CN107267147A - 一种绿光到红光发射的双钙钛矿反斯托克斯发光材料及其发光膜的制备 - Google Patents
一种绿光到红光发射的双钙钛矿反斯托克斯发光材料及其发光膜的制备 Download PDFInfo
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Abstract
本发明提供了一种以双钙钛矿钨酸盐为单一基质的上转换发光材料及发光膜的制备。所述的双钙钛矿钨酸盐为单一基质的上转换发光材料,它的化学式为Ca3‑x‑yWO6:xYb3+/yEr3+,xM1,其中,Ca3‑xWO6为基质,M1为碱金属离子Li+,Na+,K+中的一种或多种,x为Yb3+掺杂的摩尔百分数,0.01≤x≤0.5,y为Er3+掺杂的摩尔百分数,0.001≤y≤0.3。本发明通过高温固相法合成所述上转换发光材料,在980nm激光器的激发下,发射出从绿光到红光的上转换光。本发明通过简单的比例调整实现了单一基质发射出不同颜色的光,且材料制备工艺简单,无污染,适合工业化生产。在材料合成的基础上,利用电子束蒸发法实现了上转换转光膜的制备,上述转光膜具有荧光颜色可调,益于精准控制材料组分,操作简单,易于工业化推广的优点。
Description
技术领域
本发明属于稀土发光材料技术、材料化学领域,涉及到一种以双钙钛矿钨酸盐结构为单一基质的反斯托克斯发光材料及其发光膜的制备方法。
背景技术
早在20世纪60年代初就出现了反斯托克斯发光的报道。反斯托克斯发光又称上转换发光,是指发光材料在长波长光的激发照射下发射出短波长光的光转换现象。上转换发光通过将两个或者多个低能光子转换为一个高能光子,是提高光电器件对红外光子利用率的有效手段。上转换发光材料在光纤通讯技术、纤维放大器、三维立体显示、生物分子荧光标识等领域具有广泛的应用前景。但是,有红外长波辐射激发出绿光到红光发射的镱铒共掺钨酸钙上转换材料及其发光膜,仍未见报道。
发明内容
本发明的目的在于提供一种Yb3+,Er3+共掺Ca3WO6荧光粉晶相可控合成制备方法。该方法通过改变工艺参数,能够实现不同发光颜色的上转换荧光粉的可控合成,操作简便,有利于工业化生产。
本发明的另一个目的是提供该新型双钙钛矿钨酸盐上转换发光材料及发光膜的制备方法。
为达到以上目的,本发明采用的技术方案是提供一种以镱离子为感光剂,铒离子为激活剂的共掺双钙钛矿钨酸钙变色上转换发光材料。它的化学组成式为:Ca3-x-yWO6:xYb3 +/yEr3+,xM1,其中,Ca3-xWO6为基质,M1为碱金属离子Li+,Na+,K+中的一种或多种,x为Yb3+掺杂的摩尔百分数,0.01≤x≤0.5,y为Er3+掺杂的摩尔百分数,0.001≤y≤0.3。
本发明的技术方案:
(1)根据所述化学组成式Ca3-x-yWO6:xYb3+/yEr3+,xM1,,称取化学计量比的含有Ca的化合物、含有W的化合物、含有Yb的化合物、含有Er的化合物、含有碱金属Li、Na、K的化合物,并且研磨以均匀混合;
(2)将均匀混合的物料在空气中于450~850℃下预煅烧3~8小时;
(3)将预煅烧后的物料冷却至室温,并且研磨粉碎;
(4)将研磨后的物料在空气中于1000~1400℃下烧结4~10小时;
(5)将烧结后的物料冷却至室温,研磨粉碎并且过筛,即获得所述以双钙钛矿钨酸盐为单一基质的上转换发光材料。
本发明技术方案所述含有Ca的化合物为碳酸钙和氧化钙中的一种和多种;
所述含有W的化合物为氧化钨;
所述含有Yb的化合物为氧化镱;
所述含有Er的化合物为氧化铒;
所述含有碱金属Li、Na、K的化合物为碱金属Li、Na、K的碳酸盐。
所述预煅烧是在500~700℃的温度下进行4~6小时,所述煅烧是在1200~1300℃的温度下进行5~8小时。
与现有技术相比,本发明技术方案的优点在于:
1、本发明提供了一种以双钙钛矿钨酸盐为单一基质的上转换发光及其制备方法,工艺简单,原料易得,能耗小且无污染,利于工业化生产。
2、本发明提供的基质材料为钨酸盐,其具有良好的热稳定性和化学稳定性。
3、本发明制备的以双钙钛矿钨酸盐为单一基质的绿光到红光发射的上转换材料,能通过简单的配方调整实现不同颜色的上转换发光。
附图说明
图1为本发明实施例1所制得的Ca3-0.11xWO6:x Er3+10xYb3+材料样品的X射线粉末衍射图谱。
图2为本发明实施例1所制得的Ca3-0.11xWO6:x Er3+10xYb3+材料样品在980nm激发下的发射光图谱。
图3为本发明实施例1所制得的Ca3-0.11xWO6:x Er3+10xYb3+材料样品在980nm激发下得到的CIE坐标图。
图4为本发明实施例2所用的设备蒸发腔示意图,其中:蒸发舟置于蒸发源处,石英基片置于基片支架处。
图5为本发明实施例3所制得上转换发光结构的示意图,其中:1为WO6镀层,2为Yb2WO6镀层,3为Er2O3镀层,4为CaCO3镀层,5为石英基片。
具体实施方式
以下通过具体实施例进一步解释和说明本发明,但是以下具体实施例并不能用于限制本发明的保护范围。以下具体实施例的各种变化和改进都包括在权利要求书所限定的范围内。
实施例1:Ca3-0.11xWO6:x Er3+10xYb3+材料的制备
分别称取对应比例的碳酸钙(CaCO3)、氧化钨(WO3)、氧化镱(Yb2O3)、氧化铒(Er2O3),将上述原料混合物在玛瑙研钵中研磨混合均匀,然后装入刚玉坩埚中,在空气中于600℃温度下煅烧4.5小时,冷却至室温并研磨混合均匀;然后置于马弗炉中,在空气环境下于1250℃温度下煅烧4小时,冷却至室温后再次研磨均匀,过筛,最终得到上述绿光到红光发射的双钙钛矿钨酸盐上转换样品。
附图1,它是本实例1制备样品的X射线衍射图,结果显示,该样品XRD结构与标准卡片(JCPDS 22-0541)的衍射峰完全一致,没有出现杂峰,说明本实例所得的产物具有与Ca3WO6相同的双钙钛矿晶体结构。
附图2,它是本实例1制备样品在980nm激发下得到的发射光图谱;从图中可以看出,样品的主要发射峰在550nm和661nm;在低浓度镱铒掺杂时,样品的发射光谱红绿光强度相差不大,随着掺杂浓度的增加,红光发射的强度迅速增强而绿光强度保持在一个相对稳定的发射强度,从而样品的发射光呈现出从绿光到红光变化。通过简单配方变更实现了不同颜色的上转换发光。
附图3,它是实例1制备样品在980nm激发下得到的CIE坐标图,从图中可以看出,样品发射光的颜色从绿光向红光转变的趋势。
实施例2:热蒸发Ca3-0.11xWO6:x Er3+10xYb3+上转换发光膜的制备
将实施例1制备的上转换样品置于真空热蒸发镀膜机的蒸发舟内。将先后用丙酮、无水乙醇清洗后的石英基片固定在机械转盘托盘上,使基片距离蒸发源30cm。接通系统总电源后依次打开水循环机械泵电源,待真空腔内压强小于5Pa后启动涡轮分子泵,当分子泵达到27000转每分钟,腔内真空度达到3×10-4Pa~5×10-4Pa时开始蒸镀,最终得到50~150nm厚度的上转换发光膜。
附图4,它是实施例2所使用的设备蒸发腔示意图,其中:将蒸发舟置于蒸发源处,石英基片置于基片支架上。
实施例3:Ca3-0.11xWO6:x Er3+10xYb3+上转换发光膜的制备
将WO6、Yb2WO6、Er2O3、CaCO3分析纯粉末置于马弗炉中煅烧充分排气,然后放入多层镀膜机的各个独立的坩埚中。将先后用丙酮、无水乙醇清洗后的石英基片固定在机械转盘托盘上,使基片距离蒸发源30cm。先后打开机械泵、分子泵将真空室内真空抽至3.0×10- 4Pa。开启电子枪并调节输出电子流至110~140mA,依次蒸发各个原料靶,根据所需原料的比例来控制蒸发时间,将这四种材料依次被蒸发一次视为一个周期,最终得到50~150nm厚度的膜层。待基片取出后将其置于1250℃的马弗炉中煅烧4h,使蒸发式附着的碳分解,并使x Er3+,Yb3+离子进入到钨酸钙晶格中,从而获得不同颜色的上转换发光膜。
附图5,它是实施例3所制得上转换发光结构的示意图,其中:1为WO6镀层,2为Yb2WO6镀层,3为Er2O3镀层,4为CaCO3镀层,5为石英基片。
Claims (9)
1.一种绿光到红光发射的双钙钛矿结构的上转换发光材料,其特征在于,所述上转换材料的化学组成式为:Ca3-x-yWO6:xYb3+/yEr3+,xM1,其中,Ca3-xWO6为基质,M1为碱金属离子Li+,Na+,K+中的一种或多种,x为Yb3+掺杂的摩尔百分数,0.01≤x≤0.5,y为Er3+掺杂的摩尔百分数,0.001≤y≤0.3。
2.一种用于制备权利要求1所述的以双钙钛矿钨酸盐为单一基质的上转换发光材料其特征在于,所述材料在980nm激光激发下,发射绿光到红光的可见光。
3.一种用于制备权利要求1所述的以双钙钛矿钨酸盐为单一基质的上转换发光材料的方法,其特征在于,所述方法包括:
(1)根据所述化学组成式Ca3-x-yWO6:xYb3+/yEr3+,xM1,称取化学计量比的含有Ca的化合物、含有W的化合物、含有Yb、Er的化合物、含有碱金属Li、Na、K的化合物,并且研磨以均匀混合;
(2)将均匀混合的物料在空气中于450~850℃下预烧3~8小时;
(3)将预煅烧后的物料冷却至室温,并且研磨粉碎;
(4)将研磨后的物料在空气中于1000~1400℃下烧结4~10小时;
(5)将烧结后的物料冷却至室温,研磨粉碎并且过筛,即获得所述以双钙钛矿钨酸盐为单一基质的上转换发光材料。
4.一种利用权利1所述的双钙钛矿钨酸盐为单一基质的上转换转光膜的制备。
5.根据权利要求1所述的Yb/Er双掺杂上转换材料,其特征在于,所述的Yb/Er双掺杂上转换材料在980nm红外激光激发,其发射峰位于400nm-800nm范围内。
6.根据权利要求2所述的Yb/Er双掺杂上转换材料,其特征在于,所述的Yb/Er双掺杂上转换材料中,Yb,Er掺杂的量的比值为10∶1。
7.根据权利要求3所述的方法,其特征在于,所述含有Ca的化合物为碳酸钙和氧化钙中的一种和多种,所述含有W的化合物为氧化钨,所述含有Yb的化合物为氧化镱,所述含有Er的化合物为氧化铒,所述含有M1碱金属Li、Na、K的化合物为碱金属Li、Na、K的碳酸盐。
8.根据权利要求3所述的方法,其特征在于,所述预煅烧的温度为500~700℃,所述预煅烧的时间为4~6小时,并且所述烧结的温度为1200~1300℃,所述烧结的时间为5~8小时。
9.根据权利要求4所述的方法,其特征在于,所述上转换转光膜的厚度为50~150nm,所述上转换转光膜的基片为石英基片,所述基片煅烧条件为1100~1300℃。
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