CN1357599A - 彩色上转换材料制备方法 - Google Patents
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
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- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 3
- LNUFLCYMSVYYNW-ZPJMAFJPSA-N [(2r,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6r)-6-[(2r,3r,4s,5r,6r)-6-[(2r,3r,4s,5r,6r)-6-[[(3s,5s,8r,9s,10s,13r,14s,17r)-10,13-dimethyl-17-[(2r)-6-methylheptan-2-yl]-2,3,4,5,6,7,8,9,11,12,14,15,16,17-tetradecahydro-1h-cyclopenta[a]phenanthren-3-yl]oxy]-4,5-disulfo Chemical compound O([C@@H]1[C@@H](COS(O)(=O)=O)O[C@@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1[C@@H](COS(O)(=O)=O)O[C@@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1[C@@H](COS(O)(=O)=O)O[C@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1C[C@@H]2CC[C@H]3[C@@H]4CC[C@@H]([C@]4(CC[C@@H]3[C@@]2(C)CC1)C)[C@H](C)CCCC(C)C)[C@H]1O[C@H](COS(O)(=O)=O)[C@@H](OS(O)(=O)=O)[C@H](OS(O)(=O)=O)[C@H]1OS(O)(=O)=O LNUFLCYMSVYYNW-ZPJMAFJPSA-N 0.000 claims 1
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Abstract
本发明涉及一种彩色上转换材料制备方法,属于发光物理学中发光材料的合成方法。(a)该材料由下列组分组成(摩尔百分比):含钇、钆或镧的化合物中的至少一种55～90%,含镱化合物18～40%,含铒、铥、钬、镝、铈或镨的化合物中的至少一种2～4%,含钠、钾、锂、铍、钡、铝、钙、锆、硼、镁或锌化合物中的至少一种1～2%,将上述组分按摩尔百分比称重,研磨混合均匀,在500～1100℃恒温2～8小时,制成烧结体,其可以是玻璃态、陶瓷态、微晶颗粒态,再研成粒度为100～400目的粉末即成。本发明具有工艺简单,化学合成成本低廉,材料发光效率较高,适合工业化规模生产特点。
Description
技术领域 本发明属于发光物理学中发光材料的合成方法。
背景技术 彩色上转换材料能将各种不可见红外波段光束转换成可见光，如用于：各类半导体激光器的红外光检测，红外发光二极管发射光跟踪，YAG等大型激光器光束校对。用于红外防伪可以印刷涂抹于纸张、塑料、纤维制品表面，主要用于商品、商标证券等的防伪，其识别只要通过红外线遥控器或半导体激光器即可。具有结构简单、响应灵敏、使用寿命长、安全性能好、应用范围广等特点。该类产品对红外光束可有效的实现探测、跟踪、识别、校对，适用于科研、医疗、光纤通信、工业加工、军事国防等领域。
目前现有制备上转换材料的方法大多是采用干法或湿法制成，而大规模生产目前只有绿色上转换材料可以实现，该类制备工艺复杂，不易稳定，且价格昂贵。专利文献CN1183552、CN1185475、US5525380、US5541012中对上述方法有所报导。
发明内容 本发明提供一种彩色上转换材料制备方法，使用该方法可以实现红色、蓝色、绿色发光。本发明是将含钇Y、钆Gd、镧La、镱Yb、铒Er、铥Tm、钬Ho、镝Dy、Ce铈或镨Pr的化合物为其氧化物、氟化物、氯化物、硫化物至少一种按一定化学比例混合，同时加入含钠Na、钾k、锂Li、铍Be、钡Ba、铝Al、钙Ca、锆Zr、硼B、镁Mg或锌Zn化合物，为其氟化物、氯化物、氧化物至少一种与其混合，并研磨；也可以是氧化物、氯化物、硫化物，加入氢氟酸，制成氟化物；在500-1100℃高温下烧结；烧结合成时将材料放置在铂金坩锅中，加盖密封，并在真空中或含有氧气氛、氟气氛、氯气氛、硫气氛保护下完成，其可以是玻璃态、陶瓷态、微晶颗粒态再研成粒度为100～400目的粉末即成。
本发明具有工艺简单，化学合成成本低廉，材料发光效率较高，适合工业化规模生产特点。该类材料可以被0.8-1.6微米的不可见红外光激发，发出红、蓝、绿色的可见光，其粒度为10-50um或块体，上述红外发光材料使用功率10mW即可起亮，其发光强度与红外器件功率成一定的正比增长关系，用其生产的器件产品基材可以是：纸板、塑料、玻璃、陶瓷、铁板，并可根据要求订制各种形状、面积、颜色、图案、特殊性能的产品。
具体实施方式
实施例一：
称量Y2O3 9g，
Yb2O3 3.8g，
Er2O3 2g，
加入氢氟酸20ml，将制得的氟化物沉淀加入NaF 5g，一起研磨混匀，烧结时，630℃恒温4小时，制成烧结体，再研成粒度为400目粉末即可，该材料在红外波长970nm激发下即发出绿色的可见光。
实施例二
称量YF 14g，GdF 23g
YbF3 3g
DyF3 0.5g，
NaF 2.8g
一起研磨混匀，在硫气氛保护下烧结，1100℃恒温4小时，制成烧结体，再研成粒度为400目粉末即可，该材料在红外波长970nm激发下即发出绿色的可见光。实施例三：
称量La2O3 5g，
Yb2O3 1.6g
Er2O3 0.2g
MgF2 10g
一起研磨混匀，烧结时，在硫气氛保护下，1200℃恒温2小时，制成烧结体，再研成粒度为.400目粉末即可，该材料在红外波长970nm激发下即发出红色的可见光。
实施例四：
Y2O3 14g
Yb2O3 15g
Tm2O3 0.04g
加入氢氟酸20ml，将制得的氟化物沉淀，研磨混匀，烧结时，650℃恒温4小时，制成烧结体，再研成粒度为400目粉末即可，该材料在红外波长970nm激发下即发出蓝色的可见光。
Claims (6)
1、一种彩色上转换材料的制备方法，其特征在于：
(a)该材料由下列组分组成(摩尔百分比)：
含钇Y、钆Gd或镧La的化合物中的至少一种 55～90％
含镱Yb化合物 18～40％
含铒Er、铥Tm、钬Ho、镝Dy、铈Ce或镨Pr的化合物中的至少一种 2～4％
含钠Na、钾k、锂Li、铍Be、钡Ba、铝Al、钙Ca、锆Zr、硼B、镁Mg或锌Zn化合物中的至少一种 1～2％
(b)将上述组分按摩尔百分比称重，研磨混合均匀，在500～1100℃恒温2～8小时，制成烧结体，其可以是玻璃态、陶瓷态、微晶颗粒态，再研磨成粒度为100～400目的粉末即成。
2、根据权利要求1所述的彩色上转换材料的制备方法，其特征在于：含钇Y、钆Gd、镧La、镱Yb、铒Er、铥Tm、钬Ho、镝Dy、Ce铈或镨Pr的化合物为其氧化物或氟化物或氯化物或硫化物。
3、根据权利要求1所述的彩色上转换材料的制备方法，其特征在于：钠Na、钾k、锂Li、铍Be、钡Ba、铝Al、钙Ca、锆Zr、硼B、镁Mg或锌Zn的化合物为其氟化物或氯化物或氧化物。
4、根据权利要求2所述的彩色上转换材料的制备方法，其特征在于：将含钇Y、钆Gd、镧La、镱Yb、铒Er、铥Tm、、镝Dy、铈Ce、钬Ho或镨Pr的氧化物中加入氢氟酸，制成氟化物。
5、根据权利要求1所述的彩色上转换材料的制备方法，其特征在于：合成时应在真空中或含有氧气氛、氟气氛、氯气氛、硫气氛的保护下高温烧结。
6、根据权利要求1所述的彩色上转换材料的制备方法，其特征在于：该类材料可以被0.8-1.6微米的不可见红外光激发，发出红、蓝、绿色的可见光。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011389206A CN1161447C (zh) | 2001-12-23 | 2001-12-23 | 彩色上转换材料制备方法 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011389206A CN1161447C (zh) | 2001-12-23 | 2001-12-23 | 彩色上转换材料制备方法 |
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| Publication Number | Publication Date |
|---|---|
| CN1357599A true CN1357599A (zh) | 2002-07-10 |
| CN1161447C CN1161447C (zh) | 2004-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011389206A Expired - Fee Related CN1161447C (zh) | 2001-12-23 | 2001-12-23 | 彩色上转换材料制备方法 |
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| Country | Link |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003087259A1 (en) * | 2002-04-15 | 2003-10-23 | Tsinghua University | Nanometer-sized up-converting phosphor fluoride particles and process of preparation |
| CN103059853A (zh) * | 2011-10-19 | 2013-04-24 | 海洋王照明科技股份有限公司 | 钛酸盐上转换发光的荧光粉及其制备方法和应用 |
| CN103235347A (zh) * | 2013-04-23 | 2013-08-07 | 上海洞舟实业有限公司 | 一种多波段红外激光检测器件的制备 |
-
2001
- 2001-12-23 CN CNB011389206A patent/CN1161447C/zh not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003087259A1 (en) * | 2002-04-15 | 2003-10-23 | Tsinghua University | Nanometer-sized up-converting phosphor fluoride particles and process of preparation |
| US7422703B2 (en) | 2002-04-15 | 2008-09-09 | Capital Biochip Company Ltd | Nanometer-sized up-converting phosphor fluoride particles and process of preparation |
| CN103059853A (zh) * | 2011-10-19 | 2013-04-24 | 海洋王照明科技股份有限公司 | 钛酸盐上转换发光的荧光粉及其制备方法和应用 |
| CN103059853B (zh) * | 2011-10-19 | 2014-11-05 | 海洋王照明科技股份有限公司 | 钛酸盐上转换发光的荧光粉及其制备方法和应用 |
| CN103235347A (zh) * | 2013-04-23 | 2013-08-07 | 上海洞舟实业有限公司 | 一种多波段红外激光检测器件的制备 |
| CN103235347B (zh) * | 2013-04-23 | 2016-07-13 | 上海洞舟实业有限公司 | 一种多波段红外激光检测器件的制备 |
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| Publication number | Publication date |
|---|---|
| CN1161447C (zh) | 2004-08-11 |
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