CN110342569B - 一种形貌可控的CuInS2纳米材料的高压制备方法 - Google Patents
一种形貌可控的CuInS2纳米材料的高压制备方法 Download PDFInfo
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Abstract
本发明的一种形貌可控的CuInS2纳米材料的高压制备方法属于纳米材料制备技术领域。以黄铜矿CuInS2纳米粒子为起始原料，在金刚石对顶砧中对起始原料加压至15～30GPa，然后将金刚石对顶砧卸压至常压，得到不同形貌的CuInS2纳米材料。本发明方法具有过程简单、合成时间短、室温合成、绿色环保、成本低、产品可重复性高等优点，得到的产物依然保持黄铜矿相结构、相纯度高、结晶性好，产品具有很好的光学吸收性质，这有利于太阳光的吸收和转换。
Description
技术领域
本发明属于纳米材料制备的技术领域，特别涉及一种制备薄膜状CuInS2纳米片的方法。
背景技术
作为一种重要的三元硫属半导体材料，黄铜矿CuInS2具有优异的性能，包括：1.45eV的直接带隙、超过105cm-1的光学吸收效率和高的光电转换效率，这使得CuInS2材料在各类太阳能电池中具有非常好的应用前景。
CuInS2半导体纳米晶的光电性能主要取决于形貌、尺寸和晶体结构。目前，通过湿化学方法制备的CuInS2半导体纳米晶形貌主要有球形粒子、纳米棒和纳米线等，关于微米级的二维CuInS2纳米片没有过报道。众所周知，二维材料具有落在量子限域效应范围内的超薄厚度及其独特的片状形貌，这对探索材料的新的物理现象和性能非常重要。因此，发展简单、方便的方法合成二维CuInS2纳米片具有重要意义。
发明内容
本发明要解决的技术问题是：克服背景技术存在的问题和缺陷，提供一种简单的、绿色的制备二维薄膜状CuInS2纳米片的方法，该方法以用溶剂热法合成的黄铜矿相CuInS2纳米晶为起始原料，采用金刚石对顶砧压机在高压下合成二维薄膜状CuInS2纳米片。并且通过控制向样品施加压力的大小合成出了准二维 CuInS2纳米片和一维多枝形CuInS2纳米线。
本发明的具体技术方案如下：
一种形貌可控的CuInS2纳米材料的高压制备方法，以黄铜矿CuInS2纳米粒子为起始原料，在金刚石对顶砧中对起始原料加压至15～30GPa，然后将金刚石对顶砧卸压至常压，得到不同形貌的CuInS2纳米材料。
本发明中，起始材料黄铜矿CuInS2纳米粒子的尺寸优选4.3nm。
本发明可以通过改变加压的压力控制产物的形貌，当对起始原料加压至30 GPa，再卸压至常压时，得到二维薄膜状CuInS2纳米片；当对起始原料加压至 25GPa，再卸压至常压时，得到准二维CuInS2纳米片；当对起始原料加压至15 GPa，再卸压至常压时，得到一维多枝状CuInS2纳米线。
本发明制备的二维薄膜状CuInS2纳米片的优点在于：本发明制备方法得到的产品，通过同步辐射XRD对样品的晶体结构进行表征，发现这些二维薄膜状 CuInS2纳米片依然保持黄铜矿相结构，并且相纯度较高、各成分分布均匀、结晶性好，这些二维薄膜状CuInS2纳米片具有1.82eV的电子能带隙，潜在地有利于太阳光的吸收和转换。此外，本发明制备方法能够通过控制对初始原料施加压力的大小来获得不同形貌的CuInS2纳米晶，具有过程简单、室温合成、合成时间短、可重复性高、清洁无污染等优点。
附图说明
图1是起始材料-黄铜矿CuInS2纳米粒子的透射电镜图片。
图2是起始材料-黄铜矿CuInS2纳米粒子的粒径分布图片。
图3是起始材料-黄铜矿CuInS2纳米粒子的高分辨电镜图片。
图4是起始材料-黄铜矿CuInS2纳米粒子的同步辐射XRD精修数据。
图5是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的透射电镜图片。
图6是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的铜(Cu)元素分布图片。
图7是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的铟(In)元素分布图片。
图8是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的硫(S)元素分布图片。
图9是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的高分辨电镜图片。
图10是起始材料为黄铜矿CuInS2纳米粒子，经过约30GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的同步辐射XRD精修数据。
图11是起始材料为黄铜矿CuInS2纳米粒子，经过约25GPa压力处理后，完全卸压至环境条件下时回收的准二维CuInS2纳米片的透射电镜图片。
图12是起始材料为黄铜矿CuInS2纳米粒子，经过约25GPa压力处理后，完全卸压至环境条件下时回收的准二维CuInS2纳米片的高分辨电镜图片。
图13是起始材料为黄铜矿CuInS2纳米粒子，经过约15GPa压力处理后，完全卸压至环境条件下时回收的一维多枝状CuInS2纳米线的透射电镜图片。
图14是起始材料为黄铜矿CuInS2纳米粒子，经过约15GPa压力处理后，完全卸压至环境条件下时回收的一维多枝状CuInS2纳米线的高分辨电镜图片。
图15是起始材料-黄铜矿CuInS2纳米粒子的吸收光谱。
图16是起始材料为黄铜矿CuInS2纳米粒子，经过30.0GPa压力处理后，完全卸压至环境条件下时回收的薄膜状CuInS2纳米片的吸收光谱。
具体实施方式
现结合下列实施例更加具体地描述本发明，如无特殊说明，所用试剂均为市售可获得的产品，并未加进一步提纯使用。
实施例1二维薄膜状CuInS2纳米片的制备
制备二维薄膜状CuInS2纳米片是在对称式金刚石对顶砧中进行的，利用对称式金刚石对顶砧进行加压，采用的金刚石砧面大小为0.4mm，T301不锈钢片作为垫片。金刚石压腔的样品组装过程如下：首先在垫片中心预压一个凹坑(厚度约为0.042mm)，然后在凹坑中心打一个直径为0.13mm的孔作为装载样品的空腔。将打好的垫片按照预压时的方位安装到金刚石对顶砧下砧面上，垫片小孔与两块相对的金刚石表面组成了样品腔。将用溶剂热法合成的黄铜矿CuInS2纳米粒子(粒径4.3nm)连同一小块红宝石放入金刚石对顶砧样品腔内，压力的标定是采用标准红宝石荧光标压的技术。对样品进行加压至约30GPa，然后将金刚石对顶砧压机卸压到常压，可以得到微米级别大小的薄膜状CuInS2纳米片。运用同样的方法，当施加的压力为约25GPa时，然后将金刚石对顶砧压机卸压到常压，得到准二维CuInS2纳米片；当施加的压力为约15GPa时，然后将金刚石对顶砧压机卸压到常压，得到一维多枝状CuInS2纳米线。
本实施例中所说的溶剂热法合成黄铜矿CuInS2纳米粒子，具体方法可以参见Highly Emissive and Color-Tunable CuInS2-Based Colloidal SemiconductorNanocrystals:Off-Stoichiometry Effects and Improved ElectroluminescencePerformance，Adv.Funct.Mater.2012，22，2081-2088。
实施例2二维薄膜状CuInS2纳米片的晶体结构和形貌表征
对样品进行同步辐射X光射线衍射、透射电镜和高分辨电镜表征。
图1是起始材料-黄铜矿CuInS2纳米粒子的透射电镜照片。图2是CuInS2纳米粒子的粒径统计图，显示出起始材料CuInS2纳米粒子平均粒径是4.3纳米。图3是起始材料CuInS2纳米粒子的高分辨电镜图片，测量的0.317nm和0.195nm 分别对应黄铜矿类型CuInS2的(112)和(220)面晶格间距。图4是初始的CuInS2纳米粒子同步辐射XRD数据精修，显示初始的样品为黄铜矿相结构。图5是起始材料经过30GPa压力处理后，卸压产品的透射电镜图，产品为薄膜状CuInS2纳米片，大小约为4*6μm。图6-8是卸压产品的元素分布图，显示Cu、In和S 元素均匀分布，构成CuInS2纳米片，表明初始材料在加压处理以后形成二维薄膜状CuInS2纳米片。图9是是卸压产品的高分辨电镜图，展现出0.317nm的黄铜矿相CuInS2的(112)面晶格间距。图10是卸压产品的同步辐射XRD数据精修，显示卸压产品仍保持初始的黄铜矿相结构，并且相纯度很高。
图11是起始材料经过25GPa压力处理后，卸压产品的透射电镜图，产品为准二维CuInS2纳米片，图12是相对应的卸压产品的高分辨电镜图；图13是起始材料经过15GPa压力处理后，卸压产品的透射电镜图，产品为一维多枝状 CuInS2纳米线，图14是相对应的卸压产品的高分辨电镜图，展现出CuInS2纳米线是由初始纳米粒子经高压处理熔融而来。
实施例3二维薄膜状CuInS2纳米片的光学性质
图15是起始材料黄铜矿相CuInS2纳米粒子的吸收光谱，图中显示黄铜矿相 CuInS2纳米粒子的能带间隙为2.03eV。图16是卸压产品二维薄膜状CuInS2纳米片的吸收光谱，图中显示二维薄膜状CuInS2纳米片的能带间隙为1.82eV。这说明高压合成的二维薄膜状CuInS2纳米片可以应用于太阳能电池中。
Claims (1)
1.一种形貌可控的CuInS2纳米材料的高压制备方法，以黄铜矿CuInS2纳米粒子为起始原料，在金刚石对顶砧中对起始原料加压至15~30GPa，然后将金刚石对顶砧卸压至常压，得到不同形貌的CuInS2纳米材料；步骤如下：利用对称式金刚石对顶砧进行加压，采用的金刚石砧面大小为0.4 mm，T301不锈钢片作为垫片；金刚石压腔的样品组装过程如下：首先在垫片中心预压一个厚度为0.042 mm的凹坑，然后在凹坑中心打一个直径为0.13 mm的孔作为装载样品的空腔，将打好的垫片按照预压时的方位安装到金刚石对顶砧下砧面上，垫片小孔与两块相对的金刚石表面组成了样品腔，将用溶剂热法合成的黄铜矿粒径4.3nm 的CuInS2纳米粒子连同一小块红宝石放入金刚石对顶砧样品腔内，压力的标定是采用标准红宝石荧光标压的技术；对样品进行加压至指定压力，然后将金刚石对顶砧压机卸压到常压，得到不同形貌的CuInS2纳米材料：当对起始原料加压至30 GPa，再卸压至常压时，得到二维薄膜状CuInS2纳米片；当对起始原料加压至25GPa，再卸压至常压时，得到准二维CuInS2纳米片；当对起始原料加压至15 GPa，再卸压至常压时，得到一维多枝状CuInS2纳米线。
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