CN111097551B - 一种在光催化材料表面非对称性光沉积助催化剂的方法 - Google Patents
一种在光催化材料表面非对称性光沉积助催化剂的方法 Download PDFInfo
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Abstract
本发明涉及光催化材料领域,具体为一种在光催化材料表面非对称性光沉积助催化剂的方法。以各种粉体光催化材料为原材料,将样品加入到溶剂中进行超声分散,得到样品的悬浊液。然后上述悬浊液均匀分散到载玻片上,加热干燥。将胶带粘在有样品分散的载玻片正面,后将胶带揭下,放到溶剂中超声,得到一段有样品单层附着的胶带。将上述胶带放在含有牺牲剂和助催化剂前驱体的溶液中,用光源照射有样品附着的胶带面,进行光沉积,实现助催化剂在材料表面的非对称性沉积。本发明利用胶带对样品进行半包覆,实现助催化剂在光催化材料表面的非对称性沉积。从而,在光催化材料内部构建定向电场,使载流子可以定向迁移,提高载流子的分离效率。
Description
技术领域
本发明涉及光催化材料领域,具体为一种在光催化材料表面非对称性光沉积助催化剂的方法,利用胶带对样品进行半包覆,在后续光沉积助催化剂的过程中实现在光催化材料表面上助催化剂的非对称性沉积。
背景技术
光生载流子的分离是影响光催化效率的一个重要因素。材料内部的定向电场可以提高载流子的分离效率,但一般光催化材料内部鲜有定向电场存在。助催化剂的费米能级与光催化剂的费米能级往往不同,这一差异使得两者在接触界面形成不同于材料内部的能带结构,产生带弯,促进光生载流子的定向迁移,有助于光生载流子的分离。但是一般的助催化剂都是随机对称沉积在材料的表面,助催化剂材料表面的对称分布不利于定向电场的建立。
发明内容
本发明的目的在于提供一种在光催化材料表面非对称性光沉积助催化剂的方法,能够解决一般光催化材料不具备定向电场的问题,实现材料内部光生载流子的定向迁移,改善载流子分离效率低的缺点。
本发明的技术方案是:
一种在光催化材料表面非对称性光沉积助催化剂的方法,包括如下步骤:
(1)以各种粉体光催化剂为原材料,将样品加入到溶剂中进行超声分散,得到样品的悬浊液;
(2)上述悬浊液均匀分散到载玻片上,加热干燥;
(3)将胶带粘在有样品分散的载玻片正面,后将胶带揭下,放到溶剂中超声,得到一段有样品单层附着的胶带;
(4)将上述胶带放在含有牺牲剂和助催化剂前驱体的溶液中,用光源照射有样品附着的胶带面,进行光沉积,实现助催化剂在材料表面的非对称性沉积。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,各种粉体光催化剂为:金属氧化物TiO2或Cu2O,金属硫化物CdS或ZnS,金属氧和/或氮化物Ta3N5、TaON或LaTaON2,三元及以上复杂光催化材料SrTiO3或BiVO4。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,溶剂为去离子水、乙醇、甲醇、丙酮或异丙醇。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,胶带种类为透明胶带、双面胶带、绝缘胶带或导电胶带。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,胶带的面积为1mm2~100m2。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,按重量百分比计,含有牺牲剂和助催化剂前驱体的溶液成分含量如下:牺牲剂0.01%~99%,助催化剂前驱体0.0000001%~0.1%,其余为去离子水。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,牺牲剂为产氢牺牲剂或产氧牺牲剂,产氢牺牲剂为甲醇、三乙醇胺、乳酸或硫化钠/亚硫酸钠,产氧牺牲剂为Fe3+或碘酸钠;
助催化剂为产氢助催化剂或产氧助催化剂,产氢助催化剂为铂、金或铑,产氧助催化剂为二氧化锰、氧化钴或氧化铅;
产氢助催化剂前驱体为:氯铂酸、氯金酸或氯化铑,产氧助催化剂前驱体为:硫酸锰、硝酸钴或硝酸铅。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,光源为氙灯、汞灯、AM1.5或LED所发出光的波长与200nm到1200nm具有交集的连续或脉冲光源。
所述的在光催化材料表面非对称性光沉积助催化剂的方法,在进行光沉积处理时,光沉积的时间为1s~1000min,助催化剂质量与光催化剂质量之间的比例为0.01mg/10kg~10kg/1mg。
本发明的设计思想如下:
光催化剂的表面活性通常很低,很难进行光催化反应,因此通常需要在材料表面沉积一些助催化剂,这是由光催化剂的表面特性决定的。助催化剂的沉积可以改变光催化剂的表面活性和能带结构,但是一般的助催化剂都是随机沉积在材料的表面,助催化剂材料表面的对称分布不利于定向电场的建立。因此,通过助催化剂的非对称性沉积,在材料内部生成定向电场,实现载流子的定向迁移,促进载流子分离,增加材料的光催化效率。本发明考虑助催化剂的沉积位置,为解决载流子的分离效率迈出实质性的一步。
另外,本发明利用胶带将与胶带接触的样品进行半包覆,在样品未被包覆的一面沉积上助催化剂,被包覆的一面不沉积助催化剂,大量助催化剂在材料表面的非对称沉积,实现催化剂表面能带结构的空间非对称分布,人为在材料内部生成定向电场,实现光生载流子的定向迁移,从而增加载流子的分离效率。
本发明的优点及有益效果是:
1、本发明致力于解决一般光催化材料内部没有定向电场的缺点,通过助催化剂的非对称性沉积,在材料内部生成定向电场,进一步增加载流子的分离效率。
2、本发明所需的原材料可以为各类光催化材料,具有一定的普适性。
3、本发明所制备的材料具有高的载流子的分离效率。
附图说明
图1.金红石氧化钛分散到载玻片上后的主视图(a)和侧视图(b)。
图2.粘取载玻片上的金红石样品后胶带的主视图(a)和侧视图(b)。
图3.负载有金红石样品的胶带在用去离子水超声清洗之后的主视图(a)和侧视图(b)。
图4.非对称沉积MnO2的SrTiO3样品正面的扫描电子显微镜照片(SEM)。
图5.非对称沉积MnO2的SrTiO3样品背面的扫描电子显微镜照片(SEM)。
图6.非对称沉积Au的SrTiO3样品的扫描电子显微镜照片(SEM)。
具体实施方式
在具体实施过程中,本发明提供一种在光催化材料表面上非对称光沉积助催化剂的方法,以各种粉体光催化材料为原材料,将样品加入到溶剂中进行超声分散,得到样品的悬浊液。然后上述悬浊液均匀分散到载玻片上,加热干燥。将胶带粘在有样品分散的载玻片正面,后将胶带揭下,放到溶剂中超声,得到一段有样品单层附着的胶带。将上述胶带放在含有牺牲剂和助催化剂前驱体的溶液中,用光源照射有样品附着的胶带面,进行光沉积,实现助催化剂在材料表面的非对称性沉积。其中,具体的特征在于:
1、所述原材料为各种粉体光催化剂,如:TiO2、Cu2O等金属氧化物,CdS、ZnS等金属硫化物,Ta3N5、TaON、LaTaON2等金属(氧)氮化物,SrTiO3、BiVO4等三元及以上复杂光催化材料,光催化剂的粉体粒度为200nm~5μm。
2、所述的溶剂包括去离子水、乙醇、甲醇、丙酮、异丙醇等。
3、所述的胶带种类有透明胶带、双面胶带,绝缘胶带、导电胶带等。
4、所述的胶带的面积为1mm2~100m2(优选为10cm2~100cm2)。
5、所述的牺牲剂包括甲醇、三乙醇胺、乳酸、硫化钠/亚硫酸钠等产氢牺牲剂和Fe3 +、碘酸钠等产氧牺牲剂,产氢牺牲剂相对于溶液的质量分数为0.01%到99%(优选为10%~50%),产氧牺牲剂相对于溶液的质量分数为0.01%到10%(优选为0.1%~2%)。
6、所述的助催化剂包括铂、金、铑等产氢助催化剂和氧化锰、氧化钴、氧化铅等产氧助催化剂,助催化剂前驱体的加入量相对于溶液的质量分数为0.0000001%到0.1%(优选为0.001%~0.01%)。
7、所述的光源包括氙灯、汞灯、AM1.5、LED等所发出光的波长与200nm到1200nm具有交集的连续或脉冲光源。
8、在进行光沉积处理时,光沉积的时间为1s~1000min(优选为10min~100min)。
9、沉积助催化剂质量与光催化剂质量之间的比例为0.01mg/10kg~10kg/1mg(优选为0.01mg/10mg~0.1mg/1mg)。
下面结合实施例来详细说明本发明。
实施例1
本实施例中,称取金红石粉末100mg,将其放入盛有5ml无水乙醇的离心管中,超声30分钟形成悬浊液。超声结束后,滴加1ml上述悬浊液到在载玻片上,用加热台在60℃下进行干燥。然后用透明胶带粘在上述负载有样品的载玻片上,反复按压3~4次后,将胶带撕下,用去离子水反复冲洗。将上述胶带放入加满去离子水的烧杯中,超声20分钟后,用去离子水冲洗胶带,再将胶带放到盛满去离子水的烧杯中,重复上述过程2次。在石英池中加入25ml摩尔浓度0.5M的碘酸钠水溶液,再加入5ml浓度为1mg/ml的MnSO4水溶液。
用夹子夹住胶带,垂直放在石英池中。用氙灯垂直照射胶带正面,0.5小时后取出胶带,用去离子水冲洗后,干燥。
如图1所示,初始载玻片上的样品量很多。如图2所示,胶带只从载玻片上粘取部分样品。如图3所示,超声之后胶带上样品的负载量为单层。
实施例2
本实施例中,称取商业化钛酸锶粉末100mg,将其放入盛有5ml无水乙醇的离心管中,超声30分钟形成悬浊液。超声结束后,滴加1ml上述悬浊液到在载玻片上,用加热台在60℃下进行干燥。然后用透明胶带粘在上述负载有样品的载玻片上,反复按压3~4次后,将胶带撕下,用去离子水反复冲洗。将放入加满去离子水的烧杯中,超声20分钟后,用去离子水冲洗胶带,再将胶带放到盛满去离子水的烧杯中,重复上述过程2次。在石英池中加入25ml摩尔浓度0.5M的碘酸钠水溶液,再加入5ml浓度为1mg/ml的MnSO4水溶液。用夹子夹住胶带,垂直放在石英池中。用氙灯垂直照射胶带正面,1小时后取出胶带,用去离子水冲洗后,干燥。
如图4所示,由于受到光照射,所制备的样品的正面沉积大量的MnO2颗粒。如图5所示,由于样品背面被胶带包裹住,不能接触到溶液,所制备的样品的背面没有沉积MnO2颗粒。
实施例3
本实施例中,称取商业化钛酸锶粉末100mg,将其放入盛有5ml无水乙醇的离心管中,超声30分钟形成悬浊液。超声结束后,滴加1ml上述悬浊液到在载玻片上,用加热台在60℃下进行干燥。然后用透明胶带粘在上述负载有样品的载玻片上,反复按压3~4次后,将胶带撕下,用去离子水反复冲洗。将放入加满去离子水的烧杯中,超声20分钟后,用去离子水冲洗胶带,再将胶带放到盛满去离子水的烧杯中,重复上述过程2次。在石英池中加入10ml甲醇、20ml水,再加入1ml浓度为0.5mg/ml的HAuCl4水溶液。用夹子夹住胶带,垂直放在石英池中。用氙灯垂直照射胶带正面,0.5小时后取出胶带,用去离子水冲洗后,干燥。
如图6所示,通过胶带包裹然后进行光沉积,可以在SrTiO3样品上实现Au助催化剂的非对称性沉积。
实施例结果表明,本发明利用胶带对样品进行半包覆,实现助催化剂在光催化材料表面的非对称性沉积。从而,在光催化材料内部构建定向电场,使载流子可以定向迁移,提高载流子的分离效率。
Claims (1)
1.一种在光催化材料表面非对称性光沉积助催化剂的方法,其特征在于,称取商业化钛酸锶粉末100mg,将其放入盛有5ml无水乙醇的离心管中,超声30分钟形成悬浊液;超声结束后,滴加1ml上述悬浊液到在载玻片上,用加热台在60℃下进行干燥;然后用透明胶带粘在上述负载有样品的载玻片上,反复按压3~4次后,将胶带撕下,用去离子水反复冲洗;将放入加满去离子水的烧杯中,超声20分钟后,用去离子水冲洗胶带,再将胶带放到盛满去离子水的烧杯中,重复上述过程2次;在石英池中加入10ml甲醇、20ml水,再加入1ml浓度为0.5mg/ml的HAuCl4水溶液;用夹子夹住胶带,垂直放在石英池中;用氙灯垂直照射胶带正面,0.5小时后取出胶带,用去离子水冲洗后,干燥;通过胶带包裹然后进行光沉积,在SrTiO3样品上实现Au助催化剂的非对称性沉积。
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