CN112410030A - 一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法 - Google Patents
一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法 Download PDFInfo
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Abstract
一种多相复合钼酸盐氟氧化物纳米荧光材料K3HF2MoO2F4:Mn4+的制备方法,具体是取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置5~10min,过滤、洗涤,干燥。本发明制备的K3HF2MoO2F4:Mn4+为十字交叉的片状结构,颗粒均匀,具有92%以上的量子产率,具有优异的发光性能,发光温度可达到90℃,在潮湿环境中具有优异的稳定性、L90值达到5500h以上,本发明采用的原料便宜、易得,制备方法简单,制备成本低,产率高,可有效应用于工业规模生产。
Description
技术领域
本发明涉及发光材料技术领域,具体涉及一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法。
背景技术
近年来Mn4+掺杂氟化物窄带发射的红色荧光粉因其具有发光效率高、热稳定性好、色纯度高以及可以液相合成等突出优点受到了广泛关注,且其谱峰比商用氮化物红色荧光粉更窄,在宽色域液晶显示背光源应用中具有广阔的商业前景。但是其吸湿性问题还未解决,严重影响了稳定性能并导致应用受限,目前氟氧化物荧光粉因其稳定性方面的优势使得该材料的研究越来越多,开发高稳定性、高色纯度并能被近紫外和蓝光有效激发的红色荧光材料显得十分重要。
钼酸盐体系荧光粉多为自激活发光材料,热稳定性与化学稳定性好,发射峰半峰宽窄,色纯度高,合成温度低,在近紫外和蓝光区域均有较强吸收,显示出潜在的商业前景。复合钼酸盐荧光粉是指钼酸盐基质的阳离子或阴离子被部分取代,调整发光中心晶格配位环境,发光性能得以改善的荧光粉。比如,MoO4 2-被WO4 2-、PO4 3-、SO4 2-、BO3 3-等取代,同族元素如Mg2+、Ca2+、Sr2+、Ba2+等以及Y3+、Gd3+、La3+之间互换,异族元素Mg2+、Ca2+与Zn2+的互换等。
文献“Red-Emitting K3HF2WO2F4:Mn4+ for Application in Warm-WhitePhosphor-Converted LEDs–Optical Properties and Magnetic ResonanceCharacterization”报道了使用K2MnF6、KF、K2MoO4为原料在HF溶液中用沉淀法制备了新型荧光粉K3HF2MO2F4:Mn4+(M=Mo,W)包含[HF2]-和八面体[MO2F4]2-构建基质单元,这种荧光粉材料是一种高效的发光材料,在低锰的取代下,量子产率接近同一,在潮湿环境下长期稳定存在。但是该文献中使用了昂贵的K2MnF6(制备过程复杂、产率低,售价昂贵)和K2MoO4(阿拉丁定价25.9/g)作为原料,且具体方法被德国科学家掌握,为突破技术垄断,需要寻求制备相同的K3HF2MO2F4:Mn4+材料的新途径。
发明内容
本发明目的在于提供一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法。
本发明目的通过如下技术方案实现:
一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法,采用非水沉淀法制备,其特征在于:所述多相复合钼酸盐氟氧化物纳米荧光材料是K3HF2MoO2F4: Mn4+,具体是取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置5~10min,过滤、洗涤,干燥。
本发明制备的K3HF2MoO2F4:Mn4+中Mn元素取代Mo元素,形成的含量比例为0.07at%~10.8at%。
具体的反应过程如下:
(NH4)6Mo7O24·4H2O +KHF2+ KMnO4+HF→K3HF2MoO2F4:Mn4+。
本发明中以(NH4)6Mo7O24·4H2O为钼源、KMnO4为锰源、钾源,KHF2为钾源、氟源,HF溶液为溶剂、氟源和还原剂,无水乙醇为沉淀剂,通过将(NH4)6Mo7O24·4H2O、KHF2混合溶解在HF,KMnO4单独溶解在HF中,然后混合搅拌反应后,使用无水乙醇沉淀。
在制备过程中容易出现制备的产物形貌差,形成无法分辨的团聚物,分散性差,不能同时形成[HF2]-和[MoO2F4]2-,并组合在一起形成多相复合基质,而是形成的单一的[HF2]-或[MoO2F4]2-阴离子,或者形成多种不同基质的Mn4+荧光体混合在一起,而没有形成多相复合的K3HF2MoO2F4:Mn4+。
本发明中HF作为KMnO4的还原剂,在反应过程中将KMnO4中的Mn7+还原成Mn4+。
进一步,上述(NH4)6Mo7O24·4H2O和KMnO4的用量摩尔比为1:0.05~0.2。
进一步,上述(NH4)6Mo7O24·4H2O和KHF2的用量中K和Mo的摩尔量比为1:3~11。
由于K3HF2MoO2F4:Mn4+是易溶于水的荧光材料,因此本发明全程采用发明采用HF作为溶剂,采用非水沉淀降低了K3HF2MoO2F4:Mn4+的溶解,从而提高了K3HF2MoO2F4:Mn4+的产率。
本发明具有如下技术效果:
本发明制备的K3HF2MoO2F4:Mn4+为十字交叉的片状结构,颗粒均匀,具有92%以上的量子产率,具有优异的发光性能,发光温度可达到90℃,在湿度为80%的潮湿环境中具有优异的稳定性、L90值达到5200h以上,本发明采用的原料便宜、易得,制备方法简单,制备成本低,产率高,可有效应用于工业规模生产。
附图说明
图1:本发明制备的K3HF2MO2F4:Mn4+的XRD图谱。
图2:本发明制备的K3HF2MO2F4:Mn4+的扫描电镜图。
图3:本发明制备的K3HF2MO2F4:Mn4+的激发光谱。
图4:本发明制备的K3HF2MO2F4:Mn4+的发射光谱。
具体实施方式
下面通过实施例对本发明进行具体的描述,有必要在此指出的是,以下实施例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制,该领域的技术人员可以根据上述本发明内容对本发明做出一些非本质的改进和调整。
实施例1
一种K3HF2MoO2F4:Mn4+的制备方法,按如下步骤进行:
取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,(NH4)6Mo7O24·4H2O和KHF2的用量中K和Mo的摩尔量比为1:3,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,(NH4)6Mo7O24·4H2O和KMnO4的用量摩尔比为1:0.05,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置5min,倒出上层清液,再加入无水乙醇反复洗涤沉淀三次后抽滤,置于60℃的真空干燥箱烘干3h。
实施例2
一种K3HF2MoO2F4:Mn4+的制备方法,按如下步骤进行:
取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,(NH4)6Mo7O24·4H2O和KHF2的用量中K和Mo的摩尔量比为1: 11,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,(NH4)6Mo7O24·4H2O和KMnO4的用量摩尔比为1: 0.2,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置10min,倒出上层清液,再加入无水乙醇反复洗涤沉淀三次后抽滤,置于60℃的真空干燥箱烘干3h。
实施例3
一种K3HF2MoO2F4:Mn4+的制备方法,按如下步骤进行:
取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,(NH4)6Mo7O24·4H2O和KHF2的用量中K和Mo的摩尔量比为1:8,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,(NH4)6Mo7O24·4H2O和KMnO4的用量摩尔比为1:0.1,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置8min,倒出上层清液,再加入无水乙醇反复洗涤沉淀三次后抽滤,置于60℃的真空干燥箱烘干3h。
本发明中使用(NH4)6Mo7O24·4H2O为钼源(纯度为99.9%,阿拉丁定价:3.25元/g),其与原料价格便宜、易得。
在制备过程中尝试过多种方法,均无法制得K3HF2MoO2F4:Mn4+,例如,采用KF代替KHF2作为钾源和氟源参与反应时,发现其并不能生成K3HF2MoO2F4:Mn4+,而是直接形成了单独以KHF2为基质的荧光体。
本发明制备的K3HF2MoO2F4:Mn4+荧光体的XRD图谱如图1,可知本发明制备出了K3HF2MoO2F4:Mn4+荧光体。本发明制备的K3HF2MoO2F4:Mn4+荧光体可由近紫外光-可见光激发,尤其是在475nm左右激发,在630nm处有显著的红发发射,其量子率达到92%以上,具有优异的发光性能。在干燥环境下的L90达到5600h,在湿度为80%的环境中检测K3HF2MoO2F4:Mn4+荧光体的发光稳定性,可知其L90依然达到5200h以上(L90指荧光体的光通量衰减为原始光通量的90%)。
Claims (3)
1.一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法,采用非水沉淀法制备,其特征在于:所述多相复合钼酸盐氟氧化物纳米荧光材料是K3HF2MoO2F4: Mn4+,具体是取(NH4)6Mo7O24·4H2O和KHF2溶解在质量浓度为40%的HF溶液中震荡至完全溶解形成溶液A,再将KMnO4溶解在质量浓度为40%的HF酸溶液中震荡至完全溶解形成溶液B,将溶液A和溶液B混合后磁力搅拌20min,边搅拌边滴加无水乙醇,直至深紫色溶液褪色,逐渐形成粉色沉淀,且沉淀不再增加,停止搅拌,静置5~10min,过滤、洗涤,干燥。
2.如权利要求1所述的一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法,其特征在于:所述(NH4)6Mo7O24·4H2O和KMnO4的用量摩尔比为1:0.05~0.2。
3.如权利要求1或2所述的一种多相复合钼酸盐氟氧化物纳米荧光材料的制备方法,其特征在于:所述(NH4)6Mo7O24·4H2O和KHF2的用量中K和Mo的摩尔量比为1:3~11。
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