CN105038793B - 一种高比表面的Y2O3：Eu3+红粉及其制备方法 - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 5
- PXMLGXWGOVHNQX-UHFFFAOYSA-N [Y].[Eu] Chemical compound [Y].[Eu] PXMLGXWGOVHNQX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011148 porous material Substances 0.000 claims abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000975 co-precipitation Methods 0.000 claims description 17
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000005711 Benzoic acid Substances 0.000 claims description 6
- 235000010233 benzoic acid Nutrition 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 239000003086 colorant Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 238000003836 solid-state method Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000005284 excitation Effects 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种高比表面的Y2O3：Eu3+红粉及其制备方法，将钇铕共沉淀，助熔剂与致孔物质混合，再通过高温固相法合成具有多孔结构的稀土三基色红粉。该方法简单，合成的三基色红粉形成的多孔结构，具有较大的比表面积，不仅能提高红粉的亮度，而且蓬松多孔的结构解决了传统红粉比重大引起的三基色灯管涂覆不均匀等问题，并且可以减少涂覆用粉量。
Description
技术领域
本发明涉及荧光粉技术领域，尤其是一种高比表面的Y2O3：Eu3+红粉及其制备方法。
背景技术
稀土三基色节能灯与普通的白炽灯相比节电率高达80％，而且可以获得与日光相近的色温，使得被照物体颜色纯正不失真，其生产过程不污染环境，被公认为当今理想的绿色照明工程，稀土三基色粉在绿色照明领域占有重要地位。但是，稀土三基色红粉由于比重较蓝、绿两种粉大，在涂覆工艺中，引起涂覆不均匀等问题，严重影响成灯质量的稳定。
发明内容
针对现有技术的不足，本发明提供一种高比表面的Y2O3：Eu3+红粉及其制备方法，采用致孔物质制备具有多孔结构的高比表面Y2O3：Eu3+红粉，提高亮度的同时，形成多孔结构的蓬松粉体，比表面积大，解决了传统稀土三基色红粉比重大引起的涂覆不均匀等问题。
为了解决上述技术问题，本发明采用以下技术方案：
一种高比表面的Y2O3：Eu3+红粉，其特征在于，它是具有多孔结构的稀土三基色红粉。
优选的，所述的稀土三基色红粉为Y2O3:Eu3+。
优选的，所述稀土三基色红粉由以下原料组成：钇铕共沉淀，助熔剂，致孔物质。
优选的，钇铕共沉淀、助熔剂与致孔物质的质量比为50-100：1-5：1。
优选的，所述的钇铕共沉淀中铕的质量分数为6.6％。
进一步优选的，所述的钇铕共沉淀为清远加先达稀土有限公司生产，型号为(Y,Eu6.6％)。
优选的，所述的助熔剂为NaF、MgF2、LiF、KF、Li2CO3中的一种或多种。
优选的，所述的致孔物质为炭粉、尿素、苯甲酸、淀粉中的一种或多种。
优选的，所述的致孔物质的粒径小于1微米。
一种制备上述高比表面的Y2O3：Eu3+红粉的方法，其特征在于，包括以下步骤：
(1)将钇铕共沉淀、助熔剂和致孔物质按上述质量比混合均匀，得混合粉末；
(2)将步骤(1)的混合粉末置于氧化炉中，于1200～1400℃温度下煅烧4-8h，自然冷却后研磨均匀，即可。
本发明的有益效果：
(1)提高Y2O3：Eu3+红粉的亮度；
(2)解决现有红粉比重大引起的涂覆不均匀问题；
(3)特殊的多孔结构，具有高比表面积，减少用粉量。
附图说明
图1为对比例1制备的Y2O3：Eu3+红粉的扫描电子显微镜图；
图2为实施例3制备的高比表面的Y2O3：Eu3+红粉的扫描电子显微镜图；
图3为实施例3制备的高比表面的Y2O3：Eu3+红粉的发射光谱图，激发波长为254nm。
具体实施方式
实施例1
将50g铕质量分数为6.6％的钇铕共沉淀、1gKF和0.5g炭粉混合均匀后，于1300℃下煅烧4h，冷却后研磨均匀。
实施例2
将50g铕质量分数为6.6％的钇铕共沉淀、0.5gKF、0.5gLiF和0.5g淀粉，混合均匀后，于1275℃下煅烧8h，冷却后研磨均匀。
实施例3
将100g铕质量分数为6.6％的钇铕共沉淀、1gNaF、0.5g苯甲酸和0.5g淀粉，混合均匀后，于1350℃下煅烧6h，冷却后研磨均匀。
实施例4
将50g铕质量分数为6.6％的钇铕共沉淀、1gLiF、0.5gLi2CO3、0.5g炭粉和0.5g尿素，混合均匀后，于1400℃下煅烧4h，冷却后研磨均匀。
实施例5
将50g铕质量分数为6.6％的钇铕共沉淀与2gKF、1gLiF、0.5gLi2CO3、0.5g尿素、0.3g苯甲酸和0.2g淀粉混合均匀后，于1250℃下煅烧8h，冷却后研磨均匀。
实施例6
将80g铕质量分数为6.6％的钇铕共沉淀、0.5gLi2CO3、1gMgF、1g炭粉和0.2g苯甲酸混合均匀后，于1350℃下煅烧8h，冷却后研磨均匀。
实施例7
将50g铕质量分数为6.6％的钇铕共沉淀、0.5gNaF混合后，加入0.5g炭粉，混合均匀后，于1375℃下煅烧6h，冷却后研磨均匀。
实施例8
将50g铕质量分数为6.6％的钇铕共沉淀与3gMgF2混合后，加入0.5g苯甲酸和0.1g尿素，混合均匀后，于1300℃下煅烧7h，冷却后研磨均匀。
实施例9
将50g铕质量分数为6.6％的钇铕共沉淀与2gMgF2混合后，加入1g尿素，混合均匀后，于1400℃下煅烧8h，冷却后研磨均匀。
对比例1
将50g铕质量分数为6.6％的钇铕共沉淀与0.5gNaF混合均匀后，于1350℃下煅烧6h，冷却后研磨均匀。
实施例3、7、9制备得到的高比表面红粉和对比例1制备得到的红粉分别在激发波长为254nm的激发光激发下得到的发射光谱值及它们的相对亮度如表1所示。
表1实施例3、7、9制备得到的红粉和对比例1制备得到的红粉在激发波长为254nm的激发光激发下得到的发射光谱值及它们的相对亮度
Claims (6)
1.一种制备Y2O3：Eu3+红粉的方法，其特征在于，包括以下步骤：
(1)将钇铕共沉淀、助熔剂和致孔物质混合均匀，得混合粉末；
(2)将步骤(1)的混合粉末置于氧化炉中，于1200～1400℃温度下煅烧4-8h，自然冷却后研磨均匀，即可；其中，所述Y2O3：Eu3+红粉是具有多孔结构的稀土三基色红粉。
2.根据权利要求1所述的方法，其特征在于，钇铕共沉淀、助熔剂与致孔物质的质量比为50-100：1-5：1。
3.根据权利要求1所述的方法，其特征在于，所述的钇铕共沉淀中铕的质量分数为6.6％。
4.根据权利要求1所述的方法，其特征在于，所述的助熔剂为NaF、MgF2、LiF、KF、Li2CO3中的一种或多种。
5.根据权利要求1所述的方法，其特征在于，所述的致孔物质为炭粉、尿素、苯甲酸、淀粉中的一种或多种。
6.根据权利要求1或5所述的方法，其特征在于，所述的致孔物质的粒径小于1微米。
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| US6387339B1 (en) * | 1999-11-11 | 2002-05-14 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide particles and method for preparation thereof |
| CN102766457A (zh) * | 2012-06-29 | 2012-11-07 | 彩虹集团电子股份有限公司 | 一种3d pdp用氧化钇钆铕红色荧光粉的制备方法 |
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| US6387339B1 (en) * | 1999-11-11 | 2002-05-14 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide particles and method for preparation thereof |
| CN102766457A (zh) * | 2012-06-29 | 2012-11-07 | 彩虹集团电子股份有限公司 | 一种3d pdp用氧化钇钆铕红色荧光粉的制备方法 |
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| Title |
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| Facile preparation and fluorescence enhancement of mesoporous Eu-doped-Y2O3 phosphors;Guowei Chen等;《J Mater Sci: Mater Electron》;20150519;第26卷;5970-5974 * |
| 前驱溶液的pH 值对Y2O3:Eu3+荧光粉发光性质的影响;王超男等;《原子与分子物理学报》;20080831;第25卷;760-766 * |
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