CN107117831B - 一种wo3纳米片阵列的制备方法 - Google Patents
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- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 5
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
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Abstract
本发明公开了一种WO3纳米片阵列的制备方法。首先通过草酸、乙醇和六氯化钨溶剂热法在FTO、碳布、硅片表面生长带有氧缺陷的WO3‑x·H2O纳米片阵列薄膜,再在马弗炉中以一定的温度煅烧得到结晶性较好的WO3纳米片阵列。在基底上所制备的WO3呈现规则的、垂直取向的纳米片阵列,大幅提高了其比表面积,0.5mol/L Na2SO4电解质中,0.7个太阳光光强,1.2V的偏压下,WO3纳米片的光电流达到0.8mA/cm2。该方法操作简便、易于控制,制备的WO3纳米片阵列薄膜,具有大的比表面积、高的光电化学活性和稳定性。
Description
技术领域
本发明所属技术领域为光催化、光电化学材料技术领域,特别涉及WO3催化剂开发及制备方法。
背景技术
三氧化钨是一种多功能无机金属氧化物半导体材料。该材料具有优良的物理及化学性质,如光催化、光致变色、电致变色、场发射等性能,所以在光催化剂、电致变色智能窗和光电化学仪器等领域应用非常广阔。目前纳米WO3的制备方法可以概括为固相法、气相法和液相法,各种制备方法都具有一定的优缺点。常用的热蒸发法、化学气相沉积法、溅射法等面临着需要创造高温或真空环境,易造成环境污染以及操作过程繁杂等问题,而且制取的纳米WO3也有可能结晶体度低、纯度不高,进而影响纳米WO3的各种使用性能。综上所述,水热法因其设备廉价,操作简单及条件易调节等优点,目前被广泛用于纳米材料的制备。利用水热法制备氧化钨纳米材料,深入研究其综合性能,进而在推动纳米材料发展方面,具有重要的理论及实用意义
发明内容
本发明的目的是提供一种水热法制备WO3纳米片阵列,该方法操作简便、条件温和、易于操作,所制备的WO3纳米片阵列具有很高的光电化学性能。
具体步骤为:
(1)将0.1~1g的草酸溶解于10~60mL无水乙醇中,在真空手套箱中称取 0.1~0.5g六氯化钨。混合均匀后加入到容积为60mL的聚四氟乙烯反应釜中,然后将清洗干净的基底材料斜放入聚四氟乙烯反应釜中,100~240℃条件下反应6 h,自然冷却至室温后,分别用蒸馏水清洗基底材料表面,60℃真空干燥,待用。
(2)将步骤(1)合成的电极材料放入马弗炉中,以5℃/min的升温速率升温至300~600℃,退火100~150min,待其降到室温后取出,得到基底表面长有 WO3纳米片阵列的光电极。
所述基底材料为FTO导电玻璃、硅片、碳布中的一种。
所述化学试剂纯度均为化学纯以上纯度。
附图说明
图1为本发明实施例1不同水热反应温度制备的WO3纳米片阵列的XRD 谱。
图2为本发明实施例1制备WO3纳米片阵列的SEM图:(a)正面图,(b) 横截面
图3为本发明实施例1不同水热反应温度制备的WO3纳米片的光生电流曲线。
本发明WO3纳米片阵列展示出了优异的吸光性能和很强的光电化学响应,光生电流密度达到0.8mA/cm2,同时有较好的光稳定性,因此,WO3纳米片阵列作为一种可见光响应材料,在环境污染如降解染料、光催化处理污水,太阳能电池等方面具有很大的应用潜能。
具体实施方式
实施例1:
(1)将0.4g的草酸溶解于40mL无水乙醇中,在真空手套箱中称取0.2g 六氯化钨。混合均匀后加入到容积为60mL的聚四氟乙烯反应釜中,然后将清洗干净的FTO斜放入聚四氟乙烯反应釜中,180℃条件下反应6h,自来水冷却反应釜30min,用蒸馏水清洗FTO表面,60℃真空干燥,待用。
(2)将步骤(1)合成的电极材料放入马弗炉中,以5℃/min的升温速率升温至500℃,退火120min,待其降到室温后取出,得到FTO表面长有WO3纳米片阵列的光电极。
以所制备的WO3纳米片阵列光电极作为工作电极(面积为1cm2),辅助电极为铂电极,饱和甘汞电极(SCE)作为参比电极,0.5mol/L Na2SO4为支持电解质溶液,在太阳光模拟器(0.7个太阳的光强)下测试光电化学性能,从图3可以看出1.2V的偏压下,180℃反应的WO3纳米片的光电流达到0.52mA/cm2。
实施例2:
(1)将0.4g的草酸溶解于40mL无水乙醇中,在真空手套箱中称取0.2g 六氯化钨。混合均匀后加入到容积为60mL的聚四氟乙烯反应釜中,然后将清洗干净的碳布入聚四氟乙烯反应釜中,120℃条件下反应6h,自来水冷却30min,用蒸馏水清洗碳布表面,60℃真空干燥,待用。
(2)将步骤(1)合成的电极材料放入马弗炉中,以5℃/min的升温速率升温至400℃,退火120min,待其降到室温后取出,得到碳布基底表面长有WO3纳米片阵列的光电极。
以所制备的长有WO3纳米片阵列碳布作为工作电极(面积为1cm2),辅助电极为铂电极,饱和甘汞电极(SCE)作为参比电极,0.5mol/L Na2SO4为支持电解质溶液,在太阳光模拟器(0.7个太阳的光强)下测试光电化学性能,1.2V的偏压下,此方法合成的长有WO3纳米片阵列碳布的光电流达到0.8mA/cm2。
实施例3:
1)将0.8g的草酸溶解于40mL无水乙醇中,在真空手套箱中称取0.2g六氯化钨。混合均匀后加入到容积为60mL的聚四氟乙烯反应釜中,然后将清洗干净的硅片斜放入聚四氟乙烯反应釜中,180℃条件下反应6h,自来水冷却30 min,用蒸馏水清洗硅片表面,60℃真空干燥,待用。
(2)将步骤(1)合成的电极材料放入马弗炉中,以5℃/min的升温速率升温至600℃,退火120min,待其降到室温后取出,得到基底表面长有WO3纳米片阵列的光电极。
以所制备的长有WO3纳米片阵列碳布作为工作电极(面积为1cm2),辅助电极为铂电极,饱和甘汞电极(SCE)作为参比电极,0.5mol/L Na2SO4为支持电解质溶液,在太阳光模拟器(0.7个太阳的光强)下测试光电化学性能,1.2V的偏压下,此方法合成的长有WO3纳米片阵列碳布的光电流达到0.4mA/cm2。
以上实施例所述化学试剂纯度均为化学纯。
Claims (1)
1.一种WO3纳米片阵列的制备方法,其特征在于具体步骤为:
(1)将0.1~1g的草酸溶解于10~60mL无水乙醇中,在真空手套箱中称取0.1~0.5g六氯化钨;混合均匀后加入到容积为60mL的聚四氟乙烯反应釜中,然后将清洗干净的基底材料斜放入聚四氟乙烯反应釜中,100~180℃条件下反应6h,取出反应釜自然冷却后,用蒸馏水清洗基底材料表面,60℃真空干燥,待用;所述基底材料为FTO导电玻璃、硅片、碳布中的一种;
(2)将步骤(1)合成的电极材料放入马弗炉中,以5℃/min的升温速率升温至400~600℃,退火100~150min,待其降到室温后取出,得到基底表面长有WO3纳米片阵列的光电极;
以上所用到的化学试剂纯度均为化学纯以上纯度。
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