CN110165003B - 一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜及其制备方法和应用 - Google Patents
一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于半导体薄膜技术领域,公开了一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜及其制备方法和应用。所述复合薄膜是将氯化钨和钛酸异丙酯加入溶剂中配置反应前驱液,将氧化锡光子晶体加入反应前驱液在高压反应釜内密封后,在80~120℃恒温反应后,再在450~500℃下进行退火制得。该方法采用溶剂热合成,在氧化锡光子晶体上掺杂介孔核壳结构的氧化钨和氧化钛颗粒,制作出半导体薄膜。该薄膜可作为太阳能电池的阳极应用在太阳能电池领域中。
Description
技术领域
本发明属于半导体薄膜技术领域,更具体地,涉及一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜及其制备方法和应用。
背景技术
近些年,环境污染成为人们亟待解决的一个重要问题。因半导体材料展现出独特的性能,使其为催化降解污染物注入了新的活力。尤其是面对水污染处理这一严峻的挑战,半导体催化剂能够吸收利用太阳光这一绿色能源来催化降解废水中的有机物,光催化效率高、安全性好,能降解几乎所有的有机污染物,使得开发比表面积大、光催化活性高、光响应范围广的光催化材料和经济、有效、环境友好的光催化废水处理技术成为当下研究的重要内容。
二氧化锡是一种非常重要的宽能级N型半导体金属氧化物(禁带宽度为3.6eV)由于其具有良好的气敏性能和独特的光学、电学性能,在气敏元件、气体传感器、电极材料及太阳能电池等多种领域有着广阔的应用前景。然而随着人们对二氧化锡的进一步研究,发现它也是一种很好的光催化剂,越来越多的人将其应用到光催化领域。光催化作用是在具有较高能量的紫外光照射下激发产生的,但是由于二氧化锡具有较宽的能级,因此只有较小波长的紫外光才能激发它的光催化作用,使得其对太阳光的利用率较低。另外,由于在光催化的过程中发挥关键作用的光生电子-空穴对不稳定而很容易复合,这也限制了二氧化锡光催化作用的发挥。因此,为了更好的发挥二氧化锡在光催化领域中的作用就必须解决两个方面的问题:(1)减小禁带宽度;(2)降低光生电子-空穴对的复合率。
发明内容
为了解决上述现有技术存在的不足和缺点,本发明的目的在于提供了一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜。
本发明另一目的在于提供了上述氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的制备方法。该方法采用溶剂热合成法在氧化锡光子晶体上负载介孔核壳结构的氧化钨和氧化钛颗粒,制作出半导体薄膜,该方法制备工艺简单且成本低廉。
本发明再一目的在于提供了上述氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的应用。
本发明的目的通过下述技术方案来实现:
一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,所述复合薄膜是将氯化钨和钛酸异丙酯加入溶剂中配置反应前驱液,将氧化锡光子晶体加入反应前驱液在高压反应釜内密封后,在80~120℃恒温反应后,再在450~500℃下进行退火制得。
优选地,所述溶剂为甲醇或乙醇。
优选地,所述氯化钨的物质的量和溶剂的体积比为(0.6~0.8)mmol:1L;所述氯化钨的质量和钛酸异丙酯的体积比为(0.05~0.15)g:(0.5~1)ml。
优选地,所述退火的时间为1~3h,所述恒温反应的时间为8~12h。
优选地,所述氧化锡光子晶体是将FTO玻璃导电面浸泡在聚苯乙烯溶液中在55~65℃恒温15~30h,然后再浸泡在氯化锡溶液中,430~500℃退火1~2h制得。
优选地,所述聚苯乙烯溶液的浓度为50~80mmol/L,所述氯化锡溶液的浓度为0.5~0.8mol/L。
所述的氧化锡光子晶体负载氧化钨和氧化钛复合薄膜的制备方法,包括如下具体步骤:
S1.将FTO导电玻璃放入食人鱼溶液浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
S2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在55~65℃恒温15~30h,然后再浸泡在氯化锡溶液中,450~500℃退火1~3h,制得氧化锡光子晶体;
S3.将氯化钨和钛酸异丙酯加入到甲醇或乙醇溶剂中配置反应前驱液;
S4.将氧化锡光子晶体放入高压反应釜内胆,将反应前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,恒温80~120℃反应8~12h后,再进行450~500℃退火1~3h处理,得到氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜。
优选地,步骤S1中所述食人鱼溶液为浓硫酸和30%过氧化氢的混合物。
优选地,步骤S1中所述浸泡的时间为8~12h,步骤S5中所述浸泡的时间为30~60s。
所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜在太阳能电池领域中的应用。
本发明通过负载介孔核壳结构的氧化钨和氧化钛实现了对二氧化锡光子晶体的改性。由于氧化钨除具有无毒、高稳定性、低成本等优点,更重要的是它的带隙能为2.4~2.8eV,具有可见光吸收,因此WO3是理想的负载对象。为了进一步提高光催化反应速率,人们通常会采用贵金属沉积、复合半导体等方式,通过这些手段构建内建电池或外加电场来促进光生电子、空穴分离。而氧化钛和氧化钨的复合物,降低了空穴和电子的复合,从而增加了参与反应的电子和空穴数量,显著提高了载流子的利用率。
与现有技术相比,本发明具有以下有益效果:
1.本发明采用溶剂热合成法,以甲醇或乙醇为溶剂,氯化钨为钨源,钛酸异丙酯为钛源,配置反应前驱液,在FTO上的氧化锡光子晶体上负载介孔核壳结构的氧化钛和氧化钨颗粒,制作出半导体薄膜。
2.本发明合成的介孔核壳结构的氧化钨和氧化钛复合薄膜可有效地提高载流子的寿命,提高材料的性能。
3.本发明所需设备和制备工艺简单、成本低廉,可直接大批量生产。
附图说明
图1为实施例1中制备的氧化锡光子晶体薄膜的表面SEM照片。
图2为实施例1制备的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的表面SEM照片。
具体实施方式
下面结合具体实施例进一步说明本发明的内容,但不应理解为对本发明的限制。若未特别指明,实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.FTO导电玻璃衬底的清洗:将FTO导电玻璃放入食人鱼溶液(浓硫酸和30%过氧化氢)浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在60℃恒温20h,然后再浸泡在0.5mol/L氯化锡溶液中,450℃退火2h,制得氧化锡光子晶体;
3.以40ml甲醇为溶剂,0.1g氯化钨为钨源,0.75ml钛酸异丙酯为钛源,配置反应前驱液;
4.再将氧化锡光子晶体放入高压反应釜内胆,将配置的前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,100℃恒温反应6h,在溶剂热反应后,再将其放入马弗炉进行475℃退火2h处理,得到氧化锡光子晶体负载介孔核壳结构的氧化钛和氧化钨复合薄膜。
图1为本实例制备的氧化锡光子晶体薄膜的表面SEM照片。从图1中可知,在50000倍的扫描电子显微镜下观察到的氧化锡光子晶体具有多层并有序地叠在一起,说明了氧化锡光子晶体的有序排列。图2为本实例制备的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的表面SEM照片。在200000倍的扫描电子显微镜下可以看到氧化钛均匀的包裹在氧化钨纳米颗粒上,形成完美的介孔核壳结构。
实施例2
1.FTO导电玻璃衬底的清洗:将FTO导电玻璃放入食人鱼溶液浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在60℃恒温20h,然后再浸泡在0.7mol/L氯化锡溶液中,450℃退火2h,制得氧化锡光子晶体;
3.以30ml甲醇为溶剂,0.1g氯化钨为钨源,0.5ml的钛酸异丙酯为钛源,配置反应前驱液;
4.再将氧化锡光子晶体放入高压反应釜内胆,将配置的前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,100℃恒温反应6h。在溶剂热反应后,再将其放入马弗炉进行475℃退火2h处理;制得氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜。
实施例3
1.FTO导电玻璃衬底的清洗:将FTO导电玻璃放入食人鱼溶液浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在55恒温30h,然后再浸泡在0.8mol/L氯化锡溶液中,450℃退火2h,制得氧化锡光子晶体;
3.以30ml甲醇为溶剂,0.1g氯化钨为钨源,1ml的钛酸异丙酯作为钛源,配置反应前驱液;
4.再将氧化锡光子晶体放入高压反应釜内胆,将配置的前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,100℃恒温反应6h。在溶剂热反应后,再将其放入马弗炉进行475℃退火2h处理,制得氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜。
实施例4
1.FTO导电玻璃衬底的清洗:将FTO导电玻璃放入食人鱼溶液浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在65℃恒温15h,然后再浸泡在0.5mol/L氯化锡溶液中,500℃退火1h,制得氧化锡光子晶体;
3.以20ml甲醇为溶剂,0.1g氯化钨为钨源,0.75ml的钛酸异丙酯为钛源,配置反应前驱液;
4.再将氧化锡光子晶体放入高压反应釜内胆,将配置的前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,100℃恒温反应6h。在溶剂热反应后,再将其放入马弗炉进行475℃退火2h处理;制得氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (9)
1.一种氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,其特征在于,所述复合薄膜是将氯化钨和钛酸异丙酯加入溶剂中配置反应前驱液,将氧化锡光子晶体加入反应前驱液在高压反应釜内密封后,在80~120℃恒温反应后,再在450~500℃下进行退火制得;所述氯化钨的物质的量和溶剂的体积比为(0.6~0.8)mmol:1L;所述氯化钨的质量和钛酸异丙酯的体积比为(0.01~0.03)g:(0.1~0.2)mL。
2.根据权利要求1所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,其特征在于,所述溶剂为甲醇或乙醇。
3.根据权利要求1所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,其特征在于,所述退火的时间为1~3h,所述恒温反应的时间为8~12h。
4.根据权利要求1所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,其特征在于,所述氧化锡光子晶体是将FTO玻璃导电面浸泡在聚苯乙烯溶液中在55~65℃恒温15~30h,然后再浸泡在氯化锡溶液中,430~500℃退火1~2h制得。
5.根据权利要求4所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜,其特征在于,所述聚苯乙烯溶液的浓度为50~80mmol/L,所述氯化锡溶液的浓度为0.5~0.8mol/L。
6.根据权利要求1-5任一项所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的制备方法,其特征在于,包括如下具体步骤:
S1.将FTO导电玻璃放入食人鱼溶液浸泡,然后用去离子水冲洗至中性,得到干净的FTO玻璃;
S2.将干净的FTO玻璃导电面浸泡在聚苯乙烯溶液中在55~65℃恒温15~30h,然后再浸泡在氯化锡溶液中,450~500℃退火1~2h,制得氧化锡光子晶体;
S3.将氯化钨和钛酸异丙酯加入到甲醇或乙醇溶剂中配置反应前驱液;
S4.将氧化锡光子晶体放入高压反应釜内胆,将反应前驱液倒入高压反应釜内胆,密封后放入鼓风干燥箱中,恒温80~120℃反应8~12h后,再进行450~500℃退火1~3h处理,得到氧化锡光子晶体负载介孔核壳结构的氧化钛和氧化钨复合薄膜。
7.根据权利要求6所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的制备方法,其特征在于,步骤S1中所述食人鱼溶液为浓硫酸和30%过氧化氢的混合物。
8.根据权利要求6所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜的制备方法,其特征在于,步骤S1中所述浸泡的时间为8~12h,步骤S5中所述浸泡的时间为30~60s。
9.根据权利要求1-5任一项所述的氧化锡光子晶体负载介孔核壳结构的氧化钨和氧化钛复合薄膜在太阳能电池领域中的应用。
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