CN108258104A - 一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法 - Google Patents
一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法 Download PDFInfo
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Abstract
本发明公开了一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法,包括以下步骤:首先将碳酸铯和油酸溶解于1‑十八稀中,在氮气保护条件下得到铯油酸盐溶液,然后快速注入到完全溶解的、温度范围为140℃~200℃的掺锰的卤化铅盐溶液中,得到的产物即为Mn‑doped CsPbX3量子点,接着离心纯化,量子点可溶解在正己烷和甲苯中,最后,将制备好的Mn‑doped CsPbX3量子点结合油墨涂覆于玻璃表面形成厚度均匀的一层薄膜,该薄膜夹在两块玻璃中间,通过抽真空排气泡使该薄膜与外界环境密封隔绝,得到掺锰的卤化铅铯量子点荧光玻璃薄膜。本发明优点是荧光玻璃薄膜的稳定性和长久性佳。
Description
技术领域
本发明属于LED荧光技术领域,具体是指一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法。
背景技术
近几年,以碘化铅甲胺(MAPbI3)为代表的有机无机杂化钙钛矿材料凭借其优异的光电性能受到广泛关注。短短几年内钙钛矿太阳电池的光电转换效率已超过22.1%,呈现出良好的应用前景。但是,碘化铅甲胺等有机无机杂化钙钛矿材料对湿度、热、光照的不稳定性限制了其进一步应用。相比于有机无机杂化钙钛矿,全无机卤化铅铯钙钛矿(CsPbX3)具有更优越的稳定性,因此在钙钛矿太阳电池、发光器件、光电探测器等光电领域呈现出了非常诱人的应用前景。高发光效率和高可调性是全无机卤化铅铯量子点的最突出的性能。但是由于铅元素有毒,所以减少铅的含量或者完全取代铅元素是很有发展前景的。掺Mn的CsPbX3量子点中的Mn发光具有非常均匀的光谱特征,在 CsPbX3晶格中的电子顺磁共振谱表明Mn2+相对均匀的掺杂位点,说明 Mn可以替代Pb掺杂在CsPbX3。在600nm附近Mn2+表现出非常强烈的敏化Mn发光。
但是由于掺Mn的卤化铅铯量子点在空气中的稳定性较差,所以将该量子点制备成薄膜夹在玻璃中间,将其制作成封装器件,保证其稳定的环境,应用于LED器件、光电探测器、太阳能电池器件中。荧光玻璃薄膜是由两片或多片玻璃,之间夹了一层或多层中间膜,经过特殊的高温预压或抽真空及高温高压工艺处理后,是玻璃和中间膜永久性粘合为一体的复合玻璃产品。目前,用Mn-doped CsPbX3成分的钙钛矿制备的LED器件报道还没有,因此建立一种掺锰的卤化铅铯荧光玻璃薄膜静电制备方法是十分重要的。
发明内容
本发明的目的是为了克服现有技术存在的缺点和不足,而提供一种一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法,本发明方法简单有效,原料廉价易得,反应条件温和且环境友好,在一般实验室均能完成,易于推广。
(1)为实现上述目的,本发明的技术方案如下:首先将碳酸铯和油酸溶解于1-十八稀中,在氮气保护条件下得到铯油酸盐溶液;
(2)然后将MnCl2·(H2O)4和PbX2按比例溶解于十八稀中,最后将第一步制得的铯油酸盐快速的注入到完全溶解的、温度范围为140℃~200℃的掺锰的卤化铅盐溶液中,得到的产物即为Mn-doped CsPbX3量子点;
(3)接着离心纯化,量子点可溶解在正己烷中;
(4)将制备好的Mn-doped CsPbX3量子点均匀分布于油墨中,通过匀胶机使其最大化均匀,然后涂覆于玻璃表面形成厚度均匀的一层薄膜,该薄膜夹在两块玻璃中间,通过抽真空排气泡使该薄膜与外界环境密封隔绝,得到掺锰的卤化铅铯量子点荧光玻璃薄膜。
作为本发明之优选,所述Mn-doped CsPbX3量子点为Mn-doped CsPbCl3量子点、Mn-doped CsPb(Cl/Br)3量子点。
本发明采用传统的热注入法制备好量子点溶液,在365nm紫外灯照射下,合成出的掺锰的卤化铅铯量子点(Mn-doped CsPbCl3、 Mn-doped CsPb(Cl/Br)3)分别呈明亮的橙红色和蓝紫色,将量子点溶液与油墨混合,通过抽真空的方式制备出掺锰的卤化铅铯量子点荧光玻璃薄膜。
本发明所制备出的掺锰的卤化铅铯量子点荧光玻璃薄膜在LED 器件、光电探测器、太阳能电池器件中的应用。
本发明的优点与效果是:
(1)本发明通过简单的热注入法即可得到掺锰的卤化铅铯量子点,在365nm紫外灯照射下,合成出的掺锰的卤化铅铯量子点 (Mn-doped CsPbCl3、Mn-doped CsPb(Cl/Br)3)分别呈明亮的橙红色和蓝紫色的荧光。将发光性能好的量子点溶液制备成荧光玻璃薄膜,大大的提高了其稳定性和长久性;
(2)该量子点以及荧光玻璃薄膜的制备,适合产业化的要求;
(3)本方法所合成的掺锰的卤化铅铯量子点荧光玻璃既保持了量子点荧光高度高,发光可调等特性,又提高了其稳定性。在LED器件、光电探测器、太阳能电池器件等领域具有潜在的应用前景。
下面结合说明书附图和具体实施方式对本发明做进一步介绍。
附图说明
图1为本实施例制备的掺锰的CsPbCl3和CsPb(Cl/Br)3量子点以及荧光玻璃简单的制备步骤示意图。
图2为本实施例制备的掺锰和不掺锰的CsPbCl3和CsPb(Cl/Br)3量子点的荧光谱图。
图3为本实施例制备的掺锰的CsPbCl3and CsPb(Cl/Br)3量子点的XRD图。
图4为本实施例制备的掺锰的CsPbCl3and CsPb(Cl/Br)3量子点的HR-TEM以及量子点溶液分别在365nm激发下的图片。
图5为本实施例制备的量子点溶液制备成的荧光玻璃薄膜在 365nm的紫外灯照射下的图片。
具体实施方式
下面通过实施例对本发明进行具体的描述,只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限定,该领域的技术工程师可根据上述发明的内容对本发明作出一些非本质的改进和调整。
该方法首先利用碳酸铯、十八稀和油酸制备Cs油酸盐,然后将 MnCl2·(H2O)4和PbX2按比例溶解于十八稀中,最后将第一步制得的铯油酸盐快速的注入到完全溶解的、温度范围为140℃~200℃的掺锰的卤化铅盐溶液中,得到的产物即为Mn-doped CsPbX3量子点,冰水浴降温合成Mn-doped CsPbX3量子点,接着将该量子点结合油墨制成薄膜然后封装到两块玻璃中间,最后制成掺锰的卤化铅铯量子点荧光玻璃薄膜。
本发明的具体的制备步骤请参照图1。
本发明最后的步骤中掺锰和不掺锰的区别是较大的,具体可参考图2和图3,从该光谱图中可以看出,最后步骤中掺锰和不掺锰的区别非常明显。
我们利用365nm紫外灯照射,合成出的掺锰的卤化铅铯量子点 (Mn-dopedCsPbCl3、Mn-doped CsPb(Cl/Br)3)分别呈明亮的橙红色和蓝紫色的荧光,具体请见图4和图5。
实施例1
称量CsCO30.405g,OA 1.75ml和ODE 17ml于25ml的三口烧瓶中,在N2条件下制备出Cs油酸盐,然后将一定比例的PbCl2, MnCl2·(H2O)4和5ml ODE置于25ml三口烧瓶中,并在抽真空120℃下干燥1h,无水油酸和油胺在N2保护下注入,当形成完全熔化的掺锰的卤化铅盐时温度升至140℃~200℃,Cs的油酸盐溶液快速注入,1min 后冰水浴即可得亮橙红色的Mn-doped CsPbCl3量子点。最后将该量子点均匀分散于油墨中,然后封装在两块玻璃中间,制备成掺锰的氯化铅铯荧光玻璃薄膜。
实施例2
称量CsCO30.405g,OA 1.75ml和ODE 17ml于25ml的三口烧瓶中,在N2的条件下制备出Cs油酸盐,然后将一定比例的PbBr2, MnCl2·(H2O)4和5ml ODE置于25ml三口烧瓶中,并在抽真空120℃下干燥1h,无水油酸和油胺在N2保护下注入,当形成完全熔化的掺锰的卤化铅盐时温度升至140℃~200℃,Cs的油酸盐溶液快速注入,10s 后冰水浴即可得亮蓝紫色的Mn-doped CsPb(Cl/Br)3量子点。最后将该量子点均匀分散于油墨中,然后封装在两块玻璃中间,制备成掺锰的氯溴铅铯的铅铯荧光玻璃薄膜。
实施例3
将制得的Mn-doped CsPbCl3和Mn-doped CsPb(Cl/Br)3量子点溶液分别分散到油墨中,均匀搅拌,然后在两块玻璃中间进行灌注胶液,通过抽真空的设备实现玻璃和胶液紧紧粘在一起的荧光玻璃,彻底与外界大气压隔离,有效的防治了空气中的杂质对量子点不稳定的干扰,保证量子点在稳定的环境中发挥其独特的优势。最后制备出掺锰的卤化铅铯量子点荧光玻璃薄膜。
Claims (2)
1.一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法,其特征在于包括以下步骤:
(1)首先将碳酸铯和油酸溶解于1-十八稀中,在氮气保护条件下得到铯油酸盐溶液;
(2)然后将MnCl2·(H2O)4和PbX2按比例溶解于十八稀中,最后将第一步制得的铯油酸盐快速的注入到完全溶解的、温度范围为140℃~200℃的掺锰的卤化铅盐溶液中,得到的产物即为Mn-doped CsPbX3量子点;
(3)接着离心纯化,量子点可溶解在正己烷中;
(4)将制备好的Mn-doped CsPbX3量子点均匀分布于油墨中,通过匀胶机使其最大化均匀,然后涂覆于玻璃表面形成厚度均匀的一层薄膜,该薄膜夹在两块玻璃中间,通过抽真空排气泡使该薄膜与外界环境密封隔绝,得到掺锰的卤化铅铯量子点荧光玻璃薄膜。
2.根据权利要求1所述的一种掺锰的卤化铅铯荧光玻璃薄膜的静电制备方法,其特征在于,所述Mn-doped CsPbX3量子点为Mn-doped CsPbCl3量子点、Mn-doped CsPb(Cl/Br)3量子点。
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