CN104022189A - 一种制备ZnO/ZnS复合光电薄膜的方法 - Google Patents
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Abstract
一种制备ZnO/ZnS复合光电薄膜的方法,属于半导体薄膜制备技术领域。本发明通过如下步骤得到:首先清洗基片,然后将ZnO、CH4N2S放入溶剂中,采用旋涂法在基片上得到前驱体薄膜,烘干,放入有水合联氨的可密闭容器中,使前驱体薄膜样品不与联氨接触,最后进行干燥,得到ZnO/ZnS复合光电薄膜。本发明不需要高温高真空条件,对仪器设备要求低,生产成本低,生产效率高,易于操作,所得ZnO/ZnS复合光电薄膜有较好的连续性和均匀性。这种新工艺容易控制目标产物的成分和结构,为制备高性能的ZnO/ZnS复合光电薄膜提供了一种成本低、可实现工业化的制备方法。
Description
技术领域
本发明属于无机半导体薄膜制备技术领域,尤其涉及以氧化锌、硫脲为原料的一种制备ZnO/ZnS复合光电薄膜的方法。
背景技术
近年来,纳米结构ZnO和ZnS材料引起了人们的广泛关注,与其他材料相比,它们具有更好的热导电性、更强的力学韧性、更高的发光效率、更宽的发光频谱等优点。作为纳米体系之一的异质结构有序阵列体系成为了纳米材料领域研究的热点,特别是ZnO/ZnS复合异质结构,成了研究热点之一。
ZnO 是宽禁带3. 2 eV 的 n 型半导体材料,具有光电和光催化活性,在可见区有一定的吸收作用。ZnS 也是一种宽禁带的半导体材料,其禁带宽度为 3. 7eV~3. 8 eV。作为光催化剂,ZnO 和 ZnS 具有相同的缺陷,即在紫外区会发生光腐蚀,光稳定性差,导致光催化活性降低,并且具有较快的电子-空穴复合率。因此,对它们进行一定的修饰是人们十分关注的研究课题。已有研究表明,ZnO 和 ZnS 的光激发阈值较高,光活性较低,但是当二者结合在一起时,会产生一种比它们的光激发阈值都低的材料,可使得光激发更加容易。因此,将 ZnO 和 ZnS 复合往往可以提高复合材料的光催化性能。
目前,合成纳米 ZnO 和 ZnS 的方法较多,主要有溶胶-凝胶法、微乳液法、气相沉淀法、水热法、化学沉淀法以及均匀沉淀法。这些方法或对实验仪器和合成条件要求比较苛刻,或合成产物形貌较难控制,尺寸不一。本实验采用旋涂-化学共还原法制备ZnO/ZnS复合光电薄膜。
如前面所述方法一样,其它方法也有不同的缺陷。与本发明相关的还有如下文献:
[1] Guo P, Jiang J, Shen S, et al. ZnS/ZnO heterojunction as photoelectrode: Type II band alignment towards enhanced photoelectrochemical performance[J]. International Journal of Hydrogen Energy, 2013, 38(29): 13097-13103.
先通过硫化后水浴法合成ZnS/ZnO,价带偏移量的值(VBO)和导带偏移量(CBO)分别为0.96 eV和1.25 eV。异质结具有特殊电子结构有助于降低界面的能量势垒,提高光生电流。
[2] Hong E, Kim J H. Oxide content optimized ZnS–ZnO heterostructures via facile thermal treatment process for enhanced photocatalytic hydrogen production[J]. International Journal of Hydrogen Energy, 2014, 39(19): 9985-9993.
采用沉淀法合成ZnS纳米粉,然后通过控制热处理温度和通入氧气的压力来合成 ZnS/ZnO,制备的ZnS/ZnO复合结构显示更高的光催化制氢的性能比硫化锌、氧化锌纯物质。
[3] Brayek A, Ghoul M, Souissi A, et al. Structural and optical properties of ZnS/ZnO core/shell nanowires grown on ITO glass[J]. Materials Letters, 2014, 129: 142-145.
ZnO 纳米线通过电沉积在ITO玻璃上,然后沉浸入Na2S水溶液中转化为ZnS,最后通过去离子水、酒精清洗吹干得到目标产物。做得产物的禁带宽度在ZnO和ZnS之间。
[4] Sookhakian M, Amin Y M, Basirun W J, et al. Synthesis, structural, and optical properties of type-II ZnO–ZnS core–shell nanostructure[J]. Journal of Luminescence, 2014, 145: 244-252.
Na2S 和Zn(CH3COO)2.2H2O以1:1的比例,大力搅拌个半小时然后溶解于双蒸馏水中合成ZnS,然后通过直接加热或者通过添加氢氧化钠调节PH后在热处理。当PH>6时,产生ZnO:ZnS目标产物。
[5] 冯仕, 李金钗, 冯秀丽. ZnO/ZnS 核-壳纳米杆的制备及其光学性质[J]. 武汉大学学报: 理学版, 2009 (5): 535-538.
用溶液法在镀有ZnO缓冲层的硅衬底上制备出定向ZnO纳米杆阵列,然后再通过硫代乙酰胺 (TAA)辅助硫化法将氧化锌一维纳米结构转化为ZnO/ZnS的核-壳纳米结构。研究了样品的结构、形貌和光学性质,结果表明,ZnO/ZnS核-壳纳米杆的带边发光峰比ZnO纳米杆有显著增强,且峰位蓝移。
发明内容
本发明为解决现有技术的不足,而发明了一种不同与现有的制备技术。
本发明采用旋涂还原法合成ZnO/ZnS复合薄膜材料,采用钠钙玻璃片或硅片为基片,以ZnO和CH4N2S为原料,去乙醇为溶剂,先旋涂制备一定厚度的前驱体薄膜,以水合联氨为还原剂,在密闭反应釜内低温加热,使前驱体薄膜还原并发生合成反应得到目标产物。
本发明的具体制备方法包括如下顺序的步骤:
a. 进行基片的清洗,将大小为2mm×2mm玻璃基片或硅基片放入体积比HCl:蒸馏水=1:50的溶液中,加热煮沸30 min;再将基片放入体积比双氧水:HCl=1:1的溶液中,水浴加热90℃保温30 min;再在蒸馏水中将基片用超声波振荡10min;将上述得到的基片排放在玻璃皿中送入烘箱中烘干供制膜用。
b. 将ZnO和CH4N2S放入溶剂中,使溶液中的物质均匀混合。具体地说,可以将1.06~2.13份ZnO、1.0~2.0份CH4N2S放入60~240份的溶剂中,使溶液中的物质均匀混合,其中溶剂为乙醇。
c. 可以将上述溶液滴到放置在匀胶机上的基片上,再启动匀胶机以200~3500转/分旋转一定时间,使滴上的溶液涂布均匀后,并对基片进行烘干后,再次重复滴上前述溶液和旋涂后再烘干,如此重复4~8次,于是在基片上得到了一定厚度的前驱体薄膜样品。
d. 将步骤c所得前驱体薄膜样品置于支架上,放入有水合联氨的可密闭容器,使前驱体薄膜样品不与联氨接触。水合联氨放入量为60.0~105.0份。将上述装有前驱体薄膜样品的密闭容器放入烘箱中,加热至220℃~360℃之间,保温时间20~40小时,然后冷却到室温取出。
e. 将步骤d所得产物,进行自然干燥后,即得ZnO/ZnS复合光电薄膜。
本发明不需要高温高真空条件,对仪器设备要求低,生产成本低,生产效率高,易于操作。所得ZnO/ZnS复合光电薄膜有较好的连续性和均匀性,这种新工艺容易控制目标产物的成分和结构,为制备高性能ZnO/ZnS复合光电薄膜提供了一种低成本、可实现大规模的工业化生产的方法。
附图说明
图1是加热220℃保温时间为20h,所得ZnO/ZnS复合光电薄膜的XRD图谱,结果表明所得ZnS 沿 (111)、 (220) 、(311)晶面生长;ZnO沿(100)、(002)、(101)晶面生长。
具体实施方式
实施例1
a. 基片的清洗:如前所述进行清洗玻璃基片(大小为2mm×2mm)。
b. 将 1.06份ZnO和1份CH4N2S放入玻璃瓶中,加77.037份乙醇,利用超声波振动30min以上,使溶液中的物质均匀混合。
c. 将上述溶液滴到放置在匀胶机上的玻璃基片上,再启动匀胶机,匀胶机以200转/分转动5秒,以3000转/分旋转15秒,使滴上的溶液涂布均匀后,对基片进行烘干后,再次重复滴上前述溶液和旋涂后再烘干,如此重复8次,于是在基片上得到了一定厚度的前驱体薄膜样品。
d. 将上述工艺所得的前驱体薄膜样品放入可密闭的容器,并放入77.037份水合联氨,前驱体薄膜样品置于支架上使其不与联氨接触, 将装有前驱体薄膜样品的密闭容器放入烘箱中,加热至220℃,保温时间20小时,然后冷却到室温取出。
e. 将上述步骤d所得产物,进行自然干燥后,即得到ZnO/ZnS复合光电薄膜。
Claims (5)
1.一种制备ZnO/ZnS复合光电薄膜的方法,包括如下顺序的步骤:
a. 玻璃基片或硅基片的清洗;
b. 将1.06~2.13份ZnO、1.0~2.0份CH4N2S放入60~240份的溶剂中,使溶液中的物质均匀混合;
c. 制作外部均匀涂抹步骤b所述溶液的基片并烘干,得到前驱体薄膜样品;
d. 将步骤c所得前驱体薄膜样品置于支架上,放入有水合联氨的可密闭容器中,使前驱体薄膜样品不与联氨接触, 将装有前躯体薄膜样品的密闭容器放入烘箱中,加热至220℃~360℃之间,保温时间20~40h小时,然后冷却到室温取出;
e. 将步骤d所得产物,进行自然干燥,得到ZnO/ZnS复合光电薄膜。
2.如权利要求1所述的一种制备ZnO/ZnS复合光电薄膜的方法,其特征在于:步骤a所述清洗,是将大小为2mm×2mm玻璃基片或硅基片,先放入体积比HCl:蒸馏水=1:50的溶液中加热煮沸30 min;再将基片放入体积比双氧水:HCl=1:1的溶液中,水浴加热90℃保温30 min;再在蒸馏水中将基片用超声波振荡;将上述得到的基片排放在玻璃皿中送入烘箱中烘干供制膜用。
3.如权利要求1所述的一种制备ZnO/ZnS复合光电薄膜的方法,其特征在于:步骤b所述溶剂为乙醇。
4.如权利要求1所述的一种制备ZnO/ZnS复合光电薄膜的方法,其特征在于:步骤c所述均匀涂布的基片,是通过匀胶机旋涂,匀胶机以200~3500转/分旋转,然后对基片进行烘干后,再次如此重复2~15次,得到了一定厚度的前驱体薄膜样品。
5. 如权利要求1所述的一种制备ZnO/ZnS复合光电薄膜的方法,其特征在于:步骤d所述密闭容器内放入60.0~105.0份水合联氨。
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