CN106824214B - FeSe/BiVO4复合光催化剂及制备方法 - Google Patents
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Abstract
本发明涉及光催化技术，尤其涉及FeSe/BiVO4复合光催化剂及制备方法，该催化剂将FeSe纳米棒沉积在BiVO4颗粒表面，该制备方法为：化学沉淀法制备BiVO4颗粒；固相烧结法制备FeSe块状物；超声剥离法制备FeSe纳米棒；BiVO4和FeSe混合后分散在乙醇中；上述溶液蒸发得到FeSe/BiVO4复合光催化剂。本发明将BiVO4与FeSe复合，光生电子将吸附在FeSe表面的O2还原为氧自由基，剩余的空穴将‑OH氧化为羟基自由基。氧自由基和羟基自由基将有机污染物分解为二氧化碳和水。因此，FeSe与BiVO4复合后能够有效提高其光催化性能，且FeSe价格较低，整个制备工艺简单，易推广。
Description
技术领域
本发明涉及光催化技术领域，尤其涉及一种用于降解有机物的FeSe/BiVO4复合光催化剂及制备方法。
背景技术
光催化技术是从上世纪70年代逐步发展起来的在能源和环境领域有着重要应用前景的绿色技术。该技术能通过光催化剂光解水产生氢气和氧气，能使有机污染物发生氧化还原分解反应，降解为CO2、H2O和无机离子等小分子物质。当前，TiO2是被用来研究最多的光催化剂。但由于TiO2光催化剂带隙较宽（3.2eV），只能被占太阳光4%能量的紫外光激发。因此，为了充分有效利用太阳光能量，目前许多研究组正在开发新型可见光响应的半导体光催化剂，其中最重要的一类就是铋系半导体光催化剂。
铋系半导体光催化材料如 BiOX(X=Cl、Br、I)，Bi2O3, BiVO4, Bi2WO6, Bi2Mo3O12,Bi4Ti3O12,等由于其独特的晶体结构和电子结构，因而表现出较好的可见光催化活性，这是铋系半导体光催化材料的共同特点和显著优势，其中具有代表性的是 BiVO4，但是由于其光生电子-空穴复合高，电子-空穴复合会大大降低光催化活性。目前科学家用金、银、铂等贵金属与BiVO4复合能够有效降低其光生电子-空穴复合率，但贵金属价格昂贵不利于大面积推广。
发明内容
针对上述问题，本发明提供一种成本较低、效率高的FeSe/BiVO4复合光催化剂及制备方法。
为达上述发明目的，本发明采用的技术方案为：一种FeSe/BiVO4复合光催化剂，包括有FeSe纳米棒、BiVO4颗粒，FeSe纳米棒沉积在BiVO4颗粒表面。
较佳地，所述的BiVO4颗粒尺寸为0.5~5µm。
较佳地，所述的FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。
一种FeSe/BiVO4复合光催化剂制备方法，其特征在于：包括以下步骤：
S1，利用化学沉淀法制备BiVO4颗粒；
S2，采用固相烧结法制备FeSe块状物；
S3，采用超声剥离法制备FeSe纳米棒；
S4，将步骤S1制备的BiVO4和S3制备的FeSe按98:2混合后超声分散在无水乙醇中；
S5，将步骤S4分散好的溶液蒸发，得到FeSe/BiVO4复合光催化剂。
较佳地，所述步骤S3的超声剥离法为：将2mg尺寸为1µm 的FeSe块状物放入100mL无水乙醇中，接着在细胞粉碎机上超声粉碎2小时，得到长度为0.3~ 1.2 µm、直径为30 nmFeSe纳米棒。
较佳地，所述步骤S5具体为：将S4中分散好的溶液在油浴磁力搅拌器中于80℃搅拌加热8小时，随后在真空干燥箱中150℃烘干6小时，得到FeSe/BiVO4复合光催化剂。
本发明将BiVO4与FeSe复合，光生电子能够从BiVO4转移到FeSe表面上，电子能够将吸附在FeSe表面的O2还原为氧自由基。同时，剩余在BiVO4上的空穴将-OH氧化为羟基自由基。氧自由基和羟基自由基能够将有机污染物分解为二氧化碳和水。因此，FeSe与BiVO4复合后能够有效提高其的光催化性能，且FeSe价格较低，整个制备工艺简单，易推广。
附图说明
图1为本发明实施例制备FeSe纳米棒的场发射扫描电子显微镜图像；
图2为本发明实施例步骤S1中制备BiVO4的场发射扫描电子显微镜图；
图3为本发明实施例制备FeSe/BiVO4复合光催化剂的场发射扫描电子显微镜图；
图4为本发明实施例的光催化降解机理图；
图5为本发明实施例制备FeSe/BiVO4复合光催化剂用于降解有机物罗丹明B的效率图。
具体实施方式
为更好地理解本发明，下面将结合附图和具体实施方式对本发明的技术方案做进一步说明，参见图1至图5：
按本发明实施的FeSe/BiVO4复合光催化剂，进一步提高BiVO4的光催化效率，其材料由BiVO4颗粒表面沉积FeSe纳米棒制得。BiVO4颗粒大小为0.5~5µm，FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。图1为采用超声剥离法制得FeSe纳米棒的场发射扫描电子显微镜图像：FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。图2为颗粒尺寸为0.5~5µm 的BiVO4场发射扫描电子显微镜图像。图3为本发明实施例制备FeSe/BiVO4复合光催化剂的场发射扫描电子显微镜图，从图3可看出，FeSe纳米棒不均匀地分布在BiVO4颗粒表面。
按本发明实施的FeSe/BiVO4复合光催化剂制备方法，包括以下步骤：
S1，利用化学沉淀法制备BiVO4颗粒：将12 mmol Bi(NO3)3·5H2O 溶解在64 mLHNO3溶液（1 M/L）中，搅拌1.5小时。随后将12 mmol NH4VO3添加到上述溶液中继续搅拌1.5小时；接着将3 g 尿素添加到溶液中80 oC 加热 24；将沉淀用去离子水和酒精各清洗3次；最后在60 oC 干燥 24小时。
S2，采用固相烧结法制备FeSe块状物：Fe (Alfa, 99.99%) 和 Se (Alfa,99.99%) 粉末按1：1的比例在手套箱中混合均匀，并将其压成圆片；接着将圆片封装在充满氩气的石英管中；然后将其缓慢加热到700°C，并在 700°C 保温 24后随炉冷却到室温；将圆片研磨成粉末后再压片，并在700°C 保温 24小时，最后在400 °C 保温 36小时，将其研细，即得到FeSe粉末。
S3，采用超声剥离法制备FeSe纳米棒：将2mg尺寸为1µm 的FeSe块状物放入100mL无水乙醇中，接着在细胞粉碎机上超声粉碎2小时，得到长度为0.3~ 1.2 µm、直径为30 nmFeSe纳米棒。
S4，将步骤S1制备的BiVO4和S3制备的FeSe按98:2混合后超声分散在无水乙醇中；
S5，将S4中分散好的溶液在油浴磁力搅拌器中于80℃搅拌加热8小时，随后在真空干燥箱中150℃烘干6小时，得到FeSe/BiVO4复合光催化剂。
如图4，本发明工作机理图为：BiVO4与FeSe复合后，光生电子能够从BiVO4转移到FeSe表面上，电子能够将吸附在FeSe表面的O2还原为氧自由基。同时，剩余在BiVO4上的空穴将-OH氧化为羟基自由基。氧自由基和羟基自由基能够将有机污染物分解为二氧化碳和水。因此，FeSe与BiVO4复合后能够有效提高其的光催化性能。
通过降解罗丹明B来表征FeSe/BiVO4复合物的光催化性能，以罗丹明B在554 nm处的吸收峰来表征其浓度。将50mg的FeSe/BiVO4放入50mL浓度为10mg/L的罗丹明B溶液中搅拌1.5小时，随后用可见光照射溶液，每隔30分钟取一次溶液，并测量溶液的浓度。其结果如图5所示。从图5中可以得出，BiVO4与FeSe复合后其光催化性能得到了提高，大约为纯BiVO4的8倍。
Claims (6)
1.一种FeSe/BiVO4复合光催化剂，其特征在于：采用如下方法制备而成，所述包括以下步骤：S1，利用化学沉淀法制备BiVO4颗粒；S2，采用固相烧结法制备FeSe块状物；S3，采用超声剥离法制备FeSe纳米棒；S4，将步骤S1制备的BiVO4和S3制备的FeSe按98:2混合后超声分散在无水乙醇中；S5，将步骤S4分散好的溶液蒸发，得到FeSe/BiVO4复合光催化剂；所述FeSe/BiVO4复合光催化剂包括有FeSe纳米棒、BiVO4颗粒，FeSe纳米棒沉积在BiVO4颗粒表面。
2.根据权利要求1所述的FeSe/BiVO4复合光催化剂，其特征在于：所述的BiVO4颗粒尺寸为0.5~5µm。
3.根据权利要求1所述的FeSe/BiVO4复合光催化剂，其特征在于：所述的FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。
4.根据权利要求1所述的FeSe/BiVO4复合光催化剂制备方法，其特征在于：包括以下步骤：S1，利用化学沉淀法制备BiVO4颗粒； S2，采用固相烧结法制备FeSe块状物；S3，采用超声剥离法制备FeSe纳米棒；S4，将步骤S1制备的BiVO4和S3制备的FeSe按98:2混合后超声分散在无水乙醇中；S5，将步骤S4分散好的溶液蒸发，得到FeSe/BiVO4复合光催化剂。
5.根据权利要求4所述的FeSe/BiVO4复合光催化剂制备方法，其特征在于：所述步骤S3的超声剥离法为：将2mg尺寸为1µm 的FeSe块状物放入100mL无水乙醇中，接着在细胞粉碎机上超声粉碎2小时，得到长度为0.3~ 1.2 µm、直径为30 nm FeSe纳米棒。
6.根据权利要求4所述的FeSe/BiVO4复合光催化剂制备方法，其特征在于：所述步骤S5具体为：将S4中分散好的溶液在油浴磁力搅拌器中于80℃搅拌加热8小时，随后在真空干燥箱中150℃烘干6小时，得到FeSe/BiVO4复合光催化剂。
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