CN112735931A - 新型荧光屏及其制备方法 - Google Patents
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Abstract
本发明公开了一种新型荧光屏及其制备方法,其包括以下步骤:1)采用共沉淀法制备绿色荧光粉颗粒,粒径为1.5~3μm,化学通式为(La0.9Ln0.1‑xTbx)PO4,0.01≤x≤0.1,Ln为稀土离子中的一种或者几种的组合;2)将粘结剂均匀的刷涂在基底材料表面,形成粘结层;3)将所述绿色荧光粉颗粒与树脂胶在溶剂内均匀混合,获得荧光粉溶液;4)将荧光粉溶液均匀刷涂在所述粘结层上,获得荧光层;5)对获得荧光层的基底材料进行加热,然后在荧光层表面设有保护层膜,制得的新型荧光屏,具有高分辨率和高发光效率,可以广泛应用于等离子体平板显示器、平板显示器等显示器以及场发射显示器领域中。
Description
技术领域
本发明涉及荧光屏技术领域,特别涉及一种新型荧光屏及其制备方法。
背景技术
目前,现代科学技术的发展,传统工业经济向现代信息经济转变,信息技术得到快速发展,如:显示屏从小屏幕发展成大屏幕;电视机从彩视电视发展为液晶电视、投影仪;工业上传统高速相机发展成新型的超高速字分幅相机等,其中显示屏、电视机、高速相机等仪器的重要组分为显示器件,如像增强管、阴极射线管、平板显示器等,而荧光屏为显示器件中不可缺少的元件之一,因此荧光屏的发展显得尤为重要。
荧光屏的发展主要目的是获得高分辨力、高发光效率、高场强荧光屏,主要从两个方面进行研究:一是制备高性能的荧光粉;二是从荧光屏的制备工艺上进行研究。高性能荧光粉虽然有好的发光效率,但荧光屏的制备工艺对荧光粉的性能有直接的影响,如荧光屏太薄,电子束不能被阻挡在荧光材料外,一大量电子损失,能量消耗在基底上,亮度和分辨力均同时受影响;相反,荧光粉层厚度超过电子的穿过深度,在加速电压不变的情况下,电子穿透粉层的能力受到限制,荧光粉吸收一些通过它的光线而使这些光线无法通过电子束,另外粉粒对光线的散射吸收了大量的光,致使亮度降低,分辨力也降低,屏的厚度还与颗粒度大小有密切关系,因此对荧光屏研究成为一种必然。
发明内容
针对上述不足,本发明的目的在于,提供一种高分辨率以及高发光效率的新型荧光屏及其制备方法。
为实现上述目的,本发明所提供的技术方案是:
一种新型荧光屏制备方法,其包括以下步骤:
(1)采用共沉淀法制备绿色荧光粉颗粒,该绿色荧光粉颗粒的化学通式为(La0.9Ln0.1-xTbx)PO4,0.01≤x≤0.1,Ln为稀土离子中的一种或者几种的组合,所述绿色荧光粉颗粒的粒径为1.5~3μm;
(2)将粘结剂均匀的刷涂在基底材料表面,形成粘结层;
(3)将所述绿色荧光粉颗粒与树脂胶在溶剂内均匀混合,获得荧光粉溶液;
(4)将荧光粉溶液均匀刷涂在所述粘结层上,获得荧光层;
(5)对获得荧光层的基底材料进行加热,然后在荧光层表面设有保护层膜,制得的新型荧光屏。
作为本发明的一种优选方案,所述步骤(1)具体包括以下步骤:
(1.1)室温下,按照化学计量比,称取La(NO3)3·6H2O、Ln(NO3)3·6H2O以及Tb(NO3)3·6H2O溶于去离子水配制成0.1M的(La0.9Ln0.1-xTbx)(NO3)3溶液;
(1.2)选择合适的沉淀剂材料配置成溶液作为沉淀剂,然后将沉淀剂缓慢滴加到上述(La0.9Ln0.1-xTbx)(NO3)3溶液中并不断搅拌,使用pH调节剂控制溶液的pH值,滴定结束后所获得的白色沉淀;
(1.3)将白色沉淀陈化、过滤后再多次重复进行水洗和醇洗,获得到的粉末进行烘干后获得绿色荧光粉颗粒。
作为本发明的一种优选方案,所述荧光层剂量为0.5-50mg/cm2。
作为本发明的一种优选方案,所述粘结剂的厚度为0.5~30μm;所述粘结剂分子量为10000-50000,该粘结剂包括但不限于聚乙烯醇缩丁醛树脂、聚乙烯醇缩丙醛树脂、聚乙烯醇缩乙醛树脂等一种或两种树脂组成,将该粘结剂溶解于甲苯、2-丁醇、***、乙酸丁酯等一种或多种有机溶剂再刷涂在基底材料表面。
作为本发明的一种优选方案,所述pH调节剂为盐酸或氢氧化钠等,浓度为0.5~2M。
作为本发明的一种优选方案,所述沉淀剂材料为NH4H2PO4或Na2HPO4·6H2O等,浓度为0.5~2M。
作为本发明的一种优选方案,所述保护层膜的厚度为0.01~9μm;所述保护层膜为含有氨基甲酸酯(甲基)丙烯酸酯、单官能(甲基)丙烯酸酯、多官能(甲基)丙烯酸酯的放射线固化性组合物的固化物;或者所述保护层膜为具有粘合层的聚对苯二甲酸乙二醇酯薄膜。
作为本发明的一种优选方案,所述步骤(8)中的烘干温度为40~120℃。
一种实施上述的新型荧光屏制备方法制得的新型荧光屏制品。
本发明采用的绿色荧光粉颗粒化学通式为(La0.9Ln0.1-xTbx)PO4,0.01≤x≤0.1,Ln3 +和Tb3+占据La3+晶格位置,从而导致谱峰移动,Ln3+离子将能量传递给Tb3+,导致Tb3+发生4f→5d跃迁,然后逐步衰减到5D4或5D3态或同时衰减到5D4或5D32个态上,从而发生5D4→7F5跃迁,产生鲜艳的绿色荧光。采用共沉淀法制备的绿色荧光粉颗粒比传统的高温固相法等方法制备的荧光粉颗粒更均匀,再通过刷涂法制备一层均匀的荧光层,构成新型荧光屏,具有高分辨率以及高的发光效率等特点。
本发明的有益效果为:本发明制备方法步骤简单,易于实现,合理利用共沉淀法制备出微米级尺寸的绿色荧光粉颗粒,颗粒均匀,再通过均匀刷涂、固化和覆合有保护膜后获得新型荧光屏,荧光层厚度均匀,能明显提高荧光屏的分辨率和发光效率,可以广泛应用于等离子体平板显示器、平板显示器等显示器以及场发射显示器领域中。
下面结合实施例,对本发明进一步说明。
具体实施方式
实施例1:本实施例提供一种(La0.9Ce0.02Eu0.01Tb0.07)PO4荧光屏制备方法,绿色荧光粉颗粒的化学通式为(La0.9Ce1-x-yEuyTbx)PO4(x=0.07、0.05,y=0.01、0.02),选择x=0.07,y=0.01时为例,其制备方法具体如下:
(1)室温下,按照化学计量比La∶Ce∶Eu∶Tb=0.9∶0.02∶0.01∶0.07称取La(NO3)3·6H2O、Ce(NO3)3·6H2O、Eu(NO3)3·6H2O以及Tb(NO3)3·6H2O溶于去离子水配制成0.1M的(La0.9Ce0.02Eu0.01Tb0.07)PO4溶液;
(2)选择NH4H2PO4溶于去离子水配置成0.2M的NH4H2PO4溶液作为沉淀剂,然后,利用自动电位滴定仪以1mL/min速度将沉淀剂缓慢滴加到上述母液中并不断搅拌,使用0.5M盐酸控制溶液的pH值为1,滴定结束后将所获得的白色沉淀;
(3)将白色沉淀陈化3天、过滤后再多次重复进行水洗和醇洗,再将得到的粉末进行70℃烘干后获得绿色荧光粉颗粒;
(4)选择石英玻璃为基底材料进行清洗并甩干后备用;
(5)将聚乙烯醇缩丁醛树脂(平均分子量为30000)和聚氨酯树脂按照0.7:0.3比例混合后,溶解于适量的异丙醇、甲苯、2-丁醇中,充分搅拌后于涂抹在基底材料表面,形成粘结层;
(6)选择气动撒粉的方式将制备的绿色荧光粉颗粒与树脂胶在适量的溶剂异丙醇、甲苯、2-丁醇内均匀混合,均匀搅拌后,在粘结层上刷一层薄而均匀的荧光层;
(7)对获得荧光层的基底材料在氮气氛围下加热到70~80℃,再在荧光粉层表面刷一层厚度为6μm薄而均匀的不具有光散射性的聚对苯二甲酸乙二醇酯保护层膜,即制得新型荧光屏。
实施例2:其与实施例1基本相同,区别点在于:按照化学式中(La0.9Ce0.02Pr0.01Tb0.07)PO4的化学计量比La∶Ce∶Pr:Tb=0.9∶0.02:0.01∶0.07称取La(NO3)3·6H2O、Ce(NO3)3·6H2O、Pr(NO3)3·6H2O以及Tb(NO3)3·6H2O溶于去离子水配制成0.1M的(La0.9Ce0.02Pr0.01Tb0.07)(NO3)3溶液,以及选择环烯烃聚合物(日本Zeon公司制造ZEONEX480R)作为粘结剂树脂,溶解于适量的甲苯中,充分搅拌后于涂抹在基底表面,以及选择含有氨基甲酸酯(甲基)丙烯酸酯作为保护层材料,在荧光粉层表面均匀的刷一层8μm的保护层膜。
需要说明的是,环烯烃聚合物在SP值为10(cal/cm3)1/2以上的溶剂中、在5wt%、25℃的条件下不溶解。
实施例3:其与实施例2基本相同,区别点在于:按照化学式中(La0.9Gd0.02Eu0.01Tb0.07)PO4的化学计量比La∶Gd∶Eu∶Tb=0.9∶0.02∶0.01∶0.07称取La(NO3)3·6H2O、Gd(NO3)3·6H2O、Eu(NO3)3·6H2O以及Tb(NO3)3·6H2O溶于去离子水配制成0.1M的(La0.9Gd0.02Eu0.01Tb0.07)PO4溶液;以及利用自动电位滴定仪以1mL/min速度将沉淀剂缓慢滴加到上述母液中并不断搅拌,0.5M氨水控制溶液的pH值为7-8,滴定结束后将所获得的白色沉淀;按照上述的步骤(3)将白色沉淀陈化3天、过滤后再多次重复进行水洗和醇洗,再将得到的粉末进行65℃烘干后获得绿色荧光粉颗粒。
上述实施例仅为本发明较好的实施方式,本发明不能一一列举出全部的实施方式,凡采用上述实施例之一的技术方案,或根据上述实施例所做的等同变化,均在本发明保护范围内。本发明合理利用共沉淀法制备出微米级尺寸的绿色荧光粉颗粒,所制备的绿色荧光粉颗粒为1.5~3μm,颗粒均匀,再通过步骤(4)-(7)后制得新型荧光屏,荧光层厚度均匀,厚度优选为0.9~1.1mg/cm2。在使用过程中,Ln3+和Tb3+占据La3+晶格位置,从而导致谱峰移动,Ln3+离子将能量传递给Tb3+,导致Tb3+发生4f→5d跃迁,然后逐步衰减到5D4或5D3态或同时衰减到5D4或5D32个态上,从而发生5D4→7F5跃迁,产生鲜艳的绿色荧光,具有高分辨率以及高发光效率等特点,新型荧光屏的分辨率为100-1301p。
根据上述说明书的揭示和教导,本发明所属领域的技术人员还可以对上述实施方式进行变更和修改。因此,本发明并不局限于上面揭示和描述的具体实施方式,对本发明的一些修改和变更也应当落入本发明的权利要求的保护范围内。此外,尽管本说明书中使用了一些特定的术语,但这些术语只是为了方便说明,并不对本发明构成任何限制,采用与其相同或相似方法而得到的其它方法及制品,均在本发明保护范围内。
Claims (9)
1.一种新型荧光屏制备方法,其特征在于:其包括以下步骤:
(1)采用共沉淀法制备绿色荧光粉颗粒,该绿色荧光粉颗粒的化学通式为(La0.9Ln0.1- xTbx)PO4,0.01≤x≤0.1,Ln为稀土离子中的一种或者几种的组合,所述绿色荧光粉颗粒的粒径为1.5~3μm;
(2)将粘结剂均匀的刷涂在基底材料表面,形成粘结层;
(3)将所述绿色荧光粉颗粒与树脂胶在溶剂内均匀混合,获得荧光粉溶液;
(4)将荧光粉溶液均匀刷涂在所述粘结层上,获得荧光层;
(5)对获得荧光层的基底材料进行加热,然后在荧光层表面设有保护层膜,制得的新型荧光屏。
2.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述步骤(1)具体包括以下步骤:
(1.1)室温下,按照化学计量比,称取La(NO3)3·6H2O、Ln(NO3)3·6H2O以及Tb(NO3)3·6H2O溶于去离子水配制成0.1M的(La0.9Ln0.1-xTbx)(NO3)3溶液;
(1.2)选择合适的沉淀剂材料配置成溶液作为沉淀剂,然后将沉淀剂缓慢滴加到上述(La0.9Ln0.1-xTbx)(NO3)3溶液中并不断搅拌,使用pH调节剂控制溶液的pH值,滴定结束后所获得的白色沉淀;
(1.3)将白色沉淀陈化、过滤后再多次重复进行水洗和醇洗,获得到的粉末进行烘干后获得绿色荧光粉颗粒。
3.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述荧光层剂量为0.5-50mg/cm2。
4.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述粘结剂的厚度为0.5~30μm;所述粘结剂分子量为10000-50000,该粘结剂为聚乙烯醇缩丁醛树脂、聚乙烯醇缩丙醛树脂、聚乙烯醇缩乙醛树脂等一种或两种树脂组成,将该粘结剂溶解于甲苯、2-丁醇、***、乙酸丁酯等一种或多种有机溶剂再刷涂在基底材料表面。
5.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述pH调节剂为盐酸或氢氧化钠,浓度为0.5~2M。
6.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述沉淀剂材料为NH4H2PO4或Na2HPO4·6H2O,浓度为0.5~2M。
7.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述保护层膜的厚度为0.01~9μm;所述保护层膜为含有氨基甲酸酯(甲基)丙烯酸酯、单官能(甲基)丙烯酸酯、多官能(甲基)丙烯酸酯的放射线固化性组合物的固化物;或者所述保护层膜为具有粘合层的聚对苯二甲酸乙二醇酯薄膜。
8.根据权利要求1所述的新型荧光屏制备方法,其特征在于:所述步骤(8)中的烘干温度为40~120℃。
9.一种实施权利要求1-8中任意一项所述的新型荧光屏制备方法制得的新型荧光屏制品。
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