CN101376808A - 红色长余辉发光粉体La2O2S:Sm的合成方法 - Google Patents
红色长余辉发光粉体La2O2S:Sm的合成方法 Download PDFInfo
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 abstract description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 3
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Abstract
本发明公开了一种红色长余辉发光粉体La2O2S:Sm的合成方法。按摩尔比1∶1∶2称取La2O3、Na2CO3和S；加入Sm2O3作为激活剂，加入量为La2O3摩尔数的2％～8％；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的5％～20％；在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚，两个坩埚的间隙中填充碳粒；将坩埚置于微波炉中加热20～40min，冷却后取出即得样品。微波法能够快速合成纯度高、结晶好、粒度均匀的La2O2S:Sm发光粉体，并且十二烷基硫酸钠的加入能降低颗粒的团聚和长大，可得到粒径较小的发光粉体，有效提高了粉体的发光强度。
Description
技术领域
本发明涉及无机粉末材料合成技术，特别是涉及一种红色长余辉发光粉体La2O2S:Sm的合成方法。
背景技术
红色长余辉荧光粉La2O2S:Sm作为一种新型的发光材料，具有良好的稳定性，可在夜间照明、夜路标识、通道警示、工艺美术、室内装潢等诸多领域得到广泛的应用，具有重要的经济效益和社会价值。
目前，对红色长余辉荧光粉的研究主要集中在开发新种类、寻求新方法和增强粉体的分散性等方面。发光粉末的合成通常采用传统的高温固相法。固相法的缺点在于合成温度高，时间长，对设备要求高；粒径分布不均匀，难以获得球形颗粒，需粉碎减小粒径，从而使发光体的形貌不完整，晶形遭到破坏，导致发光性能下降。因此寻求新的合成途径已成为红色长余辉荧光材料研究的热门课题。
此外，粉体的分散性对其发光性能有重要影响。一般而言，分散性好的粉体，其发光强度也较好。因此改善粉体的分散性也是提高粉体整体性能的重要方面。
发明内容
本发明的目的在于提供一种红色长余辉发光粉体La2O2S:Sm的合成方法。该方法以La2O3、Na2CO3、S和Sm2O3为原料，采用微波炉为设备快速合成了La2O2S:Sm粉体。并添加阴离子表面活性剂十二烷基硫酸钠为表面改性剂，以此增加粉体的分散性，提高其发光性能。
本发明采用的技术方案是：
以稀土氧化物La2O3、助熔剂Na2CO3、硫化剂S为原料，三者摩尔比为1:1:2；以Sm2O3作为掺入的激活剂，加入量为La2O3摩尔数的2％～8％；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的5％～20％；按比例称取上述原料，在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚；因原料本身不能很好地吸收微波，所以在双坩埚的间隙填充碳粒作为微波吸收剂；将坩埚置于微波炉中微波加热20～40min，冷却后取出即得红色长余辉发光粉体La2O2S:Sm。
本发明具有的有益效果是：
1.合成速度快。微波法与传统加热方法相比，被加热物质是内部整体同时发热，升温速度较快，从而显著缩短加热时间。所以，微波合成可以有效节省能源。
2.改进了合成材料的结构与性能。由于微波加热速度快，避免了材料合成过程中晶粒的异常长大，能够在短时间内合成纯度高、粒径细、粒度分布均匀的La2O2S:Sm粉体材料。
3.为解决粉体的团聚和分散问题提供了一种简单、实用的方法。
表面活性剂分子可吸附包裹在初始形成的晶粒表面，一方面阻止了粒子之间的相互结合团聚，另一方面可减缓、控制粒子的生长，最终可得到颗粒较小、分散性好的粉体，其发光性能也得到一定程度的增强。
附图说明
图1是实施例1合成的红色长余辉发光粉体La2O2S:Sm的XRD谱图。
图2是未添加SDS的La2O2S:Sm粉体和实施例1、2、3合成的La2O2S:Sm粉体的发射光谱图。
具体实施方式
本发明选用纯度均为分析纯的La2O3、Na2CO3、S、和Sm2O3为合成La2O2S:Sm发光粉体的原料。表面改性剂为十二烷基硫酸钠(C12H25NaO4S，SDS)。合成方式为微波合成，微波炉型号为Panasonic NN-GD587S。
实施例1：
称取1.629g(0.005mol)La2O3、0.530g(0.005mol)Na2CO3和0.320g(0.010mol)S，三者摩尔量之比为1:1:2，加入摩尔数为La2O3用量5％(0.087g)的Sm2O3作为激活剂；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的5％(0.072g)。将上述原料在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚，在两个坩埚的间隙中填充碳粒作为微波吸收剂；将坩埚置于微波炉中，频率为2.45GHz，调节功率为低档，时间20min，冷却后取出合成产物。
实施例2：
称取3.258g(0.010mol)La2O3、1.060g(0.010mol)Na2CO3和0.640g(0.020mol)S，三者摩尔量之比为1:1:2，加入摩尔数为La2O3用量2％(0.070g)的Sm2O3作为激活剂；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的10％(0.288g)。将上述原料在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚，在两个坩埚的间隙中填充碳粒作为微波吸收剂；将坩埚置于微波炉中，频率为2.45GHz，调节功率为中档，时间30min，冷却后取出合成产物。
实施例3：
称取4.887g(0.015mol)La2O3、1.590g(0.015mol)Na2CO3和0.960g(0.030mol)S，三者摩尔量之比为1:1:2，加入摩尔数为La2O3用量8％(0.419g)的Sm2O3作为激活剂；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的20％(0.865g)。将上述原料在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚，在两个坩埚的间隙中填充碳粒作为微波吸收剂；将坩埚置于微波炉中，频率为2.45GHz，调节功率为中高档，时间40min，冷却后取出合成产物。
图1是实施例1合成的红色长余辉发光粉体La2O2S:Sm的XRD谱图。晶体结构与基质La2O2S相同，与PDF标准谱图27-0263相吻合。
图2是未添加SDS的La2O2S:Sm粉体和实施例1、2、3合成的La2O2S:Sm粉体的发射光谱图。由图2可见，添加十二烷基硫酸钠使粉体的发光强度增强，当加入量为10％时的效果最佳。
Claims (1)
1、一种红色长余辉发光粉体La2O2S:Sm的合成方法，其特征在于：以稀土氧化物La2O3、助熔剂Na2CO3、硫化剂S为原料，三者摩尔比为1:1:2；以Sm2O3作为掺入的激活剂，加入量为La2O3摩尔数的2％～8％；并添加十二烷基硫酸钠作为表面改性剂，加入量为La2O3摩尔数的5％～20％；按比例称取上述原料，在研钵中充分研混均匀，装入小刚玉坩埚，压实加盖后放入大坩埚；因原料本身不能很好地吸收微波，所以在双坩埚的间隙填充碳粒作为微波吸收剂；将坩埚置于微波炉中微波加热20～40min，冷却后取出即得红色长余辉发光粉体La2O2S:Sm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286285A (zh) * | 2011-09-02 | 2011-12-21 | 东华大学 | 橙-红光长余辉粉体La2O2S:Sm3+及其制备 |
| CN102827608A (zh) * | 2012-06-07 | 2012-12-19 | 华南农业大学 | 一种纳米红色长余辉发光材料及其制备方法 |
| CN103194218A (zh) * | 2013-04-12 | 2013-07-10 | 天津理工大学 | 一种红色稀土荧光材料的高温微波制备方法 |
| CN104591299A (zh) * | 2015-01-16 | 2015-05-06 | 郑州大学 | 氧化物热电材料Ca3-xKxCo4O9的微波烧结合成方法 |
-
2008
- 2008-08-22 CN CNA2008101203489A patent/CN101376808A/zh active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286285A (zh) * | 2011-09-02 | 2011-12-21 | 东华大学 | 橙-红光长余辉粉体La2O2S:Sm3+及其制备 |
| CN102286285B (zh) * | 2011-09-02 | 2013-10-09 | 东华大学 | 橙-红光长余辉粉体La2O2S:Sm3+及其制备 |
| CN102827608A (zh) * | 2012-06-07 | 2012-12-19 | 华南农业大学 | 一种纳米红色长余辉发光材料及其制备方法 |
| CN103194218A (zh) * | 2013-04-12 | 2013-07-10 | 天津理工大学 | 一种红色稀土荧光材料的高温微波制备方法 |
| CN104591299A (zh) * | 2015-01-16 | 2015-05-06 | 郑州大学 | 氧化物热电材料Ca3-xKxCo4O9的微波烧结合成方法 |
| CN104591299B (zh) * | 2015-01-16 | 2016-06-29 | 郑州大学 | 氧化物热电材料Ca3-xKxCo4O9的微波烧结合成方法 |
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