CN1235936A - 光致发光釉及其制造方法 - Google Patents
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Abstract
光致发光釉及其制造方法属于储光釉层及其烧结工艺技术领域。现有的储光釉层采用硫化物储光粉,其亮度低、余辉时间短,另外,在水气和日光作用下易分解,从而导致荧光性能下降甚至丧失。本发明采用掺有稀土元素的碱土金属铝酸盐,如SrAl2O4:Eu2+代替硫化物如ZnS制成光致发光釉,克服了现有技术的弱点。可在陶瓷、玻璃、搪瓷基体上烧制光致发光釉层。用来制做应急标志,其他光致发光标志,以及工艺美术品的装饰。
Description
本发明属于储光釉层及其绕结工艺技术领域。
在现有技术中，有如下相关技术，一是专利公开号为昭58-173182的日本专利，它涉及到一种储光性釉，釉的配比为(wt％)
SiO3 B2O3 K2O Na2O CaO MgO ZnO Al2O3
0～60 10～50 0～5 2～15 0～15 0～5 0～10 1～20
分别取其量合计100％，再掺入5～60％的硫化物储光粉，即ZnS、CdS、CaS、(ZnCd)S中的一种或一种以上，高温烧结成釉层。二是申请号为85100369的中国专利，它涉及到一种夜光釉及制造方法，夜光釉中的储光粉质为ZnS，釉本身配比为(wt％)：
SiO2 B2O3 Na2O CaO ZnO
6～12 11～22 20～40 5～10 7～14
先将上述配合料烧成熟料，粉碎后掺入ZnS，加水研磨成浆即为其所称的釉，其基底是陶、瓷、玻璃。三是中国期刊《玻璃与搪瓷》17卷6期题为“长余辉发光搪瓷的研究”的报导，它涉及到一种储光搪瓷釉及制造方法，先按一定比例称取长石、石英、硼砂、石灰石及氧化锌、氧化钙和氧化锆等添加剂，先高温烧成熟料，磨成粉后加入20％(wt％)ZnS荧光粉，用水调成浆液，涂布或喷涂在搪瓷釉面上，在高温下烧制成发光搪瓷。上述三项技术均采用硫化锌等做为储光物质，当其长期暴露在潮湿空气中或受紫外光照射，则发生分解，储光性能下降。另外，这种储光物质亮度较低，余辉时间也较短。第一种现有技术将硫化物储光粉掺入生料中，在1000℃高温制釉，势必导致储光粉发光强度丧失殆尽。第二、三种现有技术均为先制备熟料，再加入硫化锌储光粉，克服了第一种现有技术的缺陷，但二者一方面或是在陶、瓷、玻璃基底上成釉，或是在搪瓷上成釉，另一方面烧结料仅以涂、喷方式附着于基底上。
为了克服现有技术存在的缺陷和不足，制造一种不易分解、亮度高、余辉时间长的储光釉，并且将制釉温度降至较低温度，即能在陶、瓷、玻璃基底上成釉，又能在有过渡釉层的金属基底上成釉，即能以涂、喷方式，又能以细网印刷方式将发光釉料附着于基底上，我们发明了本发明之光致发光釉及其制造方法。
本发明是这样实现的，首先制备发光釉料，它由玻璃料与发光粉混合而成，玻璃料其配比为(wt％)
PbO2 SiO2 B2O3 K2O Na2O CaO MgO ZnO Al2O3
0～80 10～40 0～50 0～10 0～10 0～10 0～10 0～30 0～10
发光粉采用掺有稀土元素的碱土金属(镓)铝酸盐，通式为R(Ga,Al)2O4∶Re，碱土金属R包括Mg、Ca、Si、Ba，稀土元素Re包括Pr2+、Eu2+。发光粉占发光釉料的5～40wt％。另外，采用如下烧制方法，将发光釉料掺入有机载体制成光致发光油墨，涂刷或印刷在基体上，或者将发光釉料掺入加有其他助剂的水溶液中，喷涂在基体上。基体即可以是陶、瓷、玻璃等一种，也可以是有过渡釉层的金属。然后以5～15℃/min的速率从室温开始升温至630～700℃，保温5～30min，然后自然降温至室温，如此制得本发明之光致发光釉层。
由于采用掺有稀土元素的碱土金属(镓)铝酸盐做储光物质，使得所烧制的光致发光釉亮度高、余辉时间长，当其它条件均相同，现有技术其余辉亮度为0.01cd/m2，而本发明其余辉亮度为0.07cd/m2，现有技术其余辉时间为2～4小时，本发明其余辉时间为10～12小时。另外本发明之光致发光釉耐候性能有较大程度提高，将样品放入水中置于室外3个月，与置于室内空气中的样品相比，余辉亮度几乎一致。从而证明未发生明显水解和紫外线造成的分解。另外本发明还采用了630～700℃的低温制釉，从而确保发光粉储光性能在制釉前后基本不变。本发明在陶、瓷、玻璃、金属基体上均能制釉，同时也可以采用涂刷、印刷、喷涂的方式将发光釉料附着于基体上。
下面结合实例说明本发明。例1，玻璃料配方为：
PbO2 SiO2 B2O3 K2O Na2O ZnO
50 25 13 1 1 1
于900℃加料，在1100℃下熔化30分钟，然后冷却至软化温度以下，倒入冷水中炸碎，烘干，经研磨过200目筛后，制得所需玻璃料。其软化温度为600～650℃，在制釉温度下不与基体及发光粉发生反应。发光粉采用SrAl2O4:Eu2+，过200目筛，其用量占发光釉料的25％。光致发光油墨的制备为，首先调制有机载体，溶剂采用松节油透醇，粘接剂采用乙基纤维素，调合剂采用邻苯二甲酸二丁酯，三者重量比例为15∶1∶1，调匀后掺入发光釉料，发光釉料与有机载体的比例按所制备的光致发光油墨能蘸起拉丝的要求确定。然后将其涂刷或印刷在陶、瓷、玻璃基体上。烧结过程为，以10℃/min的速率从室温升至300℃，保温30分钟，再以相同速率升温至650℃，保温30分钟，然后自然降温至室温，即制得一种光致发光釉。光源采用普通20瓦日光灯照射一分钟后撤除，撤除光源10分钟后，测其亮度在0.07cd/m2以上，荧光光谱峰值在520nm处。例2，玻璃料配方为：
SiO2 B2O3 K2O Na2O CaO MgO ZnO Al2O3
10 50 2 2 3 3 25 5
其他内容与例1相同。发光粉选用SrGaAlO4:Pr2+,Eu2+，其量占发光釉料的40％。水溶液的制备为在水中加悬浮剂三聚磷酸钠、粘接剂甲基纤维素，三者重量比例为100∶1∶1。将发光釉料掺入该水溶液中，重量比例为1∶1。然后喷涂在有过渡釉层的金属基体上，该金属可以是铁或铝。以5℃/min的速率从室温升至680℃，保温10分钟，自然降温至室温。即制得一种光致发光釉，其性能与例1基本相同。
Claims (5)
1、一种光致发光釉，其特征在于，它由玻璃料与发光粉混成发光釉料烧结而成，并且，
(1)玻璃料其配比为(wt％)
PbO2 SiO2 B2O3 K2O Na2O CaO MgO ZnO Al2O3
0～80 10～40 0～50 0～10 0～10 0～10 0～10 0～30 0～10
(2)发光粉为掺有稀土元素的碱土金属(镓)铝酸盐，通式为R(Ga,Al)2O4:Re，碱土金属R包括Mg、Ca、Sr、Ba，稀土元素Re包括Pr2+、Eu2+，
(3)发光粉占发光釉料的5～40wt％。
2、一种烧制权利要求1所述光致发光釉的方法，其特征在于，
(1)发光料附着于基体上的方法有2种：
①将发光釉料掺入有机载体制成光致发光油墨，涂刷或印刷在基体上，
②将发光粉料掺入加有其他助剂的水溶液中，喷涂在基体上，
(2)烧结工艺为：
以5～15℃/min的速率从室温开始升温至630～700℃，保温5～30min，然后自然降温至室温。
3、根据权利要求2所述的烧制方法，其特征在于，所称的有机载体由溶剂、粘接剂、调合剂按15～20∶1∶1的比例配制而成，所称的水溶液为加有悬浮剂(减水剂)、粘接剂这些助剂的水溶液。
4、根据权利要求2所述的烧制方法，其特征在于，所称某种基体即包括有陶、瓷、玻璃，也包括有过渡釉层的金属。
5、根据权利要求2所述的烧结方法，其特征在于，可以升温至300～400℃，保温10～30min再继续升温至630～700℃。
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| Application Number | Priority Date | Filing Date | Title |
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| CN 99107289 CN1235936A (zh) | 1999-05-14 | 1999-05-14 | 光致发光釉及其制造方法 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321093C (zh) * | 2002-08-07 | 2007-06-13 | 张贵洲 | 非放射性环保蓄能发光陶瓷釉料 |
| CN100336886C (zh) * | 2005-04-08 | 2007-09-12 | 中国科学院上海硅酸盐研究所 | 一种氮氧化物荧光材料及其制备方法 |
| WO2010057649A1 (de) * | 2008-11-20 | 2010-05-27 | Eos Gmbh Electro Optical Systems | Verfahren zur identifizierung von lasersinterpulvern mit markern bestehend aus salzen von seltenerdmetallen |
| CN103606391A (zh) * | 2013-11-08 | 2014-02-26 | 江苏科技大学 | 一种用于太阳能电池的铝浆组合物 |
-
1999
- 1999-05-14 CN CN 99107289 patent/CN1235936A/zh active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321093C (zh) * | 2002-08-07 | 2007-06-13 | 张贵洲 | 非放射性环保蓄能发光陶瓷釉料 |
| CN100336886C (zh) * | 2005-04-08 | 2007-09-12 | 中国科学院上海硅酸盐研究所 | 一种氮氧化物荧光材料及其制备方法 |
| WO2010057649A1 (de) * | 2008-11-20 | 2010-05-27 | Eos Gmbh Electro Optical Systems | Verfahren zur identifizierung von lasersinterpulvern mit markern bestehend aus salzen von seltenerdmetallen |
| US10807304B2 (en) | 2008-11-20 | 2020-10-20 | Eos Gmbh Electro Optical Systems | Method for identifying laser sintering powders |
| CN103606391A (zh) * | 2013-11-08 | 2014-02-26 | 江苏科技大学 | 一种用于太阳能电池的铝浆组合物 |
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