。
3.如权利要求2所述的一种氧化钨/氧化铋网-片复合材料的制备方法，其特征在于，铋钨原子化学计量比为2：1。
4.如权利要求2所述的一种氧化钨/氧化铋网-片复合材料的制备方法，其特征在于，十六烷基三甲基溴化铵为定量加入，加入量为0.025g；所述搅拌器搅拌时间为30min。
5.如权利要求1所述的一种氧化钨/氧化铋网-片复合材料的用途，其特征在于，用于光催化还原二氧化碳。
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