CN107474843A - 上转换白光荧光材料的制备方法 - Google Patents
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Abstract
本发明公开了一种上转换白光荧光材料的制备方法,该方法包括:a)将氟化物与稀土化合物粉末按摩尔比混合后,放入研钵中,充分搅拌均匀,使得粉末融合在一起;b)将粉末放置于耐高温陶瓷容器中,并将输出激光光斑覆盖整个粉末表面,激光波长为980nm;激光器输出功率密度至少27W/cm2;反应时间10s~10mins,反应完全后,停止激光照射。本发明能够高效率合成和生产上转换白光荧光材料,整个生产过程反应快速,装置简单,操作便利,原料利用率高达95%,无废料产生,安全绿色无污染。所得材料同时辐射出红色、绿色、蓝色三种波段的荧光,荧光强度一致,不需要额外的稀土离子掺杂调控处理,即可发出白光。
Description
技术领域
本发明属于上转换发光技术领域,特别是涉及一种上转换白光荧光粉的制备方法。
背景技术
近年来,上转换荧光材料以其特殊的性能和广泛的用途成为研究的焦点,它在全色显示、荧光防伪、太阳能电池、生物标记探针等方面有很大的潜在应用价值。
目前关于上转换白光材料的研究有很多,主要是通过控制辐射荧光中红色、绿色、蓝色三基色的强度比值来调控混合荧光的颜色。国内使用最多的上转换荧光材料基质为氟化物或者氟氧化物,因为它们具有较低的声子能量,可以抑制无辐射跃迁的几率,从而提高上转换发光效率。Tm3+,Er3+,Ho3+是三种最常用到的荧光发射激活离子,分别提供三基色中的蓝色、绿色和红色。专利CN105112051A公布了用于上转换白光的镱铥掺杂氟化物的合成方法,采用助熔剂法制备镱铥掺杂氟锰钾,实验过程中需要较长时间,并且步骤复杂操作繁琐。专利CN102277171A公布了一种上转换白光荧光粉的制备方法,采用高温煅烧法合成上转换白光荧光粉,合成过程中需要较高煅烧温度,对设备的要求较高,反应时间较长,需要严格控制温度变化装置。以上缺点严格限制了上转换发光材料在实际工业方向上的应用,所以人们迫切需要研究一种绿色、快速、可控、操作简便的上转换白光荧光材料制备工艺。
发明内容
本发明所要解决的技术问题是提供一种上转换白光荧光材料的制备方法,其能够高效率合成和生产上转换白光荧光材料,整个生产过程反应快速,装置简单,操作便利,原料利用率高达95%,无废料产生,安全绿色无污染。
本发明是通过以下技术方案实现的:一种上转换白光荧光材料的制备方法,其采用激光烧结生长微晶这个核心过程;所述激光烧结生长微晶通过激光烧结稀土氧化物和稀土氟化物的混合粉末或混合粉末压片,在激光照射熔融区生长出微晶。具体制备包括以下步骤:
步骤1,将氟化物与稀土化合物粉末按摩尔比混合后,放入研钵中,充分搅拌均匀,使得粉末融合在一起;所述氟化物︰稀土化合物︰镱离子化合物︰镨离子化合物=1︰1-x-y︰x︰y;其中x的范围是5mol%~99.9mol%,y的范围是0.1mol%~2mol%,稀土化合物为一种或者多种;
步骤2,将步骤1的粉末放置于耐高温陶瓷容器中,并将输出激光光斑覆盖整个粉末表面,其中,激光器的输出激光波长为980nm;激光器输出功率密度至少27W/cm2;反应时间在10s~10mins范围内,反应完全后,停止激光照射;
步骤3,将步骤2的生成物再次研磨,使得颗粒大小尺寸均匀,得到所述上转换白光荧光材料;其中,上转换白光由镱离子(Yb3+)和镨离子(Pr3+)离子之间发生能量跃迁辐射光子产生;镱离子(Yb3+)充当敏化剂,镨离子(Pr3+)充当激活剂。
所述镱离子来源于氧化镱或氟化镱;所述镨离子来源于氧化镨或氟化镨。
所述稀土氧化物和稀土氟化物为氧化镨、氧化镱、氟化镨、氧化铈、氟化钆和氟化钇等,所述混合粉末或混合粉末压片由上述物质混合制成。
所述激光通过高功率激光器发出,高功率激光器的功率、烧结区域和烧结时间通过激光烧结熔融区产生的局部高温实现控制。
与现有技术相比,本发明具有如下优点:
本发明产生上转换白色荧光是基于在980nm激光激励下,镱离子(Yb3+)作为敏化剂吸收光子,与作为激活离子的镨离子(Pr3+)之间发生能量跃迁转移,降低了稀土离子之间的交叉驰豫现象。同时辐射出红色、绿色、蓝色三种波段的荧光,荧光强度一致,不需要额外的稀土离子掺杂调控处理,即可发出白光,操作便利,装置简单,原料利用率高。
附图说明
图1为本发明制备白光荧光粉XRD图谱;
图2为本发明制备白光荧光粉在扫描电子显微镜下得到的产物形貌图;
图3为本发明制备白光荧光粉上转换荧光发射光谱图;
图4为本发明制备白光荧光粉色坐标图;
图5为本发明制备白光荧光粉中Yb3+和Pr3+能级图以及上转换能量传递机制。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
按照摩尔比氟化钠(NaF):氟化镱(YbF3):氧化镨(Pr6O11)为1:0.995:0.0008称取该三种化合物,将三种粉末混合并在玛瑙研钵中充分研磨,使得各化合物粉末混合均匀。随后将得到的粉末放置在耐高温容器中,均匀堆叠成一个厚度为2mm,直径为13mm的圆柱粉体。激光器为连续光固体激光器,波长为980nm,输出功率调至36W,激光照射在粉体表面,其中光斑大小与圆柱粉体直径尺寸一致。烧结持续30s,关闭激光器。将生成物再次研磨,尽量使得颗粒大小尺寸均匀。对生成物进行X射线衍射测试,得到图1中的XRD图谱;进行扫描电子显微镜测试,得到图2中的产物形貌图;在980nm激光激励下,辐射荧光图谱为图3所示;将辐射产生的白色荧光转换成色坐标并在色度图中标示为图4所示。
实施例2
按照摩尔比氟化钠(NaF):氟化钇(YF3):氧化镨(Pr6O11):氧化镱(Yb2O3)为1:0.845:0.0008:0.075称取该四种化合物。将四种粉末混合并在玛瑙研钵中充分研磨,使得各化合物粉末混合均匀。随后将得到的粉末放置在耐高温容器中,均匀堆叠成一个厚度为2mm,直径为13mm的圆柱粉体。激光器为连续光固体激光器,波长为980nm,输出功率调至61W,激光照射在粉体表面,其中光斑大小与圆柱粉体直径尺寸一致。烧结持续40s,关闭激光器。将生成物再次研磨,尽量使得颗粒大小尺寸均匀。
实施例3
按照摩尔比氟化锂(LiF):氟化钇(YF3):氧化镨(Pr6O11):氧化镱(Yb2O3)为1:0.895:0.0008:0.05称取该四种化合物。将四种粉末混合并在玛瑙研钵中充分研磨,使得各化合物粉末混合均匀。随后将得到的粉末放置在耐高温容器中,均匀堆叠成一个厚度为3mm,直径为15mm的圆柱粉体。激光器为连续光固体激光器,波长为980nm,输出功率调至45W,激光照射在粉体表面,其中光斑大小与圆柱粉体直径尺寸一致。烧结持续4mins,关闭激光器。将生成物再次研磨,尽量使得颗粒大小尺寸均匀。
实施例4
按照摩尔比氟化钠(NaF):氟化钇(YF3):氧化镨(Pr6O11):氧化镱(Yb2O3):氧化铈(CeO2)为1:0.875:0.0008:0.05:0.02称取该五种化合物。将五种粉末混合并在玛瑙研钵中充分研磨,使得各化合物粉末混合均匀。随后将得到的粉末放置在耐高温容器中,均匀堆叠成一个厚度为2mm,直径为13mm的圆柱粉体。激光器为连续光固体激光器,波长为980nm,输出功率调至61W,激光照射在粉体表面,其中光斑大小与圆柱粉体直径尺寸一致。烧结持续30s,关闭激光器。将生成物再次研磨,尽量使得颗粒大小尺寸均匀。
实施例5
按照摩尔比氟化钠(NaF):氟化镱(YbF3):氟化镨(PrF3):氟化钆(GdF3)为1:0.6:0.005:0.4称取该四种化合物,质量分别为0.486g,1.6g,0.011g,0.994g。将四种粉末混合并在玛瑙研钵中充分研磨,使得各化合物粉末混合均匀。随后将得到的粉末放置在耐高温容器中,均匀堆叠成一个厚度为2mm,直径为10mm的圆柱粉体。激光器为连续光固体激光器,波长为980nm,输出功率调至38.4W,激光照射在粉体表面,其中光斑大小与圆柱粉体直径尺寸一致。烧结持续22s,关闭激光器。将生成物再次研磨,尽量使得颗粒大小尺寸均匀。
在980nm激光激励下,NaYbF4:Pr3+材料的上转换布局机制图如图5所示。980nm光子能量匹配Yb3+从2F7/2→2F5/2跃迁能量,则Yb3+基态粒子吸收光子,从基态跃迁至激发态。在此晶格场中,Yb3+和Pr3+之间会发生能量共振转移过程,Yb3+将处于激发态的光子能量转移给Pr3+,使得Pr3+处于3H4态粒子跃迁至1G4态。处于1G4态的粒子再次吸收一个光子,跃迁至3P0能级。一旦激发态能级3P0能级积累了大量粒子,这些粒子就会通过辐射光子的过程向基态跃迁。其中,白光荧光粉的发射光谱中波长为490nm、521nm、610nm、660nm、681nm峰分别对应于Pr3+离子的3P0→3H4、1I6→3H5、3P0→3H6、3P0→3F3、3P0→3F3能级的跃迁。
以上所述的具体实施例,对本发明的解决的技术问题、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种上转换白光荧光材料的制备方法,其特征在于,该方法包括以下具体步骤:
步骤1,将氟化物与稀土化合物粉末按摩尔比混合后,放入研钵中,充分搅拌均匀,使得粉末融合在一起;所述氟化物︰稀土化合物︰镱离子化合物︰镨离子化合物= 1︰1-x-y︰x︰y;其中x的范围是5mol% ~ 99.9mol%,y的范围是0.1mol% ~ 2mol%,稀土化合物为一种或者多种;
步骤2,将步骤1的粉末放置于耐高温陶瓷容器中,并将输出激光光斑覆盖整个粉末表面,其中,激光器的输出激光波长为980nm;激光器输出功率密度至少27W/cm2;反应时间在10s~10mins范围内,反应完全后,停止激光照射;
步骤3,将步骤2的生成物再次研磨,使得颗粒大小尺寸均匀,得到所述上转换白光荧光材料;其中,上转换白光由镱离子(Yb3+)和镨离子(Pr3+)离子之间发生能量跃迁辐射光子产生;镱离子(Yb3+)充当敏化剂,镨离子(Pr3+)充当激活剂。
2.根据权利要求1所述的制备方法,其特征在于,所述镱离子来源于氧化镱或氟化镱;所述镨离子来源于氧化镨或氟化镨。
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