CN102559180B - 光致发光晶体材料钨酸铋铕及其制备方法 - Google Patents

光致发光晶体材料钨酸铋铕及其制备方法 Download PDF

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CN102559180B
CN102559180B CN201110351003.6A CN201110351003A CN102559180B CN 102559180 B CN102559180 B CN 102559180B CN 201110351003 A CN201110351003 A CN 201110351003A CN 102559180 B CN102559180 B CN 102559180B
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bismuth
europium
europium tungstate
tungstate
crystalline material
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CN102559180A (zh
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李夜雨
程文旦
张�浩
张炜龙
耿磊
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

本发明提供了一种光致发光晶体材料钨酸铋铕，该晶体分子式为：EuBiW2O9，属于正交晶系，空间群为Pnma，单胞参数为a=32.30?，b=5.65?，c=3.98?,α＝β＝γ＝90°，V=727.35?3,Z=4。采用高温固相方法合成钨酸铋铕单晶，将充分研磨均匀的混合原料置于铂坩埚中，放入箱式炉中加热合成，在最高温度恒温，然后缓慢冷却，降至室温后可得到钨酸铋铕单晶。该晶体材料用于白光LED用红色荧光粉及小型高功率固体激光器。

Description

光致发光晶体材料钨酸铋铕及其制备方法
技术领域
本发明涉及新型的光致发光材料，尤其是涉及一种新颖的红光发光晶体材料钨酸铋铕。
背景技术
钨酸盐材料因其独特的结构特征，在激光材料、闪烁材料、以及荧光材料方面具有重要的应用价值；稀土元素由于其特有的4f电子层结构，具有独特的光学性能。因此，目前国内外研究者正努力将稀土元素和钨酸盐材料结合起来，开发新型的稀土钨酸盐光学材料，以满足实际应用需要。对于稀土钨酸盐的研究，主要集中在通式为MLn(WO4)2 (M为碱金属元素, Ln为稀土元素)的化合物, 例如，KEu(WO4)2在固体拉曼激光器件方面具有潜在的应用价值。而对于稀土钨铋酸盐的光学性能的研究还是空白。我们在探索稀土钨酸盐光学材料过程中，将铋元素引入到钨酸铕中，从而得到了性能优越的新型光致发光晶体材料。
发明内容
本发明的目的在于设计一种不需要繁琐的制备途径和复杂的光学设计，其材料本体就可以在激发光下发射出一定特征波长的光，以满足实际应用需要，因此我们研制出了一种新的光致发光晶体材料—钨酸铋铕。
该晶体通过单晶X—射线衍射数据得知相关的晶体学参数为：该晶体分子式为：EuBiW2O9，属于正交晶系，空间群为Pnma，单胞参数为a = 32.30 Å，b = 5.65 Å，c = 3.98 Å, α＝β＝γ＝90°，V = 727.35 Å3, Z=4。 经结构解析表明：其结构为[BiO2]- 层 和 [Eu2W2O12]6- 层通过共角顶相连的WO6 八面体链相互连接形成网络结构，见附图1。
本发明采用如下技术方案，在Eu2O3-Bi2O3-WO3体系中采用高温固相反应合成，选用含该材料元素的氧化物作为反应原料。经低温预烧后，升高温度至1000 ℃，并恒温，然后缓慢冷却至室温得到该晶体。选用Eu2O3、Bi2O3和WO3为原料，按按0.5：1：2的摩尔比称取，将充分研磨均匀的混合原料置于铂坩埚中，放入箱式炉中加热合成，在1000 ℃下恒温煅烧，然后缓慢冷却，降至室温后可得到钨酸铋铕单晶。
我们对该晶体进行了紫外—可见吸收光谱的测定，最大吸收峰在281 nm附近，吸收截止波长为341 nm。从其荧光光谱得知，在波长为395 nm和467nm的光源激发下，该晶体材料在614 nm处均存在红光强发射峰。
这种稀土钨酸盐本体的结构在国内外均未见报道，它的优势在于在一定的激发波长下实现红光发射，制备工艺简单，生产成本低。本发明为人们制备用于白光LED用红色荧光粉及小型高功率固体激光器开拓新的发光材料来源。
附图说明
附图1为钨酸铋铕晶体的结构示意图。
具体实施方式
关于钨酸铋铕晶体的合成，采用高温固相合成方法在1000 ℃熔融，缓慢降温结晶而成。所用化学试剂的用量及化学计量比如下：
Eu2O3 0.1760g(0.5 mmol) Bi2O3 0.4660g(1 mmol) WO3 0.4637(2 Mmol)
具体操作方法如下：
按0.5：1：2的摩尔比例用分析天平准确称取，在通风橱中将称量好的试剂放入玛瑙研体中充分研磨使其混合均匀，然后将样品装入铂坩埚里。为使后期反应顺利进行，放入箱式炉中在300 ℃预烧、研磨。最后在1000 ℃下恒温30 h，经分阶段缓慢冷却到室温后（第一阶段：以2 ℃/h的速度降至700 ℃；第二阶段：以10 ℃/h的速度从700℃降至室温）。最终，在坩埚底部得到无色条状晶体。对该晶体进行单晶X—射线衍射晶体学分析知其为钨酸铋铕晶体，其晶体学参数如上所述，结构如附图所示。

Claims (4)

1.一种光致发光晶体材料钨酸铋铕，其特征在于：其化学式为EuBiW2O9，分子量为 872.64, 属正交晶系，空间群为Pnma，单胞参数为a = 32.30 Å，b = 5.65 Å，c = 3.98 Å, α＝β＝γ＝90°，V = 727.35 Å3, Z=4。
2.一种根据权利要求1所述的光致发光晶体材料钨酸铋铕的制备方法，其特征在于：采用高温固相合成方法生长。
3.一种根据权利要求1所述的光致发光晶体材料钨酸铋铕的制备方法，其特征在于：选用Eu2O3、Bi2O3和WO3为原料，按按0.5：1：2的摩尔比称取，将充分研磨均匀的混合原料置于铂坩埚中，放入箱式炉中加热合成，在1000 ℃下恒温煅烧，然后缓慢冷却，降至室温后可得到钨酸铋铕单晶。
4.一种根据权利要求1所述的光致发光晶体材料钨酸铋铕的用途，其特征在于：该晶体材料用于白光LED用红色荧光粉及小型高功率固体激光器。
CN201110351003.6A 2011-05-05 2011-11-08 光致发光晶体材料钨酸铋铕及其制备方法 Expired - Fee Related CN102559180B (zh)

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CN103881712B (zh) * 2014-02-28 2015-11-04 淮南师范学院 一种白光led用钨酸盐基质红色荧光粉及其制备方法
CN104891573B (zh) * 2015-05-28 2017-04-12 新疆大学 一种固相化学反应制备钨酸铋纳米片的方法
CN110373190A (zh) * 2019-07-06 2019-10-25 五邑大学 一种近紫外激发铋掺杂钨酸盐黄色荧光粉及其制备方法
CN113249790B (zh) * 2021-05-26 2023-02-03 曲阜师范大学 一种钕激活离子掺杂Na5Lu(MoO4)4晶体及其制备方法和应用
CN113717723B (zh) * 2021-10-08 2023-07-25 常州工程职业技术学院 一种Eu3+掺杂的铋酸盐红色荧光粉及其制备方法与应用

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