CN1086727C - 细颗粒蓄光性荧光粉及其制备方法 - Google Patents
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Abstract
本发明提供一种以Eu为主要激活剂，具有颗粒细的碱土金属铝酸盐蓄光性荧光粉，其特征在于由下述一般式定义：(A1-x-yDxEy)O·a(G1-zHz)2O3式中A代表碱土金属Mg、Ca、Sr、Ba以及二价金属Zn中至少一种；D代表激活剂Eu；E代表共激活剂：稀土Dy、Nd、Pr、Ho、Er、Tm、Yb、Lu，过渡元素Mn、Zr、Nb、Ti、Sb、Li、Ge、In、W中至少一种；G代表基质共晶体Al；H代表基质共晶体B或Ga，其中0.0001≤x≤0.5，0.0001≤y≤0.3，0.0001≤z≤0.5，0.5≤a≤3.0。
Description
本发明涉及细颗粒蓄光性荧光粉及其制备方法。
蓄光性荧光粉是一种经太阳或其它光源照射后具有蓄光性能、在暗处能够长时间地发出残光、可以多次重复蓄光和再发光的材料。以往蓄光性荧光粉多为硫化物类化合物，例如ZnS：Cu、Co或CaS：Ce等，这类蓄光性荧光粉虽然能够吸收外界光，然后在暗处发射残光，但是残光时间只有1～2小时到十几小时，而且硫化物类化合物弱的化学稳定性决定了它们不耐水，易老化，经历几十小时后亮度就快速下降，使用寿命短。另一类过去开发的蓄光性荧光粉，含有放射性物质，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，所以国际上已严禁使用。
经过长期的研究，在九十年代初第一次出现了以碱土金属铝酸盐为基质的蓄光性荧光粉。这类由Eu激活的铝酸盐蓄光性荧光粉的发光亮度高，残光时间可达24小时以上，而且稳定性优良，耐湿、耐阳光曝晒，寿命长，从而在各个领域获得了应用，例如用夜光油墨、夜光涂料、夜光塑料、夜光玻璃印刷、涂布及制成各种指示或装饰类产品和在低照度光源等方面都得到广泛的推广。
但是，这类铝酸盐蓄光性荧光粉目前在工业规模生产上多半是将α-Al2O3和几种必要组份的化合物混合后，通过1300℃以上的高温固相反应进行的，在这种情况下，得到的最后产物往往是陶瓷状的硬结块，这是因为α-Al2O3的化学活性很低，只有在足够高的温度下才能与碱土金属等其它组份的化合物相互作用，生成单斜晶型铝酸盐，并使稀土激活剂如Eu2O3等进入晶格，形成发光中心和电子深陷阱。对于这样坚硬如实的产品必须施加强而有力的粉碎球磨等处理，才能达到实际要求的几十微米的粉末。但是这样必然使发光晶体结构受到一定程度的破坏，产生许多缺陷。这些缺陷会吸收激发光能而少发光。继续粉碎到1Oμm以下，亮度就急剧下降，残光也快速衰减，再继续细到3μm以下，其微弱的发光已失去了它的实用性，这就使它们在特殊领域如凹版印刷，胶版印刷的夜光油墨，复印夜光炭粉，绸缎织物印染颜料等产业的应用受到限制。为了改善颗粒尺寸粗和分布宽的弊端，以往的很多研究均没有得到很好解决。
另一方面，铝酸盐蓄光性荧光粉是依靠低价Eu离子作为主要激活剂。众所周知，Eu是变价离子，其中+2和+3价态作为荧光粉激活剂时，发出迥然不同的光谱特性，碱土金属铝酸盐只有+2价才会在能带中产生深陷阱，而在制备时，通常是用+3价的Eu2O3作为Eu离子源而添加到烧结前的混合料中。为了把Eu 3+转换为Eu 2+，固相反应必须在还原气氛中进行。不言而喻，能否把Eu 3+全部还原为Eu 2+是影响产品亮度和畜光性能的关键。以往的方法都是用含有少量H2(5％)的流动N2中来实现Eu的还原。这种方法必须在严密的管状炉中进行，不但操作不方便，而且增加了设备费用，又难以形成规模生产。
本发明的目的在于避免上述现有技术中的不足之处而提供一种不降低发光亮度和残光时间而且耐水性良好的细颗粒蓄光性荧光粉及其制造方法。
本发明的目的可以通过以下措施来达到：
根据本发明，蓄光性荧光粉的新组成，可以由下列的一般式来定义：
(A1-x-yDxEy)O·a(G1-zHz)2O3式中A代表碱土金属Mg、Ca、Sr、Ba以及二价金属Zn中至少一种；D代表激活剂Eu；E代表共激活剂：稀土Dy、Nd、Pr、Ho、Er、Tm、Yb、Lu，过渡元素Mn、Zr、Nb、Ti、Sb、Li、Ge、In、W中至少一种；G代表基质共晶体Al；H代表基质共晶体B或Ga，其中
0.0001≤x≤0.5
0.0001≤y≤0.3
0.0001≤z≤0.5
0.5≤a≤3.0
根据本发明，以AlCl3·6H2O作为组份中Al源的起始原料，以SrCl2·6H2O作为组份中Sr源的起始原料，以BaCl2·2H2O作为组份中Ba源的起始原料，以Eu2O3，Dy2O3，H3BO3作为相应Eu、Oy、B的起始原料。
以下将参考附图和制备实例来进一步说明本发明所达到的目的。
图1表示根据本发明制成的由Eu、Dy激活的铝硼酸锶钡蓄光性荧光粉的发射光谱。
图2表示根据本发明制成的由Eu、Dy激活的铝硼酸锶钡蓄光性荧光粉的颗粒分布。
图3表示根据本发明制成的由Eu、Dy激活的铝硼酸锶钡蓄光性荧光粉的在D50＝2um时的残光特性曲线。
图4表示以往起始原料和工艺制得的成品在D50＝10um时的残光特性曲线。
实施例：
准确称取：1、SrCl2·6H2O 269g
2、AlCl3·6H2O 683.2g
3、BaCl2·2H2O 1.74g
4、Eu2O3 1.96g
5、Dy2O3 2.8g
6、Sb2O3 30.7g
7、H3BO3 28g
8、COOH·COOH·2H2O 1.4g
9、(NH4)2CO3 486g
将上述量的Sr、Al、Ba的氯化物溶于5000ml去离子水中为(A)溶液，(NH4)2CO3则溶于另一份2000ml去离子水中为(B)溶液，再将(A)(B)溶液同时注入一只盛有5000ml并预先加热至80℃的去离子水中，加毕，保持80℃继续搅拌15分钟，然后静止冷却，滤出固体物，再烘干，研细，装坩埚，经1300℃烧结1小时取出，冷后混入上述量的Eu2O3、Dy2O3、Sb2O3、H3BO3和COOH·COOH·2H2O，湿磨4小时，倒出，分离弹子，烘干，研细，装入750ml坩埚。炉料装到离坩埚口4～5cm处即可，在它上面放置2只装有粒状活性炭的30ml小坩埚，最后加盖，缝口用废粉调制的淀粉浆糊涂封，移入电炉，在炉内同时放有活性炭坩埚，炉温在30℃内升至1300℃±10℃，保温2小时后切断电源，待降至400℃左右出炉，冷却开盖，去除装炭坩埚，在紫外灯下剔除异色点，再研磨粉碎，通过350目筛布及选粉即得本发明提出的具有亮度较高，蓄光性、耐水性良好的细颗粒蓄光性荧光粉，其性能示于图1、2、3。
本发明的优点为：
按本发明实施例所定义的组份，不包括共激活性中的过渡元素，分别称取对应量的SrCO3，α-Al2O3，BaCO3，Eu2O3、Dy2O3、H3BO3和COOH·COOH·2H2O，共同置于球磨罐中混料3小时，然后按实施例相同的装坩埚和烧结方法，在1300℃保温2小时，再研磨粉碎过筛，其D50＝10um的残光特性曲线示于图4。
比较图3和图4可以看出，根据本发明的制造方法所得的蓄光性荧光粉在D50＝2um时的亮度和残光时间优或相当于D50＝10um的水平。
Claims (3)
1、一种以Eu为主要激活剂，具有颗粒细的碱土金属铝酸盐蓄光性荧光粉，其特征在于由下述一般式定义：
(A1-X-YDXEY)O·a(G1-zHz)2O3式中A代表碱土金属Mg、Ca、Sr、Ba以及二价金属Zn中至少一种；D代表激活剂Eu；E代表共激活剂，共激活剂中同时加入至少一种稀土元素和至少一种过渡金属，稀土元素为Dy、Nd、Pr、Ho、Er、Tm、Yb、Lu中至少一种，过渡金属Zr、Nb、Ti、Sb、Li、Ge、In、W中至少一种；G代表基质共晶体Al；H代表基质共晶体B或Ga，其中
0.0001≤X≤0.5
0.0001≤Y≤0.3
0.0001≤Z≤0.5
0.5≤a≤3.0
2、根据权利要求1所述的细颗粒蓄光性荧光粉，其特征在于蓄光性荧光粉颗粒D50＝2μm。
3、一种细颗粒蓄光性荧光粉制备方法，其特征在于以AlCl3·6H2O作为组份中Al源的起始原料，以SrCl2·6H2O作为组份中Sr源的起始原料，以BaCl2·2H2O作为组份中Ba源的起始原料，以Eu2O3、Dy2O3、H3BO3作为相应Eu、Dy、B源的起始原料，起始原料AlCl3·6H2O、SrCl2·6H2O、BaCl2·2H2O的混合水溶液与铵盐水溶液共同注入80℃水中，保持80℃搅拌15分钟，然后静止冷却，滤出固体物，再烘干，研细，装坩埚，经1300℃烧结1小时分解获得予混体，然后该予混体再和Eu2O3、Dy2O3、Sb2O3、H3BO3和COOH·COOH·2H2O混合，湿磨4小时，倒出、分离弹子、烘干、装入坩埚，在活性碳存在的条件下从炉温30℃加热到1300℃±10℃，保温2小时，停止加热，降温至400℃出炉，冷至室温后再研磨粉碎，通过350目筛布后即得成品。
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| CN98111112A CN1086727C (zh) | 1998-01-14 | 1998-01-14 | 细颗粒蓄光性荧光粉及其制备方法 |
| JP00627399A JP3209724B2 (ja) | 1998-01-14 | 1999-01-13 | 微粒子状の蓄光性蛍光粉の製造方法及び微粒子状の蓄光性蛍光粉 |
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| CN100345934C (zh) * | 2000-12-18 | 2007-10-31 | 住友化学工业株式会社 | 生产铝酸盐发光体的方法 |
| AT410266B (de) * | 2000-12-28 | 2003-03-25 | Tridonic Optoelectronics Gmbh | Lichtquelle mit einem lichtemittierenden element |
| US7285913B2 (en) * | 2003-08-29 | 2007-10-23 | Matsushita Electric Industrial Co., Ltd. | Plasma display device having blue phosphor layers with alkaline earth metal aluminate containing molybdenum or tungsten |
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| JPH09143463A (ja) * | 1995-06-13 | 1997-06-03 | Beijing City Fengtai Kogyo Toso Horyosho | 高輝度長残光蓄光材料 |
| CN1152018A (zh) * | 1995-07-17 | 1997-06-18 | 北京市丰台区宏业涂装辅料厂 | 长余辉高亮度发光材料及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH09143463A (ja) * | 1995-06-13 | 1997-06-03 | Beijing City Fengtai Kogyo Toso Horyosho | 高輝度長残光蓄光材料 |
| CN1152018A (zh) * | 1995-07-17 | 1997-06-18 | 北京市丰台区宏业涂装辅料厂 | 长余辉高亮度发光材料及其制备方法 |
| CN1144257A (zh) * | 1995-08-29 | 1997-03-05 | 北京市丰台区宏业涂装辅料厂 | 长余辉磷光体及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1212988A (zh) | 1999-04-07 |
| JPH11256153A (ja) | 1999-09-21 |
| JP3209724B2 (ja) | 2001-09-17 |
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