CN1117134C - 长余辉无机发光材料的制备方法 - Google Patents

长余辉无机发光材料的制备方法 Download PDF

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CN1117134C
CN1117134C CN 00100321 CN00100321A CN1117134C CN 1117134 C CN1117134 C CN 1117134C CN 00100321 CN00100321 CN 00100321 CN 00100321 A CN00100321 A CN 00100321A CN 1117134 C CN1117134 C CN 1117134C
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张明
霍力
夏仕美
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Sichuan Sunfor Light Co Ltd
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XINLI INDUSTRIAL GROUP Co Ltd SICHUAN
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Abstract

提供了一种稀土离子共激活的IIA、IIIA主族元素氧化物的长余辉无机发光材料的方法,该材料具有的化学组成为aMO·bN2O3·xRO·yTR2O3,其中,M为IIA元素,N为IIIA元素;R是选自Eu、Sm、Yb,TR为镧系元素;0.5≤a≤5,0.5≤b≤7,0.0001≤x≤0.5,0.0001≤y≤0.5;包括:对物料进行在还原性气氛下灼烧,以及将灼烧或获得的产物进一步用硅酸盐溶液或甲基硅油溶液进行后处理。所得到的产品具有均匀的颗粒度和耐水性。

Description

长余辉无机发光材料的制备方法
本发明涉及一种长余辉无机发光材料的制备方法,尤其是涉及稀土离子共激活的IIA、IIIA主族元素氧化物的无机发光材料的方法。
长余辉发光材料是一种经太阳光或其他光源照射后,具有蓄能性能,在暗处能够长时间地发光,可以多次重复蓄光和发光的材料。
以往的蓄光发光材料多为硫化物类型化合物,例如ZnS:Cu(发绿光),或者,CaS:Bi(发紫蓝光),或者,ZnCdS:Cu(发黄一橙色光)。但是,这种硫化物的余辉时间短,且性能不稳定,耐光性差,使用寿命短。基本上不能用于户外,即使使用于钟表表盘,由于其余辉时间只有20~30分钟,也不能满足需要。
另一种过去开发的蓄光性荧光体含有放射性物质。这种材料可以在很长时间内自行发光,但放射性物质是公认的危险污染源,对人体、对环境均会产生严重的损害,所以,国际上已经严禁使用。
九十年代初,人们开发了一种光激发的具有长余辉的发光材料,例如CN1053807A,其公开了一种具有长余辉的发光材料,其一般式为m(Sr1-xEux)O·nAl2O3·yB2O3,其中,1≤m≤5,1≤n≤8,0.001≤x≤0.1,0.001≤y≤0.35。这种长余辉发光材料的亮度和余辉时间都不高。
此外,美国专利5,376,303和5,424,006以及日本特许号8-73845,8-127772公开了Eu2+激活的碱土金属铝酸盐长余辉荧光物质,显示出较高的亮度和余辉时间。但是,由于烧结温度过高,或者是引入过量硼酸降低了烧结温度,使烧结块难于破碎,导致粉体亮度降低较大。同时,由于采用的是N2+H2混合气,使得操作的安全性不好,设备难度增大。又由于烧结温度过高对加热体的要求也更高,费用增加。
另外,铝酸盐发光材料的发光亮度与激发光强度有关,激发光越强,亮度越高,但对弱光激发效果不理想。同时,铝酸盐发光材料遇水分解不稳定。
另外,由于合成温度过高,发光粉的颗粒较粗,不能满足印刷使用。因此,需要制造出细颗粒的发光粉。
本发明的目的在于克服现有技术的不足,改进工艺,在稀土的配比上重新组合,降低成本,提供一种能制造出更高亮度、更长余辉的低成本发光材料的方法。
本发明的另一个目的是提供一种制造在弱光下即可快速激发的发光材料的方法。
本发明的再一个目的是提供一种制造细颗粒的发光粉的方法,该荧光粉同时具有高亮度和余辉时间,满足印刷方面的需要。
本发明的另外一个目的是提供一种制造具有良好耐水性能的发光材料,满足水性涂料的需要。
为了达到上述目的,本发明提供一种蓄光性荧光体的制造方法,所述的荧光体的化学组成满足如下通式:
                    aMO·bN2O3·xRO·yTR2O3其中,
M是选自Sr、Ca、Mg、Zn中的一种或多种元素;
N是选自B、Al、Ga、Sc中的一种或多种元素;
R是选自Eu、Sm、Yb中的一种或多种元素;
TR是选自La、Pr、Y、Nd、Dy、Er、Tm、Ho中的一种或多种的元素;
a、b、x、y是摩尔数;并且,
0.5≤a≤5,
0.5≤b≤7,
0.0001≤x≤0.5,
0.0001≤y≤0.5,优选的是
0.8≤a≤2,
1≤b≤2,
0.01≤x≤0.05,
0.01≤y≤0.05,该方法包括:
按上述比例混合上述氧化物或者对应所述氧化物的草酸盐、碳酸盐或氢氧化物,加入上述物料的体积的0.5~1.5倍的去离子水,研细至2μm以下,烘干,在1200~1400℃下采用H2或H2+CO灼烧2~5小时。
在上述方法中,采用的原料是IIA、IIIA族元素的氧化物所对应的盐类,如草酸盐、碳酸盐或其氢氧化物按组分的配比称重,采用泥浆法,即加入一定量的水,如物料体积的0.5~1.5倍的去离子水,研细,一般研磨到粒度为2μm以下,烘干。然后,利用在高温炉中所发生的如下化学反应得到所需要的H2或H2+CO:
;或者
;或者
其中,也即,通过向高温炉中通入NH3,加热下,使之分解为N2或H2混合气,或者,采用碳粒在此气氛中还原为CO和H2的混合气。在所述的气氛下,在1200~1400℃、优选在1250℃左右灼烧2~5小时。
在上述的灼烧过程中,优选添加了占物料总量0.1~1%(重量)的硫,其作用是改善产品的颗粒度。
灼烧后,将物料冷却到300℃左右,得到细度均匀的发光材料。为了得到耐水性能好的发光材料,进一步将灼烧得到的发光材料的表面用浓度为0.1~2%(重量)的硅酸钠或硅酸钾进行处理,或者用浓度为0.1~2%(重量)的甲基硅油进行处理。其具体的方法是将发光粉过筛后,加入发光粉体积1倍以上到3倍的上述溶液中搅拌,沉淀20分钟-1小时,将上部清液移去,取出沉淀,在70-90℃下烘干,再在150-250℃下烘干,过筛后得到耐水性的发光粉。
通过本发明的方法,将较低稀土比的荧光体材料的性能得以提高,与用常规方法制备的产品相比,产品细度、弱光激发效果、以及余辉持续时间等指标都有提高,并具有耐水特性。
以下通过实施例的方式详细说明本发明,但这些实施例不用来限制本发明的范围。
在下述实施例中,所有试剂的规格均为优级纯。
                         实施例1
      (Sr0.9Ca0.1)O·(Al1.8Ga0.2)O3·0.005EuO·0.005Nd2O3的制备
取Al(OH)3 1.8mol、SrCO3 0.9mol、CaCO3 0.1mol、Ga2O3 0.2mol、Eu2(C2O4)3·10H2O 0.005mol、Nd2(C2O4)3 0.005mol以及H3BO3 0.08mol,用泥浆法研细至2μm以下,烘干,加入占整个物料重量的0.5%的硫粉,将试样加入电炉中,通入氨气,在1250℃下灼烧3小时,然后冷却至300℃,得到发光粉。
在不锈钢容器中加入2倍体积的1%硅酸钠醇溶液,将发光粉过200目筛后,加入溶液中搅拌,沉淀30分钟,将上部清液移去,取出沉淀,在80℃下烘干,再在200℃下烘干,过筛后得到耐水性的发光粉。
所得到的产品的发射峰在530nm,为黄绿色发光体。用200lx的光源激发,激发后亮度降至0.32mcd/m2的时间为65小时。主要性能与已知的同类产品的比较列于表1。
                          实施例2
      SrO·(Al1.8Ga0.10Sc0.10)O3·0.005EuO·0.005Tm2O3的制备
重复实施例1的步骤,不同之处在于所使用的原料是Al(OH)3 1.8mol、SrCO3 1mol、Ga2(CO3)3 0.05mol、Sc2(CO3)3 0.05mol、Eu2(C2O4)3·10H2O 0.005mol、Tm2(C2O4)3 0.005mol以及H3BO3 0.08mol。所得的产品的发射峰在518nm,为绿色发光体。用200lx的光源激发,激发后亮度降至0.32mcd/m2的时间为55小时。主要性能与已知的同类产品的比较列于表1。
                             表1性能指标       实施例1      实施例2       SrAl2O4:0.005Eu,0.010Dy发光亮度       150          120           100发光时间       65小时       55小时        48小时水中pH值       7~8(稳定)   7~8(稳定)    13.5(1小时分解)颗粒度D50     10~13μm    10~13μm     30μm以上+按US 5,424,006的方法制备
                               实施例3
      (Sr0.8Ca0.2)O·1.75Al2O3·0.005EuO·0.005Nd2O3·0.005Er2O3的制备
取Al(OH)3 3.5mol、SrCO3 0.8mol、CaCO3 0.2mol、Eu2(C2O4)3·10H2O 0.005mol、Nd2(C2O4)3 0.005mol、H3BO3 0.08mol以及Er2O3 0.005mol,用泥浆法研细至2μm以下,烘干,加入占整个物料重量的1%的硫粉,将试样加入电炉中,加入13克碳粒,在1300℃下灼烧2小时,然后冷却至300℃,得到发光粉。
在不锈钢容器中加入2倍体积的1%甲基硅油乙醇溶液,将发光粉过200目筛后,加入溶液中搅拌,沉淀30分钟,将上部清液移去,取出沉淀,在80℃下烘干,再在200℃下烘干,过筛后得到耐水性的发光粉。
所得到的产品的发射峰在490nm,为海蓝色发光体。用200lx的光源激发,激发后亮度降至0.32mcd/m2的时间为60小时。主要性能与已知的同类产品的比较列于表2。
                              表2性能指标               实施例3               SrAl4O7:Eu,Dy发光亮度               150                   100发光时间               60                    40颗粒度D50             10~13μm             30μm以上按照US 5,376,303的方法制备
                             实施例4
          (Ca0.9Sr0.1)(Al1.9Y0.1)O4·0.005EuO·0.005Nd2O3的制备
重复实施例3的步骤,不同之处在于所使用的原料是Al(OH)3 1.9mol、CaCO30.9mol、SrCO3 0.1mol、Y2O3 0.1mol、Eu2(C2O4)3·10H2O 0.005mol、Nd2(C2O4)30.005mol以及H3BO3 0.08mol。所得的产品的发射峰在440nm,为蓝紫色发光体。用200lx的光源激发,激发后亮度降至0.32mcd/m2的时间为48小时。主要性能与已知的同类产品的比较列于表3。
                        表3性能指标          实施例4                CaAl2O4:Eu,Nd$发光亮度          160                    100发光时间          48                     20颗粒度D50        10~13μm              35μm以上$按照US 5,376,303的方法制备
                       实施例5~8
                      水性涂料的制备
将固含量25%的水性丙烯酸树脂、占总重量1%的分散剂MS-1、30%的实施例1、2、3或4制备的荧光体、3%的防沉降剂M-5在1000rpm的高速分散剂中混合5分钟,得到均匀的混合体,将所得到的混合体通过120目丝网过滤,分别得到成品1~4。
所得到的成品1~4分别在水中存放三个月后,荧光体的发光未影响。

Claims (4)

1.一种制备稀土离子共激活的IIA、IIIA主族元素氧化物的无机发光材料的方法,该材料具有的化学组成为
               aMO·bN2O3·xRO·yTR2O3其中,
M是选自Sr、Ca、Mg、Zn中的一种或多种元素;
N是选自B、A1、Ga、Sc中的一种或多种元素;
R是选自Eu、Sm、Yb中的一种或多种元素;
TR是选自La、Pr、Y、Nd、Dy、Er、Tm、Ho中的一种或多种元素;
a、b、x、y是摩尔数;并且,
0.5≤a≤5,
0.5≤b≤7,
0.0001≤x≤0.5,
0.0001≤y≤0.5,该方法包括:
按上述比例混合上述的氧化物或对应所述氧化物的草酸盐、碳酸盐或氢氧化物,加入上述物料的体积的0.5~1.5倍的去离子水,研细至2μm以下,烘干,添加占物料总量O.1~1%(重量)的硫,通入NH3或加入碳粒,在1200~1400℃下灼烧2~5小时。
2.如权利要求1所述的方法,其中,所述的a、b、x、y分别为:
0.8≤a≤2,
1≤b≤2,
0.01≤x≤0.05,
0.01≤y≤0.05。
3.如权利要求1所述的方法,进一步包括将灼烧得到的发光材料的表面用浓度为0.1~2%(重量)的硅酸钠或硅酸钾进行处理。
4.如权利要求1所述的方法,进一步包括将灼烧得到的发光材料的表面用浓度为0.1~2%(重量)的甲基硅油进行处理。
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Cited By (1)

* Cited by examiner, † Cited by third party
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CN100485013C (zh) * 2005-07-01 2009-05-06 四川新力光源有限公司 一种复合基质长余辉荧光材料及其制备方法

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* Cited by examiner, † Cited by third party
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CN1301308C (zh) * 2004-01-16 2007-02-21 北京有色金属研究总院 一种高亮度铝酸盐长时发光材料及其制备方法
CN101429432B (zh) * 2008-12-12 2011-11-16 江苏博睿光电有限公司 一种超细粒径高光效长余辉荧光粉及其制造方法
CN109652011B (zh) * 2019-01-21 2021-07-06 广东工业大学 一种紫外-近红外吸收材料及其制备方法与应用

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100485013C (zh) * 2005-07-01 2009-05-06 四川新力光源有限公司 一种复合基质长余辉荧光材料及其制备方法

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