CN108728091A - 一种蓝绿色发光石及其制备方法 - Google Patents
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Abstract
本发明公开了一种蓝绿色发光石及其制备方法,其是由作为主体材料的蓝绿色发光粉体Sr2‑0.5xMxZryZn1‑2y‑zMgzSi2O7(M=Li+、Na+或K+,x=0.001~0.10,y=0.005~0.15,z=0.001~0.10)与作为辅助材料的氧化镁经混合压片后在还原性气氛下经高温煅烧而成。与现有材料不同,本发明发光材料不含稀土金属元素,能有效降低成本,具有较好的商业应用前景,所得发光石经紫外灯光照射15分钟后在暗室可以观察到明亮的蓝绿光,其目测余辉时间可达7小时以上,且硬度高,经玉石硬度测试仪测试,其莫氏硬度为6.0~7.0Mohs,经抛光打磨后表面晶莹剔透,具有很好的观赏价值。
Description
技术领域
本发明属于长余辉发光材料制备领域,具体涉及一种蓝绿色光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,做为材料的发光中心,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。本发明提供了一种由硅酸锶锌为主体制备的蓝绿光石,其材料不含稀贵金属,能有效降低成本,同时能达到相同的发光性能,具有较好的商业前景。
发明内容
本发明的目的在于提供一种蓝绿色光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:
一种蓝绿色发光石,其是由作为主体材料的蓝绿色发光粉体Sr2-0.5xMxZryZn1-2y- zMgzSi2O7(M=Li+、Na+或K+,x=0.001~0.10,y=0.005~0.15,z=0.001~0.10)与作为辅助材料的氧化镁粉末经混合压片后,在还原性气氛下高温煅烧制备而成。
所用蓝绿色发光粉体的重量百分数为80~90 %,氧化镁粉末的重量百分数为10~20%,两者重量百分数之和为100%。
其中,所述蓝绿色发光粉体是采用溶液燃烧联合高温煅烧工艺制备而成;其制备方法包括以下步骤:
1)按Sr2-0.5xMxZryZn1-2y-zMgzSi2O7的化学计量比分别称取ZnO、MgCO3、Sr(NO3)2、ZrOCl2·8H2O、(C2H5)4SiO4及MNO3(M为Li+、Na+或K+,x=0.001~0.10,y=0.005~0.15,z=0.001~0.10),并设所取各原料的总质量为1;
2)将其中易溶于水的Sr(NO3)2、ZrOCl2·8H2O、MNO3与原料总质量5~20%的硼酸、原料总质量30~200%的尿素混合溶解于蒸馏水中,配成物料质量浓度为0.5~4%的澄清溶液A;
3)将6mol/L的硝酸溶液滴加到难溶的ZnO、MgCO3混合物中,至使其完全溶解为止,并加入按体积比1:1配制的(C2H5)4SiO4无水乙醇溶液,再加入蒸馏水配成物料质量浓度为5~20%的澄清溶液B;
4)将溶液A、B混合均匀,置于坩埚中,500~700℃预燃烧5~10分钟,得白色前躯体粉末;
5)将步骤4)所得白色前躯体粉末研磨后置于高温炉中,在由H2与N2按V(H2):V(N2)=2~5:98~95组成的混合气体或CO气体等弱的还原性气氛中,于900~1200℃煅烧2-5小时,得蓝绿色长余辉发光粉体。
所述蓝绿色发光石的制备方法是按比例分别称取蓝绿色发光粉体和氧化镁粉末,将两者混合后加入两者总重量0.8-8%的去离子水润湿,然后于密闭容器中熟化1小时,而后在4~20个大气压压强下用压片机压片成型,再在由H2与N2按V(H2):V(N2)=2~5:98~95组成的混合气体或CO气体等弱的还原性气氛中,于900~1200℃煅烧3~5小时,制得所述蓝绿色发光石。
本发明的显著优点在于:
(1)本发明所制备的发光石为白色固体,能级陷阱为0.917eV,有良好的发光性能,其经15分钟紫外灯照射后,在暗室里可以观察到其发出的明亮的蓝绿光,目测余辉时间可达到7小时以上。
(2)本发明中辅助材料氧化镁的加入能有效改善发光石的硬度,经玉石硬度测试仪测试,所得发光石的莫氏硬度为6.0~7.0Mohs,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为实施例3所得蓝绿色发光石的XRD图。
图2为实施例3所得蓝绿色发光石的激发和发射光谱图。
图3为实施例3所得蓝绿色发光石的热释光谱图。
图4为实施例3所得蓝绿色发光石的余辉衰减曲线。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
1)按Sr1.995Li0.010Zr0.010Zn0.97Mg0.010Si2O7的化学计量比分别称取0.7894 g ZnO、0.0084g MgCO3、4.2220 g Sr(NO3)2、4.1666 g(C2H5)4SiO4、0.0322 g ZrOCl2·8H2O及0.0069g LiNO3;
2)将Sr(NO3)2、ZrOCl2·8H2O、LiNO3与0.5g硼酸、6g尿素混合溶解于1kg蒸馏水中,配成物料质量浓度约为1.08%的澄清溶液A;
3)将6mol/L的硝酸溶液滴加到难溶的ZnO、MgCO3混合物中,至使其完全溶解为止,并加入按体积比1:1配制的(C2H5)4SiO4无水乙醇溶液,再加入100g蒸馏水配成物料质量浓度约为5%的澄清溶液B;
4)将溶液A、B混合均匀,置于坩埚中,500℃预燃烧5分钟,得白色前躯体粉末;
5)将步骤4)所得白色前躯体粉末研磨后置于高温炉中,在由H2与N2按V(H2):V(N2)=2:98组成的混合气体还原性气氛中,于1000℃煅烧2小时,得蓝绿色发光粉体Sr1.995Li0.010Zr0.010Zn0.97Mg0.010Si2O7;
6)分别称取85g蓝绿色发光粉体Sr1.995Li0.010Zr0.010Zn0.97Mg0.010Si2O7和15g氧化镁粉末,将两者混合后加入1g去离子水润湿,于密闭容器中熟化1小时,而后在5个大气压压强下用压片机压片成型,在由H2与N2按V(H2):V(N2)=2:98组成的混合气体还原性气氛中,于1200℃煅烧3小时,制得蓝绿色发光石。
所得蓝绿色发光石经15分钟紫外灯照射后,在暗室里可以观察到其发出的明亮的蓝绿光,目测余辉时间可达到7小时以上。经玉石硬度测试仪测试,所得发光石的莫氏硬度为6.0Mohs,经抛光打磨后表面晶莹剔透,具有很好的观赏价值。
实施例2
1)按Sr1.995Na0.010Zr0.010Zn0.97Mg0.010Si2O7的化学计量比分别称取0.7894 g ZnO、0.0084g MgCO3、4.2220 g Sr(NO3)2、4.1666 g(C2H5)4SiO4、0.0322 g ZrOCl2·8H2O及0.0069g NaNO3;
2)将Sr(NO3)2、ZrOCl2·8H2O、NaNO3与0.5g硼酸、6g尿素混合溶解于2kg蒸馏水中,配成物料质量浓度约为0.54%的澄清溶液A;
3)将6mol/L的硝酸溶液滴加到难溶的ZnO、MgCO3混合物中,至使其完全溶解为止,并加入按体积比1:1配制的(C2H5)4SiO4无水乙醇溶液,再加入80g蒸馏水配成物料质量浓度约为6%的澄清溶液B;
4)将溶液A、B混合均匀,置于坩埚中,600℃预燃烧7分钟,得白色前躯体粉末;
5)将步骤4)所得白色前躯体粉末研磨后置于高温炉中,在CO气体还原性气氛中,于900℃下煅烧3小时,得蓝绿色发光粉体Sr1.995Na0.010Zr0.010Zn0.97Mg0.010Si2O7;
6)分别称取90g蓝绿色发光粉体Sr1.995Na0.010Zr0.010Zn0.97Mg0.010Si2O7和10g氧化镁粉末,将两者混合后加入2g去离子水润湿,于密闭容器中熟化1小时,而后在10个大气压压强下用压片机压片成型,在CO气体还原性气氛中,于900℃煅烧5小时,制得蓝绿色发光石。
所得蓝绿色发光石经15分钟紫外灯照射后,在暗室里可以观察到其发出的明亮的蓝绿光,目测余辉时间可达到8小时以上。经玉石硬度测试仪测试,所得发光石的莫氏硬度为6.5Mohs,经抛光打磨后表面晶莹剔透,具有很好的观赏价值。
实施例3
1)按Sr1.995K0.010Zr0.010Zn0.97Mg0.010Si2O7的化学计量比分别称取0.7894 g ZnO、0.0084g MgCO3、4.2220 g Sr(NO3)2、4.1666 g(C2H5)4SiO4、0.0322 g ZrOCl2·8H2O及0.0069 g KNO3;
2)将Sr(NO3)2、ZrOCl2·8H2O、KNO3与0.5g硼酸、6g尿素混合溶解于3kg蒸馏水中,配成质量浓度约为3.59%的澄清溶液A;
3)将6mol/L的硝酸溶液滴加到难溶的ZnO、MgCO3混合物中,至使其完全溶解为止,并加入按体积比1:1配制的(C2H5)4SiO4无水乙醇溶液,再加入50g蒸馏水配成物料质量浓度约为10%的澄清溶液B;
4)将溶液A、B混合均匀,置于坩埚中,700℃预燃烧10分钟,得白色前躯体粉末;
5)将步骤4)所得白色前躯体粉末研磨后置于高温炉中,在由H2与N2按V(H2):V(N2)=5:95组成的混合气体还原性气氛中,于1200℃下煅烧5小时后,得蓝绿色发光粉体Sr1.995K0.010Zr0.010Zn0.97Mg0.010Si2O7;
6)分别称取80g蓝绿色发光粉体Sr1.995K0.010Zr0.010Zn0.97Mg0.010Si2O7和20g氧化镁粉末,将两者混合后加入0.8g去离子水润湿,于密闭容器中熟化1小时,而后在4个大气压压强下用压片机压片成型,在由H2与N2按V(H2):V(N2)=5:95组成的混合气体还原性气氛中,于1000℃煅烧3小时,制得蓝绿色发光石。
所得蓝绿色发光石经15分钟紫外灯照射后,在暗室里可以观察到其发出的明亮的蓝绿光,目测余辉时间可达到9小时以上。经玉石硬度测试仪测试,所得发光石的莫氏硬度为7.0Mohs,经抛光打磨后表面晶莹剔透,具有很好的观赏价值。
图1为本实施例所得蓝绿色发光石的XRD图,图中未标记号的峰归属于X射线衍射国际标准数据库标准数据卡片PDF:39-0235,图中带★标记号的峰归属于X射线衍射国际标准数据库标准数据卡片的PDF:45-0946。
图2为本实施例所得蓝绿色发光石的激发和发射光谱图。由图2可见,发光石的激发发射光谱峰强且尖锐,发射峰分别位于485、510及528 nm处,其中485 nm发射峰归属于蓝光,510及528 nm归属于绿光。
图3为本实施例所得蓝绿色发光石的热释光谱图。由图中可见,材料在T=425.04 K处有一个宽的热释峰。
图4为本实施例所得蓝绿色发光石的余辉衰减曲线。由图中可见,材料经历一个快衰减过程而后进入一个十分缓慢的慢衰减过程。
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 (4)
1.一种蓝绿色发光石,其特征在于:其是由作为主体材料的蓝绿色发光粉体Sr2- 0.5xMxZryZn1-2y-zMgzSi2O7与作为辅助材料的氧化镁粉末经混合压片后,在还原性气氛下高温煅烧而成;
其中,M=Li+、Na+或K+,x=0.001~0.10,y=0.005~0.15,z=0.001~0.10。
2. 根据权利要求1所述的蓝绿色发光石,其特征在于:所用蓝绿色发光粉体的重量百分数为80~90 %,氧化镁粉末的重量百分数为10~20 %,两者重量百分数之和为100%。
3.一种如权利要求1所述蓝绿色发光石的制备方法,其特征在于:将分别称取的蓝绿色发光粉体和氧化镁粉末混合,加入去离子水润湿,于密闭容器中熟化1小时,而后在4~20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900~1200℃煅烧3~5小时,制得所述蓝绿色发光石。
4.根据权利要求1所述蓝绿色蓄能型发光石的制备方法,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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