CN111215070A - 一种暴露高活性面氧化铁光电催化剂的制备方法 - Google Patents
一种暴露高活性面氧化铁光电催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种暴露高活性面的多孔氧化铁光电催化剂的制备方法,其步骤为:将(NH4)2Fe(SO4)2,CH3COONa•3H2O,Na2SO4置于水中,搅拌均匀;将所得溶液置于反应釜中,将经亲水处理的FTO玻璃垂直放入反应釜中,进行高温反应;反应结束后,将所得样品取出清洗干净,置于管式炉中,并通入氮气,控制管式炉在1小时内升温至550℃,保持2小时,所得样品清洗、干燥即得所述的催化剂。本发明制备的样品暴露了更多的催化活性晶面,与之对应的光电产氧性能有了一个很大的提升,与此同时制备工艺简单、成本低廉,因而具有广泛的应用价值和应用前景。
Description
技术领域
本发明属于光电催化材料技术领域,具体涉及一种暴露高活性面的多孔氧化铁光电催化剂的制备方法。
背景技术
随着全球气候变暖、能源短缺以及环境污染问题的出现,光电化学分解水作为一种能将清洁太阳能转化为化学能的方式而备受关注,高效光阳极是光电化学分解水技术的瓶颈和研究的热点。氧化铁半导体材料由于其带隙窄(2.2eV)、光电化学稳定性好、价廉无污染等优点成为光电化学分解水技术最具潜力的一种光阳极材料。但由于其光生载流子的寿命短、载流子迁移率低、电导率差和出氧动力不足等因素使得其光电化学性能与理论值{开启电势为0.4V(vs.RHE)、饱和电流为12.6mA/cm-2相差较大。
针对氧化铁的各种不足已经提出多种解决办法,例如构建异质结构,进行离子掺杂等;然而很少有人注意到直接优化氧化铁的结构,使之暴露更多的催化活性面也是提高氧化铁光电解水的重要途径。
发明内容
本发明的目的在于提供一种具有优秀光电性能且可循环稳定使用、合成成本低、工艺简单的暴露高活性面多孔氧化铁光电催化剂的制备方法。
实现本发明目的的技术方案是:一种暴露高活性面的多孔氧化铁光电催化剂的制备方法,包括如下步骤:
(1)将(NH4)2Fe(SO4)2,CH3COONa·3H2O,Na2SO4置于去离子水中,搅拌均匀;
(2)将步骤(1)所得溶液置于反应釜中,将经亲水处理的FTO玻璃垂直放入反应釜中,进行高温反应;
(3)反应结束后,将所得样品取出清洗干净,置于管式炉中,并通入氮气,控制管式炉在1小时内升温至550℃,保持2小时,所得样品清洗、干燥即得所述的催化剂。
较佳的,(NH4)2Fe(SO4)2,CH3COONa·3H2O,Na2SO4的摩尔比为1:2:1。
较佳的,步骤(2)中,高温反应的温度为100℃,反应时间为7h。
与现有技术相比,本发明的有益效果是:
与传统的氧化铁相比,本发明制备的样品暴露了更多的催化活性晶面,与之对应的光电产氧性能有了一个很大的提升,与此同时制备工艺简单、成本低廉,因而具有广泛的应用价值和应用前景。
附图说明
图1为本发明所述的实施例1与实施例2对比的线性伏安曲线图。
图2为本发明所述的实施例1(A)与实施例2(B)在FTO衬底上制备出薄膜的实物图。
图3为本发明所述的实施例2的SEM平面图。
图4为本发明所述的实施例2不同放大倍数的TEM图。
图5为本发明所述的实施例2的XRD图。
具体实施方式
下面结合附图和实施例对本发明进行详细的阐述。
本发明所述的一种暴露高活性面的多孔氧化铁光电催化剂的制备方法,包括如下步骤:
(1)将实验中所用到的烧杯、量筒用超声清洗机清洗干净;
(2)清洗FTO玻璃,去除表面的油脂以及其他污染物,用超声清洗机超声10分钟;
(3)将FTO玻璃做亲水处理;
(4)称量原料0.784g的(NH4)2Fe(SO4)2,0.544g CH3COONa·3H2O,0.284g Na2SO4置于20mL去离子水中,将混合液放在磁力搅拌器上搅拌约15分钟;
(5)将搅拌完成的反应溶液转移至50mL的聚四氟乙烯反应釜中,同时将亲水后的FTO玻璃垂直放入反应釜,在烘箱进行高温高压反应,100℃下水热生长7小时;
(6)待反应釜冷却至室温将样品取出,并用去离子水冲洗;
(7)将冲洗好的样品放入管式炉中,并通入氮气,同时将管式炉设置为1小时升温至550℃,保持2小时,等待温度自然降至室温。
(8)将取出后的样品用去离子水冲洗数遍,并放入干燥箱中烘干。
本实验所用原料为:(NH4)2Fe(SO4)2(分析纯)、CH3COONa·3H2O(分析纯)、Na2SO4(分析纯),利用水热法以及管式炉氮气退火处理制备暴露高活性面氧化铁光电催化剂。
使用上海辰华CHI660E电化学工作站进行测试,在三电极系统中,使用饱和Hg/HgO电极作为参比电极,使用Pt丝电极作为对电极,我们合成的一种新型氧化铁样品作为工作电极。1M氢氧化钾溶液作为电解液,300W氙灯为光源。在开关光条件下线性伏安曲线。采用X射线衍射仪(XRD)对样品进行物相结构分析;采用扫描电子显微镜(SEM)和透射电子显微镜(TEM)观察制备化合物样品的表面形貌进行性能表征。
本发明的原理是:首先我们知道,氧化铁半导体材料由于其带隙窄(2.2eV)、光电化学稳定性好、价廉无污染等优点成为光电化学分解水技术最具潜力的一种光阳极材料,但由于其光生载流子的寿命短、载流子迁移率低、电导率差和水氧化动力不足等因素严重限制了其发展。有研究表明,氧空位的引入可以有效地调整电子结构,大大提高金属氧化物半导体的固有电导率。所以说适当浓度的氧空位有利于提高催化活性,提高光电极的光电化学性能,而且氧空位的浓度在氧化铁中通常可以由煅烧温度和气氛来决定。同时,研究具有特定晶面的氧化铁纳米材料的催化性能是发展更高效的氧化铁光电极的另一个重要途径。理论研究表明,氧化铁晶面的催化性能依次为{113}>{104}>{001},因此我们需要制备出暴露更多活性晶面的氧化铁纳米结。
基于以上考虑,本发明通过氮气,控制管式炉在1小时内升温至550℃,保持2小时,设计出了一种新型方案用以合成独特的多孔钻石状交错排列的氧化铁纳米棒阵列,该阵列相对于用传统方法制备的普通矩形状氧化铁纳米棒阵列,具有更为适当的氧空位浓度和{012}、{104}两个活性良好的晶面,从而大大提高了氧化铁的光电化学水氧化能力。
实施例1
传统氧化铁的制备:
(1)将实验中所用到的烧杯、量筒用超声清洗机清洗干净;
(2)清洗FTO玻璃,去除表面的油脂以及其他污染物,用超声清洗机超声10分钟;
(3)将FTO玻璃做亲水处理;
(4)称量原料0.811g的FeCl3·6H2O置于20mL去离子水中,并加入20uL HCl,将混合液放在磁力搅拌器上搅拌至完全溶解;
(5)将搅拌均匀的反应溶液转移至50mL的聚四氟乙烯反应釜中,同时将亲水后的FTO玻璃垂直放入反应釜,在烘箱进行高温高压反应,100℃下水热生长6小时;
(6)待反应釜冷却至室温将样品取出,并用去离子水冲洗;
(7)将冲洗好的样品放入管式炉中,并通入氮气,同时将管式炉设置为1小时升温至550℃,保持2小时,等待温度自然降至室温。
(8)将取出后的样品用去离子水冲洗数遍,并放入干燥箱中烘干。
实施例2
高活性氧化铁的制备
(1)将实验中所用到的烧杯、量筒用超声清洗机清洗干净;
(2)清洗FTO玻璃,去除表面的油脂以及其他污染物,用超声清洗机超声10分钟;
(3)将FTO玻璃做亲水处理;
(4)称量原料0.784g的(NH4)2Fe(SO4)2,0.544g CH3COONa·3H2O,0.284g Na2SO4置于20mL去离子水中,将混合液放在磁力搅拌器上搅拌约15分钟;
(5)将搅拌完成的反应溶液转移至50mL的聚四氟乙烯反应釜中,同时将亲水后的FTO玻璃垂直放入反应釜,在烘箱进行高温高压反应,100℃下水热生长7小时;
(6)待反应釜冷却至室温将样品取出,并用去离子水冲洗;
(7)将冲洗好的样品放入管式炉中,并通入氮气,同时将管式炉设置为1小时升温至550℃,保持2小时,等待温度自然降至室温。
(8)将取出后的样品用去离子水冲洗数遍,并放入干燥箱中烘干。
图1为本发明所述的实施例1与实施例2对比的线性伏安曲线图。从图中可以看出在开光情况下实施例2在同等电压下可获得更大的电流。
图2为本发明所述的实施例1(A)与实施例2(B)在FTO衬底上制备出薄膜的实物图。
图3为本发明所述的实施例2的SEM平面图,传统的氧化铁多即实施例1为矩形纳米阵列,通过实施例2制备的氧化铁从图中可以观测到呈非均匀的菱形纳米阵列。
图4为本发明所述的实施例2的TEM图,传统氧化铁即实施例1的TEM大多只能观测到(116)晶面,而通过实施例2制备的氧化铁从图中可以观测到较难暴露出来的(104)与(012)高活性晶面。
图5为本发明所述的实施例2的XRD图,XRD的测试结果也很好地佐证了TEM的测试结果,从图中很清楚地观测到了高活性的(012)与(104)晶面峰。
Claims (3)
1.一种暴露高活性面的多孔氧化铁光电催化剂的制备方法,其特征在于,包括如下步骤:
(1)将 (NH4)2Fe(SO4)2,CH3COONa•3H2O,Na2SO4置于水中,搅拌均匀;
(2)将步骤(1)所得溶液置于反应釜中,将经亲水处理的FTO玻璃垂直放入反应釜中,进行高温反应;
(3)反应结束后,将所得样品取出清洗干净,置于管式炉中,并通入氮气,控制管式炉在1小时内升温至550℃,保持2小时,所得样品清洗、干燥即得所述的催化剂。
2.如权利要求1所述的方法,其特征在于,(NH4)2Fe(SO4)2,CH3COONa•3H2O,Na2SO4的摩尔比为1:2:1。
3.如权利要求1所述的方法,其特征在于,高温反应温度为100℃,反应时间为7h。
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