CN106631816B - 一种原子级厚度二维钙钛矿纳米片的液相剥离制备方法 - Google Patents
一种原子级厚度二维钙钛矿纳米片的液相剥离制备方法 Download PDFInfo
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Abstract
本发明公开了一种原子级厚度二维钙钛矿纳米片的制备方法,采用液相剥离法,具体是先以层溶液法制备二维钙钛矿块体材料,再利用超声辅助剥离法,使用极性较低的剥离液以及在温和的剥离条件下将二维钙钛矿块体材料液相剥离成原子级厚度的纳米片。本发明制备方法方便易行,获得的二维钙钛矿超薄纳米片厚度可维持在单层至少数几个原子层之间。
Description
技术领域
本发明涉及一种二维钙钛矿纳米片的液相剥离制备方法,制得的纳米片具有单层至少数几个原子层的超薄厚度。
背景技术
二维材料是指电子仅可在两个维度的非纳米尺度上***(平面运动)的材料,典型的二维结构有纳米片、超晶格、量子阱等等。二维材料的量子限域特性赋予了它众多独特的物理化学性质,例如平面导电性、磁各向异性、可调控的能带结构及表面化学活性等,使其在催化、储能、生物、光电等诸多领域拥有巨大的应用潜力。当二维块体材料通过一定方法剥离成单层或者几个原子层厚度的超薄材料之时,巨幅增大的比表面积不仅增加了材料表面的物理和化学活性,还影响了因量子限域效应引起的二维波函数。因而,可以通过电子能带调控来修饰二维超薄材料的物理性质。随着剥离技术的日渐成熟,目前已有多种二维材料成功得以被分离成独立的纳米薄片,如石墨烯(Graphene)、过渡金属硫化物(TMDs)、金属有机框架材料(MOFs)等,它们均显示出了优异的物理化学特性。
研究者进行了各种方法尝试将二维块体材料剥离成原子级厚度的纳米薄片,液相剥离是其中的一个主要方法。液相剥离是在一定介质中通过超声手段将二维超薄纳米片从相应块体材料中剥离出来,从而得到二维超薄纳米片的胶体溶液的方法。通过剥离介质(溶剂及辅助试剂)的筛选可以有效地提高纳米片的剥离效率。液相剥离因其可以大量、均匀获得二维超薄纳米片而被广泛研究,现如今已成为一种较为成熟的剥离方法。目前,主要的液相剥离法有:离子***法、离子交换法和超声辅助剥离法。
近年来,一种有机-无机卤化铅类钙钛矿材料因其低缺陷密度、高载流子迁移率、发光效率及强光吸收能力而具备优异的光电性能,并成为如今最为火热的光伏材料。短短五、六年间,基于此类钙钛矿的太阳能电池的光电转换效率已从3.8%提升到22.1%。
理想的钙钛矿结构是立方晶体结构,由共顶点MX6八面体构成,它在三维无限延伸形成网状结构,半径较小的原子或分子A位于八面体间隙内。对于三维有机-无机钙钛矿材料,M通常是一种二价金属原子,X表示卤素原子,其中金属阳离子M位于八面体中心,而较小的有机小分子A(通常为甲胺)填充在六个相邻八面体围成的十二面体间隙内,结构通式为AMX3。而当有机阳离子分子链长度较大时,就可根据有机阳离子价态分别形成A2MX4(A为+1价)或AMX4(A为+2价)两种形式的二维层状类钙钛矿结构,其中A位阳离子一般为RNH3 +或NH3RNH3 2+(R为烷烃基或芳香烃基)。研究表明,对于R为烷烃基的情况,有机部分C原子个数大于3的时候即会出现钙钛矿由三维向二维的结构转变,而当R为芳香烃基时,有机部分主链C原子个数小于3的时候也能形成二维层状结构,如(C6H5C2H4)2PbX4。
对于二维AMX4型钙钛矿,其有机阳离子和无机卤化物阴离子之间以氢键N-H…X的方式结合,相邻的有机分子链之间通过范德华力结合,即钙钛矿层内各原子结合力大于层间结合力,但目前,尚无液相剥离法制备原子级厚度的二维钙钛矿超薄纳米片的报道。
发明内容
本发明的目的是提供一种基于液相剥离制备原子级厚度二维钙钛矿纳米片的方法,该方法是将原子级厚度二维材料的结构特性与钙钛矿材料的优异光电性能相结合,利用液相剥离技术,实现二维钙钛矿的超薄制备,得到原子级厚度的二维钙钛矿纳米片。
本发明的原子级厚度二维钙钛矿纳米片的制备方法,采用的是超声辅助剥离法,具体包括以下步骤:
1)在惰性气氛中,将金属卤化物粉末加入试管中,将试管口密封,通过注射器向试管内加入氢卤酸溶解上述粉末,再在溶液的上层注入无水甲醇溶液作为缓冲层,最后通过注射器注入反应所需的液态有机胺,所述的有机胺和金属卤化物的摩尔比为2:1;氢卤酸和甲醇过量即可;
2)将经步骤1)处理的反应液静置至少2个星期,在缓冲层析出片状晶体,将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的片状晶体按1mg/ml的比例分散在低极性剥离液中,在温和的条件下超声处理,即可得到原子级厚度的二维钙钛矿纳米片悬浮液。
上述的惰性气氛由手套箱达成,手套箱中氧含量、水含量均小于0.5ppm。
上述的金属卤化物为卤化铅PbX2,氢卤酸为HX,其中X为Br或I。
上述液态有机胺为苯乙胺,分子式为C6H5C2H4NH3。
上述析出的大片状晶体为二维钙钛矿块体层状材料,分子式为(C6H5C2H4)2PbX4,其中X为Br或I。已有文献表明,(C6H5C2H4NH3)2PbX4单层原子厚度在1.75nm左右。
本发明方法所用的方法主要含有两个步骤。第一步为层溶液法制备二维钙钛矿块体材料。第二步为块体材料的液相剥离过程,是本方法的主体步骤,形成的纳米片的形貌、厚度均由该反应来控制。本发明获得的二维钙钛矿纳米片其厚度可以维持在单层至少数几个原子层之间。
本发明反应过程中,剥离液采用甲苯溶液,是由于钙钛矿材料的强离子特性,剥离液的极性不能超过***。
本发明反应过程中,采用温和的超声条件是由于二维钙钛矿材料的机械易碎性,剧烈的超声条件极易造成二维钙钛矿的有机部份断裂。所述的温和条件通常是指功率60~240W,超声时长5~30min。
超声辅助剥离制备二维钙钛矿纳米片的方法,对外界环境、设备等要求低,制备十分简便。
附图说明
图1为原子级厚度二维钙钛矿纳米片的原子力显微电镜(AFM)照片。
具体实施方式
实施例1
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.367g PbBr2加入长直试管中,将试管口密封,通过注射器加入7.5ml HBr溶液溶解PbBr2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量白色片状的(C6H5C2H4NH3)2PbBr4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbBr4片状晶体按1mg/ml的比例分散在甲苯中,在60W的超声功率下超声5min,即可得到原子级厚度的(C6H5C2H4NH3)2PbBr4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbBr4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌保持完整四边形,纳米片厚度约为4.5nm。
实施例2
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.367g PbBr2加入长直试管中,将试管口密封,通过注射器加入7.5ml HBr溶液溶解PbBr2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量白色片状的(C6H5C2H4NH3)2PbBr4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbBr4片状晶体按1mg/ml的比例分散在甲苯中,在60W的超声功率下超声30min,即可得到原子级厚度的(C6H5C2H4NH3)2PbBr4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbBr4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌各异,已不能够保持完整四边形,纳米片厚度约为3.7nm。
实施例3
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.367g PbBr2加入长直试管中,将试管口密封,通过注射器加入7.5ml HBr溶液溶解PbBr2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量白色片状的(C6H5C2H4NH3)2PbBr4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbBr4片状晶体按1mg/ml的比例分散在甲苯中,在240W的超声功率下超声30min,即可得到原子级厚度的(C6H5C2H4NH3)2PbBr4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbBr4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌各异,已不能够保持完整四边形,纳米片厚度约为1.9nm。
实施例4
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.461g PbI2加入长直试管中,将试管口密封,通过注射器加入7.5ml HI溶液溶解PbI2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量橙黄色片状的(C6H5C2H4NH3)2PbI4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbI4片状晶体按1mg/ml的比例分散在甲苯中,在60W的超声功率下超声5min,即可得到原子级厚度的(C6H5C2H4NH3)2PbI4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbI4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌保持完整四边形,纳米片厚度约为5.1nm。
实施例5
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.461g PbI2加入长直试管中,将试管口密封,通过注射器加入7.5ml HI溶液溶解PbI2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量橙黄色片状的(C6H5C2H4NH3)2PbI4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbI4片状晶体按1mg/ml的比例分散在甲苯中,在60W的超声功率下超声30min,即可得到原子级厚度的(C6H5C2H4NH3)2PbI4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbI4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌各异,已不能够保持完整四边形,纳米片厚度约为3.5nm。
实施例6
1)在氧含量、水含量均小于0.5ppm的手套箱中,称取0.461g PbI2加入长直试管中,将试管口密封,通过注射器加入7.5ml HI溶液溶解PbI2粉末,再在溶液的上层通过注射器加入15ml无水甲醇溶液作为缓冲层,最后通过注射器注入0.3ml苯乙胺溶液;
2)将经步骤1)处理的反应液静置2个星期,反应期间会有大量橙黄色片状的(C6H5C2H4NH3)2PbI4晶体在缓冲层析出,到反应后期片状晶体逐渐增多。将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的(C6H5C2H4NH3)2PbI4片状晶体按1mg/ml的比例分散在甲苯中,在240W的超声功率下超声30min,即可得到原子级厚度的(C6H5C2H4NH3)2PbI4纳米片悬浮液。
将制备得到的(C6H5C2H4NH3)2PbI4纳米片悬浮液滴涂在SiO2/Si衬底上,对其进行原子力显微电镜(AFM)表征,纳米片形貌各异,已不能够保持完整四边形,纳米片厚度约为2.1nm。
以上所述仅为本发明的较佳实施例,并不用以限制本发明。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.原子级厚度二维钙钛矿纳米片的液相剥离制备方法,其特征在于,包括以下步骤:
1)在惰性气氛中,将金属卤化物粉末加入试管中,将试管口密封,通过注射器向试管内加入氢卤酸溶解上述粉末,再在溶液的上层注入无水甲醇溶液作为缓冲层,最后通过注射器注入反应所需的液态有机胺,所述的有机胺和金属卤化物的摩尔比为2:1;所述的金属卤化物为卤化铅PbX2,氢卤酸为HX,其中X为 Br或I,所述的液态有机胺为苯乙胺,分子式为C6H5C2H4NH2;
2)将经步骤1)处理的反应液静置至少2个星期,在缓冲层析出片状晶体,将析出的片状晶体取出,用无水***清洗2~3遍后,真空干燥;
3)将真空干燥得到的片状晶体按1mg/ml的比例分散在低极性剥离液中,在温和的条件下超声处理,即可得到原子级厚度的二维钙钛矿纳米片悬浮液;所述的低极性剥离液为甲苯溶液,所述的温和的超声条件为:功率为60~240 W,超声时长5~30 min。
2. 根据权利要求1所述的原子级厚度二维钙钛矿纳米片的液相剥离制备方法,其特征是,所述的惰性气氛由手套箱实现,制备过程在手套箱中进行,手套箱中氧含量、水含量均小于0.5 ppm。
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