CN114634816B - 一种双钙钛矿荧光材料及其制备方法与应用 - Google Patents
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Abstract
本发明公开了一种双钙钛矿荧光材料及其制备方法与应用，属于稀土发光材料技术领域。本发明双钙钛矿荧光材料，化学式为Ba2LuNbO6:x Bi3+,0＜x≤1，双钙钛矿结构，双钙钛矿荧光材料在X射线激发下发射蓝绿色光。本发明通过铋离子的掺杂，选择性占据不同的阳离子格位，实现在高能紫外(尤其是在200‑400nm波段)激发下没有发光，X射线(管电压40KV，管电流30mA)激发下有明亮的蓝绿色发光发射；载流子的俘获过程经用X射线而非紫外光激发实现，在X射线延时探测中排除了紫外光的干扰进而实现高的空间分辨率；经高能X射线连续循环辐射后，仍可保持较高的X射线发光亮度；本发明双钙钛矿材料实现了高空间分辨的X射线间接及延时探测领域应用。
Description
技术领域
本发明涉及一种双钙钛矿荧光材料及其制备方法于应用，属于稀土发光材料技术领域。
背景技术
X射线辐射的检测在可穿戴个人剂量学、工业辐射检测和环境监测等领域越来越重要，尤其是由于大量放射性废水进入海洋危及海洋生物的生存和人类健康。
无论是直接的还是间接的X射线探测中，由于高能紫外(尤其是在200-400nm波段)的干扰，限制了其在工业和环境检测领域的准确检测。因此，迫切需要进一步设计和开发无高能紫外干扰的性能优异材料和器件结构，以满足高信噪比下的X射线探测需求。
发明内容
针对现有技术中由于高能紫外(尤其是在200-400nm波段)的干扰，限制X射线在工业和环境检测领域的准确检测的问题，本发明提供一种双钙钛矿荧光材料及其制备方法与应用，本发明通过铋离子的掺杂，选择性占据不同的阳离子格位，实现在高能紫外(尤其是在200-400nm波段)激发下没有发光，X射线(管电压40KV，管电流30mA)激发下有明亮的蓝绿色发光发射；实现高空间分辨率的X射线间接和延时探测。
一种双钙钛矿荧光材料，化学式为Ba2LuNbO6:x Bi3+,0＜x≤1，双钙钛矿结构，双钙钛矿荧光材料在X射线激发下发射蓝绿色光。
所述双钙钛矿荧光材料的制备方法，具体步骤如下：
(1)将高纯BaCO3、Lu2O3、Nb2O5和Bi2O3混合得到混合物A，混合物A研磨均匀得到混合物粉料；
(2)将步骤(1)的混合粉料置于温度为1200～1600℃、空气氛围中焙烧4～8h，冷却至室温，研磨即得双钙钛矿荧光材料。
所述步骤(1)研磨时加入乙醇，乙醇的加入量为混合物A体积的80～120％。
所述双钙钛矿荧光材料在X射线探测中的应用：高能紫外激发下不发光，X射线激发下发射蓝绿色光。
本发明的有益效果：
(1)本发明通过铋离子的掺杂，选择性占据不同的阳离子格位，实现在高能紫外(尤其是在200-400nm波段)激发下不发光，X射线(管电压40KV，管电流30mA)激发下发射明亮的蓝绿色光；
(2)本发明载流子的俘获过程经用X射线而非紫外光激发实现，在X射线延时探测中排除了紫外光的干扰进而实现高的空间分辨率；经高能X射线连续循环辐射后，仍可保持较高的X射线发光亮度；
(3)本发明实现了高空间分辨率的X射线间接及延时探测，可应用在可穿戴个人剂量学、工业辐射检测和环境监测等领域。
附图说明
图1为实施例1-3所得Bi3+掺杂的Ba2LuNbO6双钙钛矿材料的XRD图谱；
图2为实施例1-3所得Ba2LuNbO6的X射线发光光谱；
图3为实施例1所得Ba2LuNbO6的X射线、紫外分别辐照后PSL光谱。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
实施例1：本实施例的双钙钛矿荧光材料，化学式为Ba2LuNbO6:0.005Bi3+；
所述双钙钛矿荧光材料的制备方法，具体步骤如下：
(1)高纯原料BaCO3(99.99％)、Lu2O3(99.99％)、Nb2O5(99.99％)、Bi2O3(99.99％)按照摩尔比为4:1:1:0.005的比例混合；然后加入纯度为99.99wt％的乙醇，采用玛瑙研钵充分研磨20min使其混合均匀得到混合粉料；
(2)将步骤(1)的混合粉料置于温度为1200℃、空气氛围中煅烧4h，冷却至室温，研磨即得Ba2LuNbO6:0.005Bi3+双钙钛矿荧光材料；
本实施例Ba2LuNbO6:0.005Bi3+双钙钛矿荧光材料通过铋离子的掺杂，选择性占据不同的阳离子格位，实现在高能紫外(尤其是在200-400nm波段)激发下不发光，X射线(管电压40KV，管电流30mA)激发下发射明亮的蓝绿色光。
实施例2：本实施例的双钙钛矿荧光材料，化学式为Ba2LuNbO6:0.03Bi3+；
所述双钙钛矿荧光材料的制备方法，具体步骤如下：
(1)高纯原料BaCO3(99.99％)、Lu2O3(99.99％)、Nb2O5(99.99％)、Bi2O3(99.99％)按照摩尔比为4:1:1:0.03的比例混合；然后加入纯度为99.99wt％的乙醇，采用玛瑙研钵充分研磨25min使其混合均匀得到混合粉料；
(2)将步骤(1)的混合粉料置于温度为1400℃、空气氛围中煅烧6h，冷却至室温，研磨即得Ba2LuNbO6:0.03Bi3+双钙钛矿荧光材料；
本实施例Ba2LuNbO6:0.03Bi3+双钙钛矿荧光材料通过铋离子的掺杂，选择性占据不同的阳离子格位，实现在高能紫外(尤其是在200-400nm波段)激发下不发光，X射线(管电压40KV，管电流30mA)激发下发射明亮的蓝绿色光。
实施例3：本实施例的双钙钛矿荧光材料，化学式为Ba2LuNbO6:0.10Bi3+；
所述双钙钛矿荧光材料的制备方法，具体步骤如下：
(1)高纯原料BaCO3(99.99％)、Lu2O3(99.99％)、Nb2O5(99.99％)、Bi2O3(99.99％)按照摩尔比为4:1:1:0.10的比例混合；然后加入纯度为99.99wt％的乙醇，采用玛瑙研钵充分研磨22min使其混合均匀得到混合粉料；
(2)将步骤(1)的混合粉料置于温度为1500℃、空气氛围中煅烧8h，冷却至室温，研磨即得Ba2LuNbO6:0.10Bi3+双钙钛矿荧光材料；
实施例1-3制备的X射线探测的双钙钛矿荧光材料Ba2LuNbO6:x Bi3+的XRD图谱见图1，从图1可知，图中显示与PDF卡片24-1059对比没有杂峰，合成的材料均为单相；
实施例1-3制备的Ba2LuNbO6:x Bi3+的X射线激发的发光光谱见图2；从图2可知，合成的材料选择性占据阳离子格位，在X射线激发下发出强烈的蓝光，发光波长在425nm,485nm左右，尤其是实施例2制备得到的双钙钛矿材料蓝色发光最亮；
本实施例Ba2LuNbO6:0.10Bi3+的X射线、紫外分别辐照后用980nm激发的PSL发光光谱见图3，从图3可知，在紫外激发下，合成材料的发光颜色几乎不可见；在X射线激发下，发出明亮的蓝色，这实现了不受紫外干扰的高空间分辨率的X射线探测。
以上结合附图对本发明的具体实施方式作了详细说明，但本发明并不局限于上述实施方式，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下做出各种变化。
Claims (3)
1.双钙钛矿荧光材料在X射线探测中的应用，其特征在于：所述双钙钛矿荧光材料在高能紫外激发下不发光，X射线激发下发射蓝绿色光；
所述双钙钛矿荧光材料，化学式为Ba2LuNbO6: x Bi3+, 0.005≤x≤0.10，双钙钛矿结构。
2.根据权利要求1所述双钙钛矿荧光材料在X射线探测中的应用，其特征在于：所述双钙钛矿荧光材料的制备方法，具体步骤如下：
（1）将高纯BaCO3、Lu2O3、Nb2O5和Bi2O3混合得到混合物A，混合物A研磨均匀得到混合物粉料；
（2）将步骤（1）的混合粉料置于温度为1200~1600℃、空气氛围中焙烧4~8h，冷却至室温，研磨即得双钙钛矿荧光材料。
3.根据权利要求2所述双钙钛矿荧光材料在X射线探测中的应用，其特征在于：步骤（1）研磨时加入乙醇，乙醇的加入量为混合物A体积的80~120%。
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| CN112852422A (zh) * | 2021-02-05 | 2021-05-28 | 成都理工大学 | 一种白色led荧光材料及其制备方法 |
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| WO2022033501A1 (zh) * | 2020-08-11 | 2022-02-17 | 吉林大学 | 一种钙钛矿晶体、其制备方法及x射线探测器 |
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