CN109012685B - 一种BiFeO3和Bi2WO6复合薄膜的制备方法 - Google Patents
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Abstract
本发明专利公开了一种BiFeO3和Bi2WO6复合薄膜的制备方法,分别以硝酸铋、硝酸铁、钨酸铵、去离子水、乙酰丙酮、乙二醇、冰乙酸和硝酸为主要原料分别制备BiFeO3和Bi2WO6前驱体溶液,然后将两种溶液混合搅拌得到稳定的Bi3WFeO9前驱体溶液。混合的前驱体溶液在玻璃基体上经过涂膜,热解和退火得到晶态薄膜。Bi3WFeO9薄膜具有比BiFeO3和Bi2WO6更好的光催化性,可以应用于建筑物玻璃或者外墙表面,可高效分解污染物具有自清洁功能。本发明在光催化领域具有广阔的应用前景。
Description
技术领域
本发明涉及光电子材料领域,尤其涉及一种BiFeO3和Bi2WO6复合薄膜的制备方法。
背景技术
半导体光催化技术是当前解决全球环境污染问题的研究热点之一。Bi2WO6是一类非金属含氧酸盐结构的新型光催化材料,因其较高的催化活性和稳定性而作为近年来半导体光催化材料研究一个重点,而且钨酸盐根等酸根离子具有结构稳定、不易发生光腐蚀等优点。但Bi2WO6具有较大的禁带宽度( 2.70eV) ,只能被紫外光或部分可见光激发,可见光吸收范围为420-470nm,且光生电子空穴对容易发生复合,从而使材料的光催化性能降低,不能达到预期的要求。因此,为了降低电子-空穴复合率,对Bi2WO6材料进行复合以提高材料的光催化性能成为近年来以及以后的一个研究热点。铁酸铋BiFeO3作为一种典型的铁磁材料,由于其带隙较窄(2.1 eV)可利用太阳光中的可见光部分,以及利用其铁电材料微观固有的电场来实现光生电子-空穴的高效分离,可以降低Bi2WO6中的光生载流子的复合几率、提高光催化效率,所以BiFeO3材料是一种具有潜在应用价值的可见光催化材料。因此,将Bi2WO6与BiFeO3进行复合,有望成为性能良好的纳米复合光催化材料。
将BiFeO3和Bi2WO6复合光催化材料应用于建筑物玻璃或者外墙表面,可高效分解污染物,此外,由于其具有优良的亲水性,当雨水冲刷时,水流从污染物根部进行全面冲洗,可将附着在墙体上的残留的灰尘和分解后的带有油性污迹清洗干净,即BiFeO3和Bi2WO6纳米复合光催化材料具有自清洁功能。为了更加方便的应用复合薄膜,我们发明了一种直接涂覆在平板玻璃上BiFeO3/Bi2WO6复合薄膜的制备方法。
发明内容
本发明采用化学溶液沉积法,结合层层退火工艺制备BiFeO3/Bi2WO6复合薄膜,薄膜的制备及测试过程主要分为三个阶段,即前驱体溶液的配制阶段,湿膜的制备阶段,热处理成膜阶段,以普通平板玻璃为基体。
具体方案如下:
(1)BiFeO3薄膜前驱体溶液配制:首先用电子天平按照各溶质的摩尔计量比进行称取,硝酸铁与硝酸铋的摩尔比为1:1:1;用移液管量取体积比为1:3的乙二醇和冰乙酸作为溶剂,将上述溶质和溶液置于磁力搅拌器上搅拌12小时,直至溶质全部溶解,待溶液搅拌均匀后,量取与硝酸铋摩尔比为1:1的乙酰丙酮作为螯合剂加入其中,在磁力搅拌器上匀速搅拌12小时,得到暗红色半透明溶液。最后再补充乙二醇和冰乙酸,控制溶液浓度为0.3mol/L, pH值在0.3-0.4。将所得的半透明暗红色溶液置于常温下静置24小时,得到制备BiFeO3薄膜样品所需的前驱体溶液。
(2)Bi2WO6薄膜前驱体溶液的配制:用电子天平称取摩尔比为1:2的钨酸铵和硝酸铋,将上述溶质溶解在去离子水中,量取钨酸铵摩尔比为1:1的乙酰丙酮作为螯合剂,去离子水调节溶液浓度为0.3mol/L,用硝酸调节pH值在0.3-0.4。将上述溶液放在磁力搅拌器中搅拌12小时,得到澄清透明的溶液,常温静止24小时,得到Bi2WO6薄膜前驱体溶液。
(3)将BiFeO3和Bi2WO6溶液按照摩尔比1:1混合搅拌24小时,得到混合的前驱体溶液。
(4)将混合的前驱体溶液均匀旋涂在清洗干净的玻璃衬底上。将衬底置于匀胶机的样品台上,将前驱体溶液滴在衬底上(每次滴加液体时控制高度并保证滴加量大致相等),为使溶液在衬底上得以充分扩散,须等待30s后打开真空泵,将衬底牢牢吸附在样品台上,启动匀胶机。
(5)湿膜烘干:将涂膜结束的薄膜样品快速转移到100-150℃的电热板上60s烘干,使所制备湿膜中的部分有机溶剂得以挥发,从而得到所要求薄膜的干膜。
(6)预处理:将前期所制备的干模置于快速退火炉中,预处理温度为300-400℃,保温时间100-200s。
(7)最终退火:这一过程和预处理过程相类似,只是温度不同。退火温度为400-500℃,保温时间都为200-300s,得到晶态薄膜样品。
(8)将湿膜的制备和热处理成膜两个阶段重复,从而制得所需厚度的薄膜样品,制备的薄膜层数为10层。
本发明的效益是制备出来光催化效果更好的BiFeO3和Bi2WO6复合材料。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
实施例1
将混合的前驱体溶液均匀旋涂在清洗干净的玻璃衬底上。将衬底置于匀胶机的样品台上,将前驱体溶液滴在衬底上,为使溶液在衬底上得以充分扩散,须等待30s后打开真空泵,将衬底牢牢吸附在样品台上,启动匀胶机。将涂膜结束的薄膜样品快速转移到125℃的电热板上60s烘干,使所制备湿膜中的部分有机溶剂得以挥发,从而得到所要求薄膜的干膜。将前期所制备的干模置于快速退火炉中,预处理温度为300℃,保温时间150s。将热解的薄膜退火处理,退火温度为400℃,保温时间都为250s,得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复,从而制得所需厚度的薄膜样品,制备的薄膜层数为10层。
实施例2
将混合的前驱体溶液均匀旋涂在清洗干净的玻璃衬底上。将衬底置于匀胶机的样品台上,将前驱体溶液滴在衬底上,为使溶液在衬底上得以充分扩散,须等待30s后打开真空泵,将衬底牢牢吸附在样品台上,启动匀胶机。将涂膜结束的薄膜样品快速转移到125℃的电热板上60s烘干,使所制备湿膜中的部分有机溶剂得以挥发,从而得到所要求薄膜的干膜。将前期所制备的干模置于快速退火炉中,预处理温度为350℃,保温时间150s。将热解的薄膜退火处理,退火温度为450℃,保温时间都为250s,得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复,从而制得所需厚度的薄膜样品,制备的薄膜层数为10层。
实施例3
将混合的前驱体溶液均匀旋涂在清洗干净的玻璃衬底上。将衬底置于匀胶机的样品台上,将前驱体溶液滴在衬底上,为使溶液在衬底上得以充分扩散,须等待30s后打开真空泵,将衬底牢牢吸附在样品台上,启动匀胶机。将涂膜结束的薄膜样品快速转移到125℃的电热板上60s烘干,使所制备湿膜中的部分有机溶剂得以挥发,从而得到所要求薄膜的干膜。将前期所制备的干模置于快速退火炉中,预处理温度为400℃,保温时间150s。将热解的薄膜退火处理,退火温度为500℃,保温时间都为250s,得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复,从而制得所需厚度的薄膜样品,制备的薄膜层数为10层。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (1)
1.一种BiFeO3和Bi2WO6复合薄膜的制备方法,其特征在于,具体步骤如下:
(1)BiFeO3薄膜前驱体溶液配制:首先用电子天平按照各溶质的摩尔计量比进行称取,硝酸铁与硝酸铋的摩尔比为1:1.1;用移液管量取体积比为1:3的乙二醇和冰乙酸作为溶剂,将上述溶质和溶液置于磁力搅拌器上搅拌12小时,直至溶质全部溶解,待溶液搅拌均匀后,量取与硝酸铋摩尔比为1:1的乙酰丙酮作为螯合剂加入其中,在磁力搅拌器上匀速搅拌12小时,得到暗红色半透明溶液,最后再补充乙二醇和冰乙酸,控制溶液浓度为0.3mol/L,pH值在0.3-0.4,将所得的半透明暗红色溶液置于常温下静置24小时,得到制备BiFeO3薄膜样品所需的前驱体溶液;
(2)Bi2WO6薄膜前驱体溶液的配制:用电子天平称取摩尔比为1:2的钨酸铵和硝酸铋,将上述溶质溶解在去离子水中,量取钨酸铵摩尔比为1:1的乙酰丙酮作为螯合剂,去离子水调节溶液浓度为0.3mol/L,用硝酸调节pH值在0.3-0.4;将上述溶液放在磁力搅拌器中搅拌12小时,得到澄清透明的溶液,常温静止24小时,得到Bi2WO6薄膜前驱体溶液;
(3)将BiFeO3和Bi2WO6溶液按照摩尔比1:1混合搅拌24小时,得到混合的Bi3WFeO9前驱体溶液;
(4)将混合的前驱体溶液均匀旋涂在清洗干净的玻璃基体上;
(3)湿膜烘干:将涂膜结束的薄膜样品快速转移到100-150℃的电热板上60s烘干;
(4)预处理:将前期所制备的干模置于快速退火炉中,预处理温度为300-400℃,保温时间100-200s;
(5)最终退火:将预处理好的薄膜在快速退火炉中退火,退火温度为400-500℃,保温时间都为200-300s,得到Bi3WFeO9晶态薄膜;
(6)将湿膜的制备和热处理成膜两个阶段重复,从而制得所需厚度的薄膜样品,制备的薄膜层数为10层。
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