CN114057220A - 一种钙钛矿纳米晶的制备方法 - Google Patents
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Abstract
本发明公开了一种室温下微量水辅助的无溶剂机械化学合成化学式为Cs(PbyA1‑y)X3(其中,A=Zn、Sr,X=Cl、Br、I,0.8≤y≤1.0)的全无机钙钛矿纳米晶的方法,首先将所需原料球磨5‑180分钟,再加入原料总量0.05‑5%的微量水后继续球磨即可获得高发光性能的无机钙钛矿。本发明所述合成方法不需高温加热、惰性气体保护、有机溶剂、额外有机配体,只需简单混合原料并进行机械化学反应,直接得到粉体,产品稳定性高,易于规模化生产,生产成本低。
Description
技术领域
本发明属于光电材料领域,涉及一种室温下机械化学合成全无机钙钛矿纳米晶的方法。
背景技术
全无机CsPbX3钙钛矿量子点是一种新兴的发光材料,与传统的镉系量子点相比,由于CsPbX3钙钛矿光谱狭窄(15~25nm)、高缺陷容忍度的特性和明亮的发射,其在显示和照明领域具有巨大的应用前景。目前,CsPbX3钙钛矿量子点的光致发光量子产率已经达到90%以上,以CsPbX3钙钛矿为发光层的绿色LED器件的效率已经提升到20%以上,CsPbX3钙钛矿在太阳能电池、显示器、激光器等光电器件上具有广阔的应用前景。
2015年,L. Protesescu研究团队率先报道了通过高温热注入法制备钙钛矿量子点(Nano Lett., 2015, 15, 3692)。随后,李晓明等人采用饱和结晶法快速制备了钙钛矿量子点(Adv.Funct.Mater., 2016, 26, 2435)。不得不指出的是,上述方法均为液相合成方法,需要使用大量对环境不友好的有机溶剂,合成成本高。另一方面,由于钙钛矿材料本身的离子特性,其对极性溶剂,如乙醇等稳定性差,限制了其进一步发展。
为了避免溶剂、高温等复杂的制备条件,机械化学合成方法引起了研究者的关注。文献(Chem Commun., 2017, 53, 3046)通过添加四正辛基溴化铵配体,采用机械化学的方法制备了球形、片形的钙钛矿纳米晶体,其量子产率达到13%。文献报道了(J. Phys. Chem.Lett., 2017, 8, 1610)使用油酰胺为配体,溴化铅、溴化铯为前驱体通过球磨的方法也可以获得发光的钙钛矿纳米晶体。尽管这些方法避免使用有机溶剂、高温、惰性气体保护等复杂条件,整个制备过程中仅使用机械作用促使体相的钙钛矿大颗粒转化为纳米晶体使得材料表面缺陷增加,其发光效率降低,同时需要花费时间久。此外,制备的钙钛矿材料由于表面配体不稳定,极易脱落,使得钙钛矿材料与空气、极性溶剂接触引起发光淬灭。中国发明专利公开号CN112520784A报道提供了一种机械化学制备NH4PbIxCl3-x钙钛矿光电材料的方法,但其低光致发光限制了其在发光领域的应用。中国发明专利CN109354059A提出一种无机钙钛矿量子点的固相合成方法,遗憾的是,制备过程需要在500~800摄氏度的高温条件下进行,容易导致钙钛矿材料团聚,影响发光性能,同时高温条件及复杂的后处理过程不利于资源节约和环境保护。
发明内容
针对现有技术存在的问题,本发明提出一种微量水辅助的无溶剂机械化学合成化学式为Cs(PbyA1-y)X3(其中,A=Zn、Sr,X=Cl、Br、I,0.8≤y≤1.0)的全无机钙钛矿纳米晶的方法。本方法仅使用长链有机酸根作为唯一配体,在室温、无惰性气体保护的条件下合成了高稳定性的CsPbX3钙钛矿。
该制备方法包括下述步骤:
(1)将化学式为RCOOCs的有机酸铯、PbX2、ZnX2、SrX2按钙钛矿纳米晶化学式中阳离子的化学计量比组成的混合原料球磨5~180分钟;
(2)加入微量水继续球磨1~240分钟;
(3)球磨结束后,过筛去除球磨珠后即可得到钙钛矿纳米晶粉体。
其特征在于所述化学式为RCOOCs的有机酸铯中R为含碳原子大于等于7、小于等于19的有机碳链,有机酸铯中的有机酸根在合成反应过程中作为配体与钙钛矿中的Cs和Pb离子结合,控制合成的纳米晶的尺寸及作为纳米晶的保护层,当有机酸配根中碳原子数小于8时易脱附造成纳米晶易团聚长大,稳定性变差,高于20时则不易发生反应形成钙钛矿纳米晶。
步骤1所述的球磨时间不少于5分钟,不超过180分钟,优选为10~30分钟,在本步骤中,原料之间反应形成所需的钙钛矿体相晶体,当研磨时间小于5分钟,混合物不均匀反应不充分,导致产物纯度低,影响产物发光性能;反应时间过长易导致生产效率降低。
步骤2所述添加的微量水的质量为步骤1中混合原料的0.05~5%,加入微量水可以促进步骤1生成的钙钛矿晶体由体相转变为纳米晶体,水用量低于0.05%,则需要较长时间使之转变为纳米晶,用量高于5%则导致钙钛矿材料水解从而造成发光效率急剧下降,优选为0.1~1%。
步骤2所述的球磨所需时间为1~240分钟,与微量水的加入量负相关,即水的加入量少,球磨所用时间长,水的加入量多,球磨所用时间短,时间低于1分钟,存在大量的体相晶体,时间高于240分钟,则生产效率降低。
对照现有技术,本发明的优势在于:(1)本发明所述合成方法不需高温加热,只要简单混合原料并机械化学,不需要惰性气体保护以及避免了大量使用有机溶剂,合成所需条件及实验操作人员的专业技术要求大大降低,易于规模化生产,也而有利于降低生产成本;(2)在制备过程中添加微量的水,在与机械化学作用力的共同作用下加速了体相材料向纳米晶体的转换过程;(3)不额外添加有机酸和有机胺类配体,而是直接采用铯盐中的有机酸根作为单一配体,在极性溶剂(如乙醇)中具有非常高的稳定性;(4)直接得到粉体材料,易于应用。
附图说明
附图1:实施例1所制备的钙钛矿纳米晶的发射光谱。
附图2:实施例1所制备的钙钛矿纳米晶的透射电子显微镜照片。
附图3:实施例1所制备的钙钛矿纳米晶的X射线晶体衍射图谱。
附图4:实施例1所制备的钙钛矿纳米晶在乙醇溶液中存放时发光强度与保存天数关系曲线。
附图5:对照例的扫描电子显微镜照片。
具体实施方案
实施例1
将82.8 g 油酸铯与73.4 g 溴化铅混合,加入52.1 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨180分钟获得体相CsPbBr3钙钛矿,然后,加入3 g水继续球磨30分钟,过筛去除球磨珠,即可得到化学式为CsPbBr3的钙钛矿纳米晶粉体。
实施例2
将82.8 g 油酸铯、58.7 g 溴化铅与9 g 溴化锌混合,加入50.2 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨20分钟获得体相CsPb0.8Zn0.2Br3钙钛矿,然后,加入0.3 g水继续球磨120分钟,过筛去除球磨珠,即可得到化学式为CsPb0.8Zn0.2Br3的钙钛矿纳米晶粉体。
实施例3
将82.8 g 油酸铯、58.7 g 溴化铅与9.9 g 溴化锶混合,加入50.5 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨20分钟获得体相CsPb0.8Sr0.2Br3钙钛矿,然后,加入0.3g水继续球磨120分钟,过筛去除球磨珠,即可得到化学式为CsPb0.8Sr0.2Br3的钙钛矿纳米晶粉体。
实施例4
将66.6 g 月桂酸铯与73.4 g 溴化铅混合,加入52.1 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨5分钟获得体相CsPbBr3钙钛矿,然后,加入0.07 g水继续球磨240分钟,过筛去除球磨珠,即可得到化学式为CsPbBr3的钙钛矿纳米晶粉体。
实施例5
将18.5 g辛酸铯、14.2 g溴化铯与17.3 g碘化铯混合后,再加入73.4 g 溴化铅混合,之后加入41.1 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨5分钟获得体相CsPbBr2I钙钛矿,然后,加入1 g水继续球磨60分钟,过筛去除球磨珠,即可得到化学式为CsPbBr2I的钙钛矿纳米晶粉体。
实施例6
将22.2 g二十烷酸铯与、14.2 g溴化铯和11.2 g氯化铯混合,加入73.4 g 溴化铅混合,之后加入42.8 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨5分钟获得体相CsPbBr2Cl钙钛矿,然后,加入6.05 g水继续球磨1分钟,过筛去除球磨珠,即可得到化学式为CsPbBr2Cl的钙钛矿纳米晶粉体。
对照例
将82.8 g 油酸铯与73.4 g 溴化铅混合,加入52.1 g(混合料的1/3)直径0.5mm的氧化锆球磨珠,球磨180分钟获得体相CsPbBr3钙钛矿。与实施例1不同,该过程不加入微量水,所得产物为体相CsPbBr3钙钛矿具有极弱的荧光强度。
Claims (3)
1.一种钙钛矿纳米晶粉体的制备方法,其特征是化学式为Cs(PbyA1-y)X3(其中,A=Zn、Sr,X=Cl、Br、I,0.8≤y≤1.0)的钙钛矿纳米晶使用微量水辅助的无溶剂的机械化学合成法制备,其具体制备方法是:将化学式为RCOOCs的有机酸铯、PbX2、ZnX2、SrX2按钙钛矿纳米晶化学式中阳离子的化学计量比组成的混合原料球磨5~180分钟后,加入微量水继续球磨1~240分钟,取出后过筛去除球磨珠后即可得到钙钛矿纳米晶粉体。
2.根据权利要求1所述的钙钛矿纳米晶粉体的制备方法,其特征在于所述化学式为RCOOCs的有机酸铯中R为含碳原子大于等于7、小于等于19的有机碳链。
3.根据权利要求1所述的钙钛矿纳米晶粉体的制备方法,其特征在于微量水的质量为混合原料总质量的0.05~5%。
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US6017504A (en) * | 1998-07-16 | 2000-01-25 | Universite Laval | Process for synthesizing perovskites using high energy milling |
CN110194954A (zh) * | 2018-02-27 | 2019-09-03 | 中国科学院福建物质结构研究所 | 一种abx3型全无机钙钛矿纳米晶的制备方法 |
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