CN112852413A - 含锰钙钛矿可调谐发光材料及其制备方法和应用 - Google Patents
含锰钙钛矿可调谐发光材料及其制备方法和应用 Download PDFInfo
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- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 5
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- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
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Abstract
本发明公开了含锰钙钛矿可调谐发光材料及其制备方法和应用,所述材料的基体为含锰钙钛矿材料,通过不同制备方法获得,即可通过改变钙钛矿ABX3上的有机胺分子的大小和种类、数量、材料主体组分,或者改变处理温度、甚至是吸附水来调控其组成、微结构或电子态,实现发光行为调控,实现调谐其发光波长和发光效率。本发明制得的含锰钙钛矿可调谐发光材料结晶性好,结构稳定,制备过程简便,可快速大量合成,发光效率高;这类材料发光颜色可调,其制成的LED可实现510nm的宽带绿光、550nm的宽带黄绿色、600nm橙黄色、640nm红色以及超宽带白色调谐发射,在照明、显示、投影、LED及荧光探针等诸多领域具有很好的应用前景。
Description
技术领域
本发明属于卤素钙钛矿衍生物及其光电技术领域,具体涉及到几种含锰钙钛矿可调谐高效发光材料的制备方法及器件应用。
背景技术
长期以来发光材料多采用稀土离子掺杂材料,处理成本高,价格昂贵,且激发条件苛刻。而有机材料稳定性差,光谱线宽大,应用受限。近年来,得益于高光致发光量子产率、低成本、结构灵活、载流子迁移率高等显著优势,卤素基钙钛矿材料由于其特殊的发光特性,如高亮度、颜色可调性和强吸收系数,在下一代固态照明、显示生物成像等领域中有着巨大潜在应用前景。然而,发光颜色单一,不能在宽的或者绝大部分可见区域内调谐,有的材料生产过程复杂,也是该类材料在大规模应用中需要解决的重要问题。因此,寻找生产过程简单,在可见区域可调谐的材料是亟待解决的。另外有些钙钛矿材料含有毒性元素,影响人类健康,也是需要避免的。还有,锰是重要的地球富有元素,是多种功能材料的必备元素,如能源、催化、发光等。如能用锰做高效可调谐发光材料,替代稀土,将极大地降低成本,并提高稳定性和应用范围,有利于实现可持续发展。
同时白光LED作为第四代照明材料具有节能环保、使用寿命长、高效等特点,在照明等领域获得了广泛应用,目前获得白光LED的方式主要是在GaN蓝色芯片上涂覆黄色荧光粉。这种白光LED器件受所加的驱动电压和所涂荧光粉的厚度影响很大。并且目前商用的白光LED色彩还原性差、显色指数低,照明效率受芯片影响很大。因此,寻找一种单组分高效白光LED材料十分有必要。
本发明中所提供的几种含锰钙钛矿可调谐发光材料的制备方法及发光应用,其发光可在绝大部分的可见区域内调谐,具备单组分白色发射功能,发光效率高,制备方法简单易行,可能替代稀土发光材料,具有极大的市场应用潜力。
发明内容
针对现有技术的以上缺陷或改进需求,本发明通过不同物理机制调谐含锰钙钛矿发光,简单一步合成具有稳定高效的可调谐发光含锰钙钛矿材料,合成的含锰钙钛矿可调谐发光材料的发光可覆盖绝大部分可见区域,其中还有单组分白光材料。
本发明解决其技术问题所采用的技术方案如下:
本发明的含锰钙钛矿可调谐发光材料的基本为含锰钙钛矿材料,通过不同制备方法获得,所述含锰钙钛矿可调谐发光材料为吡啶溴化锰钙钛矿材料、哌嗪溴化锰钙钛矿材料、吡咯烷溴化锰钙钛矿材料、双吡咯烷溴化锰钙钛矿材料、Mn2+掺杂ACdCl3钙钛矿材料、Mn2+掺杂APbCl3钙钛矿材料、Mn2+掺杂哌嗪铅溴钙钛矿材料或有机胺铅锰氯溴化物钙钛矿材料,这类材料通过不同物理机制可调谐发光。
其中吡啶溴化锰钙钛矿材料可做绿色发光材料,哌嗪溴化锰钙钛矿材料可做黄绿色发光材料,吡咯烷溴化锰钙钛矿材料可做绿色发光材料,双吡咯烷溴化锰钙钛矿材料可做红色发光材料,Mn2+掺杂ACdCl3钙钛矿材料可做橙黄色发光材料,Mn2+掺杂APbCl3钙钛矿材料和Mn2+掺杂哌嗪铅溴钙钛矿材料可做红色发光材料,有机胺铅锰氯溴化物钙钛矿材料可做白色发光材料。
所述吡啶溴化锰钙钛矿材料和哌嗪溴化锰钙钛矿材料均是通过改变钙钛矿(ABX3)上的A位有机胺分子的大小和种类,调谐其发光。包括以下步骤制备得到:(1)将氨基吡啶和溴化锰按摩尔比为2:1加入,再向氨基吡啶和溴化锰中加入氢溴酸使其完全溶解;(2)蒸发结晶:以50-80℃蒸发72-96h;(3)收集晶体产物,洗涤干燥,得到所述吡啶溴化锰钙钛矿材料。将步骤(1)中的氨基吡啶改为哌嗪,重复步骤(1)、(2)、(3)得到所述哌嗪溴化锰钙钛矿材料。
所述吡咯烷溴化锰钙钛矿材料和双吡咯烷溴化锰钙钛矿材料均是通过改变钙钛矿(ABX3)上的A位有机胺分子的数量,调谐其发光。包括以下步骤制备得到:(1)将氢溴酸吡咯烷和溴化锰按摩尔比为1:1加入,再向氢溴酸吡咯烷和溴化锰中加入氢溴酸其完全溶解;(2)蒸发结晶:以50-80℃蒸发72-96h;(3)收集晶体产物,洗涤干燥,得到吡咯烷溴化锰钙钛矿材料。将步骤(1)中的摩尔比例改为2:1,重复步骤(1)、(2)、(3)得到所述双吡咯烷溴化锰钙钛矿材料。
所述Mn2+掺杂ACdCl3钙钛矿材料和Mn2+掺杂APbCl3钙钛矿材料均是通过改变钙钛矿(ABX3)上的B位元素主体,调谐其发光。包括以下步骤制备得到:(1)将金属氯化物或者有机胺、氯化镉和氯化锰按摩尔比为1:0.85:0.15加入反应釜聚四氟乙烯内衬中,再加入浓盐酸;(2)放入烘箱中以30-240℃的温度反应4-100h;(3)自然冷却至室温,收集固体产物,洗涤干燥,得到Mn2+掺杂ACdCl3钙钛矿材料。将步骤(1)中的氯化镉改为氯化铅,摩尔比例改为1:0.7:0.3,重复步骤(1)、(2)、(3)得到所述Mn2+掺杂APbCl3钙钛矿材料。
所述Mn2+掺杂哌嗪铅溴钙钛矿材料是通过调节处理温度,调谐其发光,即室温下发红光,80K下发绿光,120K下发黄光。所述Mn2+掺杂哌嗪铅溴钙钛矿材料通过以下步骤的方法制备得到:(1)将哌嗪、溴化铅和溴化锰按摩尔比为1:1:14一起加入反应釜聚四氟乙烯内衬中,再加入氢溴酸;(2)放入烘箱中以30-240℃的温度反应4-100h;(3)自然冷却至室温,收集固体产物,洗涤干燥,得到Mn2+掺杂哌嗪铅溴钙钛矿材料。
所述有机胺铅锰氯溴化物钙钛矿材料是通过调节吸附水,调谐其发光,吸附水产物发白光,热处理产物发红光。所述有机胺铅锰氯溴化物钙钛矿材料通过以下步骤的方法制备得到:(1)将短链有机胺、溴化铅和溴化锰按摩尔比为2:0.5:1一起加入玛瑙研钵中研磨30min;(2)放入烘箱中以65℃的温度反应12h;(3)自然冷却至室温,得到有机胺铅锰氯溴化物钙钛矿材料。
本发明的再一个技术方案是,所述的含锰钙钛矿可调谐发光材料可应用作绿光、黄绿光、橙黄光、红光、白光器件及可调谐发光器件的材料;所述绿光、黄绿光、橙黄光、红光、白光器件及可调谐发光器件可应用于照明、背光源、显示器件或太阳能电池器件中。
与现有技术相比,本发明具有以下有益效果:
(1)本发明的材料作为发光材料用于制备单组分白光LED发光二极管具有体积小、能耗低、响应快、寿命长、无污染等显著的优点。
(2)本发明制备的含锰钙钛矿可调谐发光材料的光致发光效率高;光吸收范围广,可在365nm或280nm紫外灯激发下即可获得明亮的发光。
(4)本发明可通过不同方法,实现500-640nm可见光调谐及白光发射。
(5)本发明提供的简单一步溶剂热方法和研磨方法,制备效率高,成本低,可用于大规模生产。
(6)本发明制备的粉体分散性较好。
(7)本发明制备的材料所采用的原材料容易获得,制备工艺简单,适合于工业化生产,在照明、背光源、显示器件和太阳能电池器件等领域有广泛的应用前景。
(8)本发明可通过改变钙钛矿ABX3上的有机胺分子的大小和种类、数量、材料主体组分,或者是处理温度、甚至是吸附水来调控其组成、微结构或电子态,实现发光行为调控,实现调谐其发光波长和发光效率。本发明制得含锰钙钛矿材料结晶性好,结构稳定,制备过程简便,可快速大量合成,发光效率高;这类材料发光颜色可调,其制成的LED可实现510nm的宽带绿光、550nm的宽带黄绿色、600nm橙黄色、640nm红色以及超宽带白色调谐发射,在照明、显示、投影、LED及荧光探针等诸多领域具有很好的应用前景。
附图说明
图1为实施例1-8所制备的几种含锰钙钛矿可调谐发光材料的光致发光光谱。本发明的材料可实现500-640nm可见光调谐及白光发射。
图2为实施例1所制备的吡啶溴化锰钙钛矿材料绿色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。吡啶溴化锰钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.28,0.69)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图3为实施例2所制备的哌嗪溴化锰钙钛矿材料黄绿色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。哌嗪溴化锰钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.39,0.58)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图4为实施例3所制备的吡咯烷溴化锰钙钛矿材料绿色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。吡咯烷溴化锰钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.29,0.69)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图5为实施例4所制备的双吡咯烷溴化锰钙钛矿材料红色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。双吡咯烷溴化锰钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.51,0.3)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图6为实施例5所制备的Mn2+掺杂ACdCl3钙钛矿橙黄色材料发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。Mn2+掺杂ACdCl3钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.58,0.41)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在280nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图7为实施例6所制备的Mn2+掺杂APbCl3钙钛矿红色材料发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。Mn2+掺杂APbCl3钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.59,0.31)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图8为实施例7所制备的Mn2+掺杂哌嗪铅溴钙钛矿材料红色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。Mn2+掺杂哌嗪铅溴钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.62,0.34)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图9为实施例8所制备的有机胺铅锰氯溴化物钙钛矿材料白色发光二极管的色坐标(CIE)图。插图为发光二极管工作照片。有机胺铅锰氯溴化物钙钛矿材料发光二极管的色坐标(CIE)图,坐标值(0.33,0.35)。这种二极管体积小、能耗低、响应快、寿命长、无污染;在365nm紫外灯激发下即可获得明亮的发光;发光均匀,粉体分散性较好。
图10为Mn2+掺杂哌嗪铅溴钙钛矿材料是通过调节处理温度,调谐其发光光谱图,即室温下发红光,80K下发绿光,120K下发黄光。
图11为有机胺铅锰氯溴化物钙钛矿材料是通过调节吸附水,调谐其发光光谱图,即吸附水为白色(65℃),烘干后为红色(100℃)。
具体实施方式
为使本发明更易理解,下面结合附图和具体实施例对本发明内容作进一步的详细描述,下面列举的具体实施例不用于限定本发明的权利范围。
实施例1
(1)将氨基吡啶和溴化锰按摩尔比为2:1一起加入烧杯中,再加入氢溴酸至完全溶解;
(2)蒸发结晶:将步骤(1)的烧杯放置于加热台上,以50-80℃蒸发72-96h;
(3)收集:反应完成后,收集晶体产物,洗涤干燥,得到吡啶溴化锰钙钛矿材料。
(4)将0.2g步骤(3)制备得到的吡啶溴化锰钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到吡啶溴化锰钙钛矿材料绿色发光二极管。
实施例2
(1)将哌嗪和溴化锰按摩尔比为1:1一起加入烧杯中,再加入氢溴酸至完全溶解;
(2)蒸发结晶:将步骤(1)的烧杯放置于加热台上,以50-80℃蒸发72-96h;;
(3)收集:反应完成后,收集晶体产物,洗涤干燥,得到哌嗪溴化锰钙钛矿材料。
(4)将0.2g步骤(3)制备得到的哌嗪溴化锰钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到哌嗪溴化锰钙钛矿材料黄绿色发光二极管。
实施例3
(1)将氢溴酸吡咯烷和溴化锰按摩尔比为1:1一起加入烧杯中,再加入氢溴酸至完全溶解;
(2)蒸发结晶:将步骤(1)的烧杯放置于加热台上,以50-80℃蒸发72-96h;
(3)收集:反应完成后,收集晶体产物,洗涤干燥,得到吡咯烷溴化锰钙钛矿材料。
(4)将0.2g步骤(3)制备得到的哌嗪溴化锰钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到吡咯烷溴化锰钙钛矿材料绿色发光二极管。
实施例4
(1)将氢溴酸吡咯烷和溴化锰按摩尔比为2:1一起加入烧杯中,再加入氢溴酸至完全溶解;
(2)蒸发结晶:将步骤(1)的烧杯放置于加热台上,以50-80℃蒸发72-96h;
(3)收集:反应完成后,收集晶体产物,洗涤干燥,得到双吡咯烷溴化锰钙钛矿材料。
(4)将0.2g步骤(3)制备得到的哌嗪溴化锰钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到双吡咯烷溴化锰钙钛矿材料红色发光二极管。
实施例5
(1)将金属氯化物(或有机胺)、氯化镉和氯化锰按摩尔比为1:0.85:0.15一起加入反应釜聚四氟乙烯内衬中,再加入浓盐酸,其中每1mmol氯化镉对应加入10mL的浓盐酸;
(2)加热:将步骤(1)的反应釜密封后,放入烘箱中以30-240℃的温度反应4-100h;
(3)收集:反应完成后,自然冷却至室温,收集固体产物离心,用乙醇洗涤,干燥,得到Mn2+掺杂ACdCl3钙钛矿材料。
(4)将0.2g步骤(3)制备得到的Mn2+掺杂ACdCl3钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的280nm紫外光LED芯片上,在常温25℃下使其自然固化,得到Mn2+掺杂ACdCl3钙钛矿材料橙黄色发光二极管。
实施例6
(1)将金属氯化物(或者有机胺)、氯化铅和氯化锰按摩尔比为1:0.85:0.15一起加入反应釜聚四氟乙烯内衬中,再加入浓盐酸,其中每1mmol氯化铅对应加入10mL的浓盐酸;
(2)加热:将步骤(1)的反应釜密封后,放入烘箱中以30-240℃的温度反应4-100h;
(3)收集:反应完成后,自然冷却至室温,收集固体产物离心,用乙醇洗涤,干燥,得到Mn2+掺杂APbCl3钙钛矿材料。
(4)将0.2g步骤(3)制备得到的Mn2+掺杂APbCl3钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到Mn2+掺杂APbCl3钙钛矿材料红色发光二极管。
实施例7
(1)将哌嗪、溴化铅和溴化锰按摩尔比为1:1:14一起加入反应釜聚四氟乙烯内衬中,再加入氢溴酸,其中每1mmol溴化铅对应加入10mL的浓盐酸;
(2)加热:将步骤(1)的反应釜密封后,放入烘箱中以30-240℃的温度反应4-100h;
(3)收集:反应完成后,自然冷却至室温,收集固体产物离心,用乙醇洗涤,干燥,得到Mn2+掺杂哌嗪铅溴钙钛矿材料。
(4)将0.2g步骤(3)制备得到的Mn2+掺杂哌嗪铅溴钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到Mn2+掺杂哌嗪铅溴钙钛矿材料红色发光二极管。
实施例8
(1)将短链有机胺、溴化铅和溴化锰按摩尔比为2:0.5:1一起加入玛瑙研钵中研磨30min;
(2)放入烘箱中以65℃的温度反应12h;
(3)自然冷却至室温,得到有机胺铅锰氯溴化物钙钛矿材料。
(4)将0.2g步骤(3)制备的有机胺铅锰氯溴化物钙钛矿材料和硅树脂A/B胶(其中A胶1mL,B胶4mL)均匀混合,将混合物涂敷在己固定且已连接好电极的365nm紫外光LED芯片上,在常温25℃下使其自然固化,得到有机胺铅锰氯溴化物钙钛矿材料白色发光二极管。
Claims (12)
1.含锰钙钛矿可调谐发光材料,其特征在于,所述材料的基本为含锰钙钛矿材料,通过不同制备方法获得吡啶溴化锰钙钛矿材料、哌嗪溴化锰钙钛矿材料、吡咯烷溴化锰钙钛矿材料、双吡咯烷溴化锰钙钛矿材料、Mn2+掺杂ACdCl3钙钛矿材料、Mn2+掺杂APbCl3钙钛矿材料、Mn2+掺杂哌嗪铅溴钙钛矿材料或有机胺铅锰氯溴化物钙钛矿材料,这类材料通过不同物理机制可调谐其发光。
2.根据权利要求1所述的含锰钙钛矿可调谐发光材料,其特征在于,所述含锰钙钛矿可调谐发光材料可通过改变钙钛矿ABX3上的A位有机胺的分子大小和种类,调谐其发光。
3.根据权利要求2所述的含锰钙钛矿可调谐发光材料,其特征在于,所述吡啶溴化锰钙钛矿材料发绿光,通过以下步骤的方法制备得到:
S31.将氨基吡啶和溴化锰按摩尔比为2:1加入,再向氨基吡啶和溴化锰中加入氢溴酸使其完全溶解;
S32.蒸发结晶:以55-85℃蒸发72-96h;
S33.收集晶体产物,洗涤干燥,得到所述吡啶溴化锰钙钛矿材料;
所述哌嗪溴化锰钙钛矿材料发黄绿光,通过以下步骤的方法制备得到:
S3⑴.将哌嗪和溴化锰按摩尔比为2:1加入,再向哌嗪和溴化锰中加入氢溴酸使其完全溶解;
S3⑵.蒸发结晶:以55-85℃蒸发72-96h;
S3⑶.收集晶体产物,洗涤干燥,得到所述哌嗪溴化锰钙钛矿材料。
4.根据权利要求1所述的含锰钙钛矿可调谐发光材料,其特征在于,所述含锰钙钛矿可调谐发光材料可通过改变钙钛矿ABX3上的A位有机胺分子的数量,调谐其发光。
5.根据权利要求4所述的含锰钙钛矿可调谐发光材料,其特征在于,所述吡咯烷溴化锰钙钛矿材料发绿光,通过以下步骤的方法制备得到:
S51.将氢溴酸吡咯烷和溴化锰按摩尔比为1:1加入,再向氢溴酸吡咯烷和溴化锰中加入氢溴酸使其完全溶解;
S52.蒸发结晶:以55-85℃蒸发72-96h;
S53.收集晶体产物,洗涤干燥,得到吡咯烷溴化锰钙钛矿材料;
所述双吡咯烷溴化锰钙钛矿材料发红光,通过以下步骤的方法制备得到:
S5⑴.将氢溴酸吡咯烷和溴化锰按摩尔比值为2:1加入,再向氢溴酸吡咯烷和溴化锰中加入氢溴酸使其完全溶解;
S5⑵.蒸发结晶:以55-85℃蒸发72-96h;
S5⑶.收集晶体产物,洗涤干燥,得到双吡咯烷溴化锰钙钛矿材料。
6.根据权利要求1所述的含锰钙钛矿可调谐发光材料,其特征在于,所述含锰钙钛矿可调谐发光材料可通过改变钙钛矿ABX3上的B位元素主体,调谐其发光。
7.根据权利要求6所述的含锰钙钛矿可调谐发光材料,其特征在于,所述Mn2+掺杂ACdCl3钙钛矿材料发黄光,通过以下步骤的方法制备得到:
S71.将金属氯化物或有机胺、氯化镉和氯化锰按摩尔比为1:0.85:0.15加入反应釜聚四氟乙烯内衬中,再加入浓盐酸;
S72.放入烘箱中以30-240℃的温度反应4-100h;
S73.自然冷却至室温,收集固体产物,洗涤干燥,得到Mn2+掺杂ACdCl3钙钛矿材料;
所述Mn2+掺杂APbCl3钙钛矿材料发红光,通过以下步骤的方法制备得到:
S7⑴.将金属氯化物或者有机胺、氯化铅和氯化锰按摩尔比为1:0.7:0.3加入反应釜聚四氟乙烯内衬中,再加入浓盐酸;
S7⑵.放入烘箱中以30-240℃的温度反应4-100h;
S7⑶.自然冷却至室温,收集固体产物,洗涤干燥,得到Mn2+掺杂APbCl3钙钛矿材料。
8.根据权利要求1所述的含锰钙钛矿可调谐发光材料,其特征在于,所述含锰钙钛矿可调谐发光材料可通过调节处理温度,调谐其发光,即室温下发红光,80K下发绿光,120K下发黄光。
9.根据权利要求8所述的含锰钙钛矿可调谐发光材料,其特征在于,所述Mn2+掺杂哌嗪铅溴钙钛矿材料通过以下步骤的方法制备得到:
S91.将哌嗪、溴化铅和溴化锰按摩尔比为1:1:14一起加入反应釜聚四氟乙烯内衬中,再加入氢溴酸;
S92.放入烘箱中以30-240℃的温度反应4-100h;
S93.自然冷却至室温,收集固体产物,洗涤干燥,得到Mn2+掺杂哌嗪铅溴钙钛矿材料。
10.根据权利要求1所述的含锰钙钛矿可调谐发光材料,其特征在于,所述含锰钙钛矿可调谐发光材料可通过调节吸附水,调谐其发光,吸附水产物发白光,热处理产物发红光。
11.根据权利要求10所述的含锰钙钛矿可调谐发光材料,其特征在于,所述有机胺铅锰氯溴化物钙钛矿材料通过以下步骤的方法制备得到:
S111.将短链有机胺、溴化铅和溴化锰按摩尔比为2:0.5:1一起加入玛瑙研钵中研磨30min;
S112:放入烘箱中以65℃的温度反应12h;
S113.自然冷却至室温,得到有机胺铅锰氯溴化物钙钛矿材料。
12.权利要求1-11任一项所述的含锰钙钛矿可调谐发光材料可应用作绿光、黄绿光、橙黄光、红光、白光器件及可调谐发光器件的材料;所述绿光、黄绿光、橙黄光、红光、白光器件及可调谐发光器件可应用于照明、背光源、显示器件或太阳能电池器件中。
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