CN106929830A - 一种高温下纳米结构可控的金属氧化物半导体薄膜电极材料的制备方法 - Google Patents
一种高温下纳米结构可控的金属氧化物半导体薄膜电极材料的制备方法 Download PDFInfo
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Abstract
本发明公开一种高温下纳米结构可控的金属氧化物半导体薄膜电极材料的制备方法。本发明以钛片为导电基底、钛片表面通过水热法生长羟基氧化铁纳米棒、利用葡萄糖为碳源在高温下合成纳米结构可控的复合电极材料碳层包覆的钛掺杂三氧化二铁纳米棒,即C/Ti‑Fe2O3。所述电极材料包括钛金属片和三氧化二铁纳米棒、碳层。所述碳层包覆在三氧化二铁纳米棒表面,在高温下能有效维持纳米棒的微观形貌,显著改善电极材料的光电化学性能。可应用于太阳能光伏电池制备、光电化学传感器构建以及光催化水分解制氢、光催化降解有机污染物等领域。
Description
技术领域
本发明涉及一种高温下合成纳米结构可控的金属氧化物半导体薄膜电极材料的制备方法,所制备的纳米结构金属氧化物半导体薄膜电极材料具有光电化学性能,可应用于太阳能光伏电池制备、光电化学传感器构建以及光催化水分解制氢、光催化降解有机污染物等领域。本发明属于纳米功能电极材料与绿色能源技术领域。
背景技术
能源短缺和环境恶化一直是人类社会面临的棘手问题,因此寻找清洁可再生能源是科研工作者的努力方向。光电化学分解水利用清洁可再生的太阳能分解水制取氢气,反应过程不会造成环境污染,氢气的使用亦不会对环境造成破坏(氢气燃烧生成水),因此,光电化学分解水技术在绿色能源可再生利用等方面引起了科研工作者的广泛关注。这一技术现已成为新能源、新材料、催化和环保等领域的研究热点之一。
金属氧化物因其性质稳定、来源丰富、成本低廉且无毒性等优点引起了人们的格外关注,其中金属氧化物半导体在太阳能光伏电池、光电化学传感器、光催化分解水制氢等领域显示出广泛的应用前景。具有一定微观形貌的纳米金属氧化物半导体,通常拥有更大的比表面积,能有效减少光生电子和空穴的复合,因而具有更优良的光电化学性能。目前,国内外科研工作者已成功制备出了具有各种微观形貌的纳米金属氧化物半导体,如:纳米线、纳米带、纳米片、纳米棒等,并对其光电化学性能进行了深入的研究。为了进一步提高纳米金属氧化物半导体的光电化学性能,提高其结晶度或对其掺杂改性是较常用的方法,而高温煅烧是最常用的处理手段之一。然而纳米金属氧化物半导体的微观结构经高温处理后往往会因为团聚遭到破坏,如何在高温下对纳米金属氧化物半导体的微观结构进行精确控制,获得具有一定微观结构的纳米金属氧化物半导体薄膜电极材料成为大家普遍关心和亟待解决的问题。
综上可知,研发一种成本低、方法简单、在高温下能有效控制纳米金属氧化物半导体电极材料的微观结构的合成方法,具有重要的科学意义和应用价值。
发明内容
本发明的目的在于提供一种高温下微观结构可控的纳米金属氧化物半导体薄膜电极材料的制备方法,具有成本低、制备简单的优点,且所得材料具备完好的纳米棒微观结构和高光电化学活性。
本发明的技术方案如下:
一种高温下微观结构可控的纳米金属氧化物半导体薄膜电极材料的制备方法,以钛片为导电基底、钛片表面通过水热法生长羟基氧化铁纳米棒、利用葡萄糖为碳源,在高温下合成纳米结构可控的复合电极材料碳层包覆的钛掺杂三氧化二铁纳米棒,即C/Ti-Fe2O3,具体包括如下步骤:
(1)配制铁盐和非铁无机盐的水溶液,搅拌分散均匀;
(2)将纯钛片用砂纸打磨光滑后,依次用自来水、超纯水、丙酮乙醇混合液和超纯水超声清洗干净,将其放置于聚四氟乙烯内胆水热反应釜中,将步骤(1)所得溶液加入到水热反应釜中,然后在80~200℃反应2~24h;
(3)步骤(2)反应完成后,自然冷却至室温,将钛片用去离子水和乙醇分别清洗干净,然后将钛片浸渍于葡萄糖溶液中,然后利用氩气将钛片吹干,50~80℃下真空干燥1~6h;
(4)将步骤(3)所得干燥钛片放置于管式炉中,在氩气气氛,600~900℃下煅烧10~60min,得到高温下纳米结构可控的金属氧化物半导体薄膜电极材料,即C/Ti-Fe2O3。
进一步地,所述的铁盐优选氯化铁、硝酸铁、硫酸铁中的一种或两种以上。
进一步地,所述的非铁无机盐优选硫酸钠或硝酸钠中的一种或两种。
进一步地,步骤(1)的铁盐浓度为0.05~1mol/L,非铁无机盐浓度为0.05~1mol/L。
进一步地,步骤(3)的浸渍,浸渍时间为10~60min,葡萄糖溶液浓度为0.1~0.5mg/mL。
本发明的有益效果在于:
本发明的制备方法工艺简单,条件容易控制,所得金属氧化物半导体薄膜电极为纳米结构,在导电基底钛表面生长的钛掺杂三氧化二铁纳米棒,在纳米棒表面进一步包覆碳层,制得电极的光电化学性能得到明显提高,光电化学性能优良,具有重要的科学意义和应用价值。
附图说明
图1为高温下未利用碳层控制纳米结构制得Ti-Fe2O3电极的微观照片。
图2为高温下利用碳层有效控制纳米结构制得C/Ti-Fe2O3电极的微观照片。
图3为C/Ti-Fe2O3电极和Ti-Fe2O3电极光电化学性能测试,即模拟太阳光下的线性扫描曲线:(a)C/Ti-Fe2O3电极材料(b)Ti-Fe2O3电极材料。
具体实施方式
下面结合具体实施例对本发明做进一步详细说明,但本发明并不限于此。
实施例1
C/Ti-Fe2O3的制备
(1)配制0.05mol/L的氯化铁和0.05mol/L硫酸钠的水溶液,搅拌分散20min;
(2)将纯钛片用砂纸打磨光滑后,依次用自来水、超纯水、丙酮乙醇混合液和超纯水超声清洗干净,将其放置于聚四氟乙烯内胆水热反应釜中,取20ml步骤(1)所得溶液加入到水热反应釜中,然后在120℃恒温箱中反应4h;
(3)步骤(2)反应完后,自然冷却至室温,将钛片用去离子水和乙醇清洗三遍,然后将钛片浸渍于0.1mg/ml的葡萄糖溶液中10min,浸渍完后,再利用氩气将钛片吹干,60℃下真空干燥2h;
(4)将步骤(3)干燥好的钛片放置于管式炉中,在氩气气氛,800℃下煅烧20min,即制得C/Ti-Fe2O3。
实施例2
C/Ti-Fe2O3的制备
(1)配制0.1mol/L的硝酸铁和0.1mol/L的硝酸钠的水溶液,搅拌分散20min;
(2)将金属钛片放置于聚四氟乙烯内胆水热反应釜中,取20ml步骤(1)所得溶液加入到水热反应釜中,然后在120℃恒温箱中反应4h;
(3)步骤(2)反应完后,自然冷却至室温,将钛片用去离子水和乙醇清洗三遍,然后将钛片浸渍于0.5mg/ml的葡萄糖溶液中30min,浸渍完后,再利用氩气将钛片吹干,80℃下真空干燥3h;
(4)将步骤(3)干燥好的钛片放置于管式炉中,在氩气气氛,900℃下煅烧40min,即制得C/Ti-Fe2O3。
实施例3
C/Ti-Fe2O3的制备
(1)配制1mol/L的硫酸铁和1mol/L的硫酸钠的水溶液,搅拌分散20min;
(2)将金属钛片放置于聚四氟乙烯内胆水热反应釜中,取20ml步骤(1)所得溶液加入到水热反应釜中,然后在80℃恒温箱中反应8h;
(3)步骤(2)反应完后,自然冷却至室温,将钛片用去离子水和乙醇清洗三遍,然后将钛片浸渍于0.2mg/ml的葡萄糖溶液中60min,浸渍完后,再利用氩气将钛片吹干,50℃下真空干燥6h;
(4)将步骤(3)干燥好的钛片放置于管式炉中,在氩气气氛,600℃下煅烧60min,即制得C/Ti-Fe2O3。
实施例4
C/Ti-Fe2O3的制备
(1)配制1mol/L的硫酸铁和1mol/L的硫酸钠的水溶液,搅拌分散20min;
(2)将金属钛片放置于聚四氟乙烯内胆水热反应釜中,取20ml步骤(1)所得溶液加入到水热反应釜中,然后在200℃恒温箱中反应2h;
(3)步骤(2)反应完后,自然冷却至室温,将钛片用去离子水和乙醇清洗三遍,然后将钛片浸渍于0.4mg/ml的葡萄糖溶液中50min,浸渍完后,再利用氩气将钛片吹干,70℃下真空干燥1h;
(4)将步骤(3)干燥好的钛片放置于管式炉中,在氩气气氛,600℃下煅烧60min,即制得C/Ti-Fe2O3。
实施例5
C/Ti-Fe2O3的制备
(1)配制1mol/L的硫酸铁和1mol/L的硫酸钠的水溶液,搅拌分散20min;
(2)将金属钛片放置于聚四氟乙烯内胆水热反应釜中,取20ml步骤(1)所得溶液加入到水热反应釜中,然后在80℃恒温箱中反应24h;
(3)步骤(2)反应完后,自然冷却至室温,将钛片用去离子水和乙醇清洗三遍,然后将钛片浸渍于0.2mg/ml的葡萄糖溶液中60min,浸渍完后,再利用氩气将钛片吹干,50℃下真空干燥6h;
(4)将步骤(3)干燥好的钛片放置于管式炉中,在氩气气氛,600℃下煅烧60min,即制得C/Ti-Fe2O3。
实施例6
C/Ti-Fe2O3的光电化学测试
将实施例1所制备的C/Ti-Fe2O3的金属片电极作为光阳极;以银氯化银电极作为参比电极,铂片电极作为辅助电极,共同组成三电极体系,链接到电化学工作站设备上:在石英电解槽中加入30ml的0.1mol/L的NaOH溶液;采用LSV测试手段,测试所得光电流强度较之未有碳层控制其纳米棒结构有约20%光电流的提高(偏压1.6V)。因此本发明在高温下有效控制纳米结构金属氧化物半导体薄膜电极材料的制备方法具有实际应用价值。
上述实施例并非是对于本发明的限制,本发明并非仅限于上述实施例,只要符合本发明要求,均属于本发明的保护范围。
Claims (5)
1.一种高温下纳米结构可控的金属氧化物半导体薄膜电极材料的制备方法,其特征在于,以钛片为导电基底、钛片表面通过水热法生长羟基氧化铁纳米棒、利用葡萄糖为碳源,在高温下合成纳米结构可控的复合电极材料碳层包覆的钛掺杂三氧化二铁纳米棒,即C/Ti-Fe2O3,具体包括如下步骤:
(1)配制铁盐和非铁无机盐的水溶液,搅拌分散均匀;
(2)将纯钛片用砂纸打磨光滑后,依次用自来水、超纯水、丙酮乙醇混合液和超纯水超声清洗干净,将其放置于聚四氟乙烯内胆水热反应釜中,将步骤(1)所得溶液加入到水热反应釜中,然后在80~200℃反应2~24h;
(3)步骤(2)反应完成后,自然冷却至室温,将钛片用去离子水和乙醇分别清洗干净,然后将钛片浸渍于葡萄糖溶液中,然后利用氩气将钛片吹干,50~80℃下真空干燥1~6h;
(4)将步骤(3)所得干燥钛片放置于管式炉中,在氩气气氛,600~900℃下煅烧10~60min,得到高温下纳米结构可控的金属氧化物薄膜电极材料,即C/Ti-Fe2O3。
2.如权利要求1所述的制备方法,其特征在于,所述的铁盐为氯化铁、硝酸铁、硫酸铁中的一种或两种以上。
3.如权利要求1所述的制备方法,其特征在于,所述的非铁无机盐为硫酸钠或硝酸钠中的一种或两种。
4.如权利要求1所述的制备方法,其特征在于,步骤(1)的铁盐浓度为0.05~1mol/L,非铁无机盐浓度为0.05~1mol/L。
5.如权利要求1所述的制备方法,其特征在于,步骤(3)的浸渍,浸渍时间为10~60min,葡萄糖溶液浓度为0.1~0.5mg/mL。
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