CN110835262B - 一种锆钕离子共同发光中心的蓝绿色硬质发光石及其制备方法 - Google Patents

一种锆钕离子共同发光中心的蓝绿色硬质发光石及其制备方法 Download PDF

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CN110835262B
CN110835262B CN201911139556.8A CN201911139556A CN110835262B CN 110835262 B CN110835262 B CN 110835262B CN 201911139556 A CN201911139556 A CN 201911139556A CN 110835262 B CN110835262 B CN 110835262B
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郑子山
吴梅华
陈雯
陈国良
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Abstract

本发明公开了一种锆钕离子共同发光中心的蓝绿色硬质发光石及其制备方法，其是由作为主体材料的锆钕离子共同发光中心蓝绿色发光粉体xNd2O3·(1‑1.5x)ZrO2·(1‑0.6y)P2O5·yAl2O3(x=0.002~0.08;y=0.001~0.15)与作为辅助材料的铝酸镁粉末混合物经混合压片后在还原性气氛下经高温煅烧而成。本发明所制取的硬质发光石经灯光照射后可发射明亮的蓝绿光，停止光照后在黑暗中可持续发光13小时以上，且硬度高，经玉石硬度测试仪测试，其莫氏硬度为6.3~7.5Mohs，经抛光打磨后表面晶莹剔透，具有很好的观赏价值。

Description

一种锆钕离子共同发光中心的蓝绿色硬质发光石及其制备 方法
技术领域
本发明属于发光材料制备领域，具体涉及一种锆钕离子共同发光中心蓝绿色硬质发光石及其制备方法。
背景技术
长余辉发光材料又称为蓄光型自发光材料，其能够吸收太阳光、紫外光、杂散光等进行蓄能，并在停止光源激发后产生余辉效应，持续发光。至今，长余辉发光材料制品有发光涂料、发光陶瓷、发光橡胶、发光皮革、发光玻璃、发光装饰石等，且其拥有化学稳定性好、光致发光、节能环保等特点，被称为21世纪鲜有发展前途的装饰发光材料。长余辉发光材料由主体材料和激活剂（以及辅助激活剂）组成。目前报道的长余辉发光材料主要是将不同的主体材料进行激活剂掺杂，作为材料的发光中心，以此提高主体物质的发光性能。如发明专利“一种Mn2+掺杂的黄色长余辉发光材料及其制备方法”（申请号：201710651844.6）公开了一种Mn2+掺杂的黄色长余辉发光材料，该发光材料的化学表达式为Ca2-xSn2-yAl2O9:xMn2+,yR3+；其中，0.002≤x≤0.080,，0<y≤0.120；R=Tb、Ce、Dy、Tm、Nd、Gd、Y、Er、La、Pr、Sm、Yb、Lu或Ho中的一种，其中Ca2Sn2Al2O9为主体材料，Mn2+为激活剂，R离子则为辅助激活剂。
大自然中，许多矿石本身具有长余辉发光特性，这些材料因其特殊的发光特性被用于制作各种物品，常见的如夜光杯、夜明珠等。利用蓄光型自发光材料仿制天然夜明珠制作发光石，可减少矿石昂贵的制造成本，使材料趋于商品化。本发明提供了一种锆钕离子共同发光中心蓝绿色硬质发光石，具有很好的发光性能和商业应用前景。
发明内容
本发明的目的在于提供一种锆钕离子共同发光中心的蓝绿色硬质发光石及其制备方法。
为实现上述目的，本发明采用如下技术方案：
一种锆钕离子共同发光中心蓝绿色硬质发光石，是由作为主体材料的锆钕离子共同发光中心蓝绿色发光粉体xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3 (x=0.002~0.08; y= 0.001~0.15)与作为辅助材料的铝酸镁粉末混合物经混合压片后，在还原性气氛下高温煅烧而成。辅助材料的铝酸镁粉末的引入对发光石的硬度发挥极大的作用。双发光中心蓝绿色发光粉体的重量百分数为85~95%，铝酸镁粉末的重量百分数为5~15%，两者重量百分数之和为100%。
上述锆钕离子共同发光中心蓝绿色硬质发光石的制备方法具体为;将分别称取的一种锆钕离子共同发光中心蓝绿色发光粉体及铝酸镁粉末混合物混合，加入去离子水润湿，于密闭容器中熟化2-3小时，而后在6-26个大气压压强下用压片机压片成型，再置于还原性气氛中，于950~1200℃煅烧2~5小时，制得所述蓝绿色硬质发光石。
进一步地，还原性气氛是由H2与N2按体积比2~5:98~95组成的混合气体或CO气体。
其中，所述锆钕离子共同发光中心蓝绿色发光粉体采用高温预烧结合压片高温煅烧破碎的制备工艺在弱还原性气氛中制备样品；制备方法包括以下步骤：
一种锆钕离子共同发光中心的蓝绿色发光粉体，其化学组成为xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3 (x=0.002~0.08; y= 0.001~0.15)。
制备方法包括以下步骤：
1) 按化学计量比分别称取原料纳米ZrO2、NH4H2PO4、Nd2O3、Al2O3 ，并按xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3 (x=0.002~0.08; y= 0.001~0.15)的摩尔百分比为2-20 mol%称取助熔剂H3BO3；
2) 将称好的原材料混合后置于球磨罐中并加入无水乙醇至罐的高度一半处，以600~1000 r/min的转速研磨2~4小时后，把原材料混合物取出于100℃下风干半小时后转移至坩埚中；
3) 将坩埚置于箱式炉中，在900 ℃下预烧2小时获得产物前驱体粉末，冷却后把产物前驱体粉末置于球磨罐中并加入无水乙醇至罐的高度一半处，以600~1000 r/min的转速研磨2~ 4小时后，把产物前驱体粉末取出于100 ℃下风干半小时，而后用压力机在5-15个大气压压力下压成片状置于坩埚中在弱的还原性气氛（H2、N2或CO）中，于950-1200℃下煅烧3-4小时，制得蓝绿色长余辉发光材料块体xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3 (x=0.002~0.08; y= 0.001~0.15)。发光材料块体经过破碎机破碎或者玛瑙研钵研磨成为发光粉体。
有益效果：本发明所制取的硬质发光石经灯光照射后可发射明亮的蓝绿光，停止光照后在黑暗中可持续发光13小时以上，且硬度高，经玉石硬度测试仪测试，其莫氏硬度为6.3~7.5Mohs，经抛光打磨后表面晶莹剔透，具有很好的观赏价值。
附图说明
图1为本发明制得的锆钕离子共同发光中心的蓝绿色硬质发光石的XRD谱图；
图2为本发明制得的锆钕离子共同发光中心的蓝绿色硬质发光石的激发发射光谱图。
具体实施方式
为进一步公开而不是限制本发明，以下结合实例对本发明作进一步的详细说明。
本技术中锆钕离子共同发光中心的蓝绿色发光粉体的最佳化学组成为0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3。其制备方法包括以下步骤：
1) 按化学计量比分别称取原料纳米ZrO2、NH4H2PO4、Nd2O3、Al2O3 ，并按0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3的摩尔百分比为8 mol%称取助熔剂H3BO3；
2) 将称好的原材料混合后置于球磨罐中并加入无水乙醇至罐的高度一半处，以800 r/min的转速研磨3小时后，把原材料混合物取出于100 ℃下风干半小时后转移至坩埚中；
3) 将坩埚置于箱式炉中，在900 ℃下预烧2小时获得产物前驱体粉末，冷却后把产物前驱体粉末置于球磨罐中并加入无水乙醇至罐的高度一半处，以800 r/min的转速研磨3小时后，把产物前驱体粉末取出于100 ℃下风干半小时，而后用压力机在12个大气压压力下压成片状置于坩埚中在弱的还原性气氛（H2、N2或CO）中，于1200℃下煅烧3小时，制得蓝绿色长余辉发光材料0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3。
实施例1
按锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）的重量百分数为85 %，铝酸镁粉末的重量百分数为5 %，分别称取的锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）及铝酸镁粉末并进行混合，加入去离子水润湿，于密闭容器中熟化2小时，而后在6个大气压压强下用压片机压片成型，再置于CO还原性气氛中，于950℃煅烧2小时，制得所述蓝绿色硬质发光石。所制备的发光石的余辉时间为 9小时，莫氏硬度为5.0。
实施例2
按锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）的重量百分数为90 %，铝酸镁粉末的重量百分数为10 %，分别称取的锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）及铝酸镁粉末并进行混合，加入去离子水润湿，于密闭容器中熟化2小时，而后在26个大气压压强下用压片机压片成型，再置于H2/N2(H2和N2体积比为5%比95%)还原性气氛中，于1150℃煅烧3小时，制得所述蓝绿色硬质发光石。所制备的发光石的余辉时间为13小时，莫氏硬度为7.5。
实施例3
按锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）的重量百分数为95 %，铝酸镁粉末的重量百分数为5 %，分别称取的锆钕离子共同发光中心蓝绿色发光粉体（0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3）及铝酸镁粉末并进行混合，加入去离子水润湿，于密闭容器中熟化3小时，而后在15个大气压压强下用压片机压片成型，再置于H2/N2(H2和N2体积比为3%比97%)还原性气氛中，于1200℃煅烧5小时，制得所述蓝绿色硬质发光石。所制备的发光石的余辉时间为11 小时，莫氏硬度为6.5。
图1为锆钕离子共同发光中心的蓝绿色硬质发光石的XRD谱图，本技术所制备的样品的物相主要由物相PDF#49-1079和物相PDF#21-1152以及部分物相PDF#36-0352所组成。图2为锆钕离子共同发光中心的蓝绿色硬质发光石的激发发射光谱，487 nm属于蓝光范围、521 nm和545 nm落在绿光范围。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。

Claims (3)

1.一种锆钕离子共同发光中心的蓝绿色硬质发光石，其特征在于：其是由作为主体材料的锆钕离子共同发光中心蓝绿色发光粉体与作为辅助材料的铝酸镁粉末混合物经混合压片后，在还原性气氛下高温煅烧而成；所述锆钕离子共同发光中心蓝绿色发光粉体的化学组成为xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3 ；x=0.002~0.08；y= 0.001~0.15；
将锆钕离子共同发光中心蓝绿色发光粉体及铝酸镁粉末混合物混合，加入去离子水润湿，于密闭容器中熟化2-3小时，然后在6-26个大气压压强下用压片机压片成型，再置于还原性气氛中，于950~1200℃煅烧2~5小时，制得锆钕离子共同发光中心的蓝绿色发光石。
2.根据权利要求1所述的锆钕离子共同发光中心蓝绿色硬质发光石，其特征在于：所述锆钕离子共同发光中心的蓝绿色硬质发光石中锆钕离子共同发光中心蓝绿色发光粉体的重量百分数为85~95%，铝酸镁粉末的重量百分数为5~15 %，两者重量百分数之和为100%。
3.根据权利要求1所述的锆钕离子共同发光中心蓝绿色硬质发光石，其特征在于：所述还原性气氛是由H2与N2按体积比2~5:98~95组成的混合气体或CO气体。
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