CN107117831A - 一种wo3纳米片阵列的制备方法 - Google Patents
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
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- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 abstract description 5
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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6h,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30min,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 (2)
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,100~220℃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。
(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。
所述化学试剂纯度均为化学纯以上纯度。
2.根据权利要求1所述的一种制备WO3纳米片阵列的方法,其特征在于:步骤(1)中的基底材料为FTO导电玻璃、硅片、碳布中的一种。
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