CN103045248A - Bismuth and europium ion codoped tungstate fluorescent ceramic powder and preparation method thereof - Google Patents
Bismuth and europium ion codoped tungstate fluorescent ceramic powder and preparation method thereof Download PDFInfo
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- CN103045248A CN103045248A CN2013100009209A CN201310000920A CN103045248A CN 103045248 A CN103045248 A CN 103045248A CN 2013100009209 A CN2013100009209 A CN 2013100009209A CN 201310000920 A CN201310000920 A CN 201310000920A CN 103045248 A CN103045248 A CN 103045248A
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- Prior art keywords
- bismuth
- europium ion
- powder
- tungstate
- ion codoped
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- 239000000843 powder Substances 0.000 title claims abstract description 27
- 229910052693 Europium Inorganic materials 0.000 title claims abstract description 18
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 title claims abstract description 18
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 17
- -1 europium ion Chemical class 0.000 title claims abstract description 17
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 230000005284 excitation Effects 0.000 abstract description 10
- 238000005245 sintering Methods 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 description 6
- 239000010431 corundum Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention provides bismuth and europium ion codoped tungstate fluorescent ceramic powder and a preparation method thereof. The powder comprises MWO4, Eu and Bi at a mole ratio of 1:(0.0005-0.1):(0.0005-0.1), wherein M is one of Mg, Ca, Sr and Ba. MCO3, WO3, Bi2O3 and Eu2O3 are weighed according to the mole ratio, and then mixed uniformly; an obtained mixture is subjected to previous calcining in air at 800-1300 DEG C for 1-5h, and cooled naturally; and the bismuth and europium ion codoped tungstate fluorescent ceramic powder is obtained. The powder has a high-efficiency response characteristic to ultraviolet light excitation, and can emit white light under the ultraviolet light excitation; a luminous color gamut is wide under the ultraviolet light excitation; proportioning of various fluorescent powder is not required; sintering in a reducing atmosphere is not required; and no color temperature drift appears.
Description
Technical field
The invention belongs to display and lighting fluorescent material technology, be specifically related to a kind of ceramic fluorescent powder that under ultraviolet excitation, has the display lighting function.
Background technology
White light LEDs is a kind of novel solid-state illumination energy, and it is energy-conservation with it, long service life, and it is low, pollution-free to consume energy, and the efficient advantages of higher is considered to the new forms of energy that 21 century might replace the traditional lighting light source.Obtain at present white light LEDs and mainly contain two kinds of methods: a kind of is that multi-chip is combined, the LED combination of launching respectively red, green, blue, mixes three kinds of light and forms white light emission.The advantages such as the white light of this scheme has the brightness height, and stability and color developing are good; But cost is high, and driving circuit is complicated, does not have at present large-scale production.Another kind is the fluorescent material conversion hysteria, and with the fluorescent material of blue-ray LED excitation energy emission gold-tinted, remaining blue light and gold-tinted are compounded to form white light.This scheme comparative maturity all on technology and technique is the main product of present industrialization.But the white light that this scheme obtains lacks red composition, and color developing is lower.Because blue light derives from different matrixes with ruddiness, luminous thermostability is undesirable in addition.Mixed fluorescent powder by ultraviolet excitation emission red, green, blue three primary colours, can obtain the white light emission of high-color rendering, cause the problem that heavily absorbs that luminous efficiency descends and the proportioning of fluorescent material to regulate and control masty problem but exist between the different fluorescent material, limited its application.Therefore, if adopt the white light emission fluorescent material of single-matrix, be expected to obtain simultaneously high luminous efficiency and stability of photoluminescence, so that the LED packaging process is simplified greatly, therefore the research of the white emitting fluorescent powder of single-matrix is very active in recent years simultaneously.By contrast, the white light ceramic fluorescent powder material that also lacks in the market the good single-matrix of excellent performance, thermostability and chemical stability.
Summary of the invention
The objective of the invention is narrow for the luminous colour gamut of existing LED lighting fluorescent powder visible light, color developing is lower, the multiple fluorescent material of needs is compound, the problems such as preparation method's cost is high, complicated the invention provides tungstate fluorescence ceramics powder of a kind of bismuth and europium ion codoped and preparation method thereof.
The present invention realizes by following technical proposal: the tungstate fluorescence ceramics powder of a kind of bismuth and europium ion codoped, MWO in this material
4: mol ratio=1:0.0005 of Eu:Bi～0.1:0.0005～0.1; Wherein, M is any one among Mg, Ca, Sr, the Ba.
Another object of the present invention is to provide the preparation method of the tungstate fluorescence ceramics powder of a kind of bismuth and europium ion codoped, through following each step:
(1) presses mol ratio=1:1:0.0005 of M:W:Eu:Bi～0.1:0.0005～0.1, weighing MCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix, wherein, M is any one among Mg, Ca, Sr, the Ba;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 800～1300 ℃ of lower precalcining 1～5h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder of bismuth and europium ion codoped.
The present invention compares with existing phosphor material powder, has following outstanding advantage:
Adopt Bi, Eu ion as active ions, the preparation bismuth, the tungstate white fluorescent powder material of europium ion codoped has efficient response characteristic to ultraviolet excitation, can transmitting white under ultraviolet excitation.Illuminant colour field width under ultraviolet excitation need not multiple fluorescent material proportioning, need not sintering in the reducing atmosphere, colour temperature drift problem can not occur.This fluorescent material presents white light emission under the 340nm ultraviolet excitation, have the Bi of coming from
3+Be positioned at 532nm broadband emission peak and Eu
3+Red characteristic emission; This material can be used as fluorescent lighting, shows the phosphor material powder in field.
Description of drawings
Fig. 1 is the CaWO of the embodiment of the invention 1 gained
4: the emission spectrogram of 0.002Eu:0.005Bi fluorescent material.
Embodiment
Further illustrate content of the present invention below in conjunction with embodiment, but these examples do not limit protection scope of the present invention.
Embodiment 1
(1) presses mol ratio=1:1:0.002:0.005 of Ca:W:Eu:Bi, weighing CaCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 1100 ℃ of lower precalcining 5h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder CaWO of bismuth and europium ion codoped
4: 0.002Eu:0.005Bi.
Embodiment 2
(1) presses mol ratio=1:1:0.0005:0.0005 of Mg:W:Eu:Bi, weighing MgCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 800 ℃ of lower precalcining 5h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder MgWO of bismuth and europium ion codoped
4: 0.0005Eu:0.0005Bi.
Embodiment 3
(1) presses mol ratio=1:1:0.0008:0.01 of Ba:W:Eu:Bi, weighing BaCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 1300 ℃ of lower precalcining 3h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder BaWO of bismuth and europium ion codoped
4: 0.0008Eu:0.01Bi.
Embodiment 4
(1) presses mol ratio=1:1:0.1:0.1 of Sr:W:Eu:Bi, weighing SrCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 1100 ℃ of lower precalcining 1h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder SrWO of bismuth and europium ion codoped
4: 0.1Eu:0.1Bi.
Embodiment 5
(1) presses mol ratio=1:1:0.03:0.009 of Ba:W:Eu:Bi, weighing BaCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix;
(2) step (1) gained compound is placed in the corundum crucible, in air, in 900 ℃ of lower precalcining 4h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder BaWO of bismuth and europium ion codoped
4: 0.03Eu:0.009Bi.
Claims (2)
1. the tungstate fluorescence ceramics powder of a bismuth and europium ion codoped is characterized in that: MWO in this material
4: mol ratio=1:0.0005 of Eu:Bi～0.1:0.0005～0.1; Wherein, M is any one among Mg, Ca, Sr, the Ba.
2. the preparation method of the tungstate fluorescence ceramics powder of a bismuth and europium ion codoped is characterized in that through following each step:
(1) presses mol ratio=1:1:0.0005 of M:W:Eu:Bi～0.1:0.0005～0.1, weighing MCO
3, WO
3, Bi
2O
3And Eu
2O
3, then mix, wherein, M is any one among Mg, Ca, Sr, the Ba;
(2) with step (1) gained compound in air in 800～1300 ℃ of lower precalcining 1～5h, treat naturally cooling, namely obtain the tungstate fluorescence ceramics powder of bismuth and europium ion codoped.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100009209A CN103045248A (en) | 2013-01-04 | 2013-01-04 | Bismuth and europium ion codoped tungstate fluorescent ceramic powder and preparation method thereof |
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|---|---|---|---|
| CN2013100009209A CN103045248A (en) | 2013-01-04 | 2013-01-04 | Bismuth and europium ion codoped tungstate fluorescent ceramic powder and preparation method thereof |
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|---|---|
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Family
ID=48058113
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361049A (en) * | 2013-06-17 | 2013-10-23 | 青岛农业大学 | Tungstate LED (light-emitting diode) fluorescent powder and preparation method thereof |
| CN104263363A (en) * | 2014-10-14 | 2015-01-07 | 中国科学院上海硅酸盐研究所 | 7Al2O3*12CaO white light emitting material co-doped with europium and bismuth ions and preparation method of material |
| CN105199728A (en) * | 2015-06-01 | 2015-12-30 | 井冈山大学 | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof |
| CN107815312A (en) * | 2017-10-27 | 2018-03-20 | 江苏师范大学 | A kind of adjustable Tungstate fluorescent powder of glow color and preparation method thereof |
| CN112851345A (en) * | 2019-11-12 | 2021-05-28 | 深圳市绎立锐光科技开发有限公司 | Fluorescent ceramic and light source device |
| CN117327490A (en) * | 2023-09-28 | 2024-01-02 | 昆明理工大学 | Bi-doped europium salt fluorescent powder and preparation method and application thereof |
Citations (5)
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|---|---|---|---|---|
| JPH04146990A (en) * | 1990-10-09 | 1992-05-20 | Kasei Optonix Co Ltd | Calcium tungstate phosphor and radiation-sensitized paper prepared therefrom |
| CN1876754A (en) * | 2006-07-07 | 2006-12-13 | 中山大学 | Rare earth red fluorescent powder for emitting 400nm bluish violet light for InGaN chip, and its preparation method |
| US20070114495A1 (en) * | 2005-11-23 | 2007-05-24 | National Central University | Red phosphor for white light emitting diodes |
| KR100735287B1 (en) * | 2005-06-10 | 2007-07-03 | 삼성전기주식회사 | Red light emitting phosphor and light emitting device |
| CN102433119A (en) * | 2011-12-09 | 2012-05-02 | 常熟理工学院 | Tungsten molybdate red fluorescent powder for white light-emitting diode (LED) and preparation method of tungsten molybdate red fluorescent powder |
-
2013
- 2013-01-04 CN CN2013100009209A patent/CN103045248A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04146990A (en) * | 1990-10-09 | 1992-05-20 | Kasei Optonix Co Ltd | Calcium tungstate phosphor and radiation-sensitized paper prepared therefrom |
| KR100735287B1 (en) * | 2005-06-10 | 2007-07-03 | 삼성전기주식회사 | Red light emitting phosphor and light emitting device |
| US20070114495A1 (en) * | 2005-11-23 | 2007-05-24 | National Central University | Red phosphor for white light emitting diodes |
| CN1876754A (en) * | 2006-07-07 | 2006-12-13 | 中山大学 | Rare earth red fluorescent powder for emitting 400nm bluish violet light for InGaN chip, and its preparation method |
| CN102433119A (en) * | 2011-12-09 | 2012-05-02 | 常熟理工学院 | Tungsten molybdate red fluorescent powder for white light-emitting diode (LED) and preparation method of tungsten molybdate red fluorescent powder |
Non-Patent Citations (5)
| Title |
|---|
| KANG FENGWEN 等: "Luminescence investigation of Eu3+-Bi3+ co-doped CaMoO4 phosphor", 《JOURNAL OF RARE EARTHS》, vol. 29, no. 9, 30 September 2011 (2011-09-30), pages 837 - 842 * |
| R. B. PODE 等: "Photoluminescence in CaWO4:Bi3+, Eu3+ Material", 《PHYS. STAT. SOL. (B)》, vol. 203, no. 2, 31 October 1997 (1997-10-31), pages 571 - 577 * |
| SUXIA YAN 等: "Enhanced Red Emission in CaMoO4:Bi3+,Eu3+", 《J.PHYS.CHEM.C》, vol. 111, no. 35, 14 August 2007 (2007-08-14), pages 13256 - 13260 * |
| 张丽霞等: "CaWO_4∶Eu~(3+),M~(3+)(M=Tb,Sm,Bi,Dy)的水热合成及发光性能研究", 《广西大学学报(自然科学版)》, vol. 36, no. 03, 30 June 2011 (2011-06-30), pages 440 - 444 * |
| 杨继兰 等: "白光LED用红色荧光粉CaWO4: Eu3+,Li+,Bi3+ 的制备与表征", 《中国稀土学报》, vol. 28, no. 5, 31 October 2010 (2010-10-31), pages 536 - 542 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361049A (en) * | 2013-06-17 | 2013-10-23 | 青岛农业大学 | Tungstate LED (light-emitting diode) fluorescent powder and preparation method thereof |
| CN104263363A (en) * | 2014-10-14 | 2015-01-07 | 中国科学院上海硅酸盐研究所 | 7Al2O3*12CaO white light emitting material co-doped with europium and bismuth ions and preparation method of material |
| CN105199728A (en) * | 2015-06-01 | 2015-12-30 | 井冈山大学 | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof |
| CN105199728B (en) * | 2015-06-01 | 2017-03-22 | 井冈山大学 | Novel Eu＜3+＞ and Mn＜2+＞ co-doped tungstate red fluorescent material |
| CN107815312A (en) * | 2017-10-27 | 2018-03-20 | 江苏师范大学 | A kind of adjustable Tungstate fluorescent powder of glow color and preparation method thereof |
| CN112851345A (en) * | 2019-11-12 | 2021-05-28 | 深圳市绎立锐光科技开发有限公司 | Fluorescent ceramic and light source device |
| CN112851345B (en) * | 2019-11-12 | 2023-09-15 | 深圳市绎立锐光科技开发有限公司 | Fluorescent ceramic and light source device |
| CN117327490A (en) * | 2023-09-28 | 2024-01-02 | 昆明理工大学 | Bi-doped europium salt fluorescent powder and preparation method and application thereof |
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Application publication date: 20130417 |