CN104830342A - Silicate fluorescent powder capable of exciting blue-green light and preparation method therefor - Google Patents
Silicate fluorescent powder capable of exciting blue-green light and preparation method therefor Download PDFInfo
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- CN104830342A CN104830342A CN201510188151.9A CN201510188151A CN104830342A CN 104830342 A CN104830342 A CN 104830342A CN 201510188151 A CN201510188151 A CN 201510188151A CN 104830342 A CN104830342 A CN 104830342A
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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
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- 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 discloses silicate fluorescent powder capable of exciting blue-green light and a preparation method therefor. The chemical constitution formula of the fluorescent material is as the following: La6-x-yBa2Ca2(SiO4)6F2:xCe<3+>,yTb<3+>, wherein x and y are respectively molar percentage of rear-earth ions Ce<3+> and Tb<3+> which are respectively mixed into a substrate material La6Ba2Ca2(SiO4)6F2; x is greater than or equal to 0.05 but less than or equal to 0.20, and y is greater than or equal to 0.00 but less than or equal to 0.30. Oxides or corresponding salts in the structural formula are selected as raw materials, and the raw materials are roasted for 4-6 hours under a reducing atmosphere at a temperature of 1350 DEG C-1450 DEG C through a high-temperature solid-phase synthesis method to obtain the fluorescent material. The fluorophor can be matched with a near-ultraviolet light-emitting diode to be applied to a white-light LED apparatus with three primary colors. Besides, the fluorescent powder prepared by the preparation method is high in purity and easy to operate, and does not pollute the environment.
Description
Technical field
The present invention relates to luminescent material technical field, particularly, the present invention relates to a kind of white light LEDs borosilicate fluorescent material that can excite blue green light and preparation method thereof.
Background technology
In recent years, energy-saving illumination industry is flourish, but illuminating product is while power saving, reducing energy consumption efficiently, and incident is the mercury pollution problem that cannot evade.White light-emitting diodes (w-LED) solid state lighting is with its less energy-consumption, the significant advantage such as luminous efficiency is high, pollution-free, volume is little, the life-span is long, and future progressively certainly will substitute luminescent lamp and electricity-saving lamp, incandescent light become green illumination light source of future generation.At present; countries in the world commercialization; the mainly fluorescent conversion type w-LED of large-scale production; i.e. coating fluorescent powder on LED chip; the light (as blue light, near-ultraviolet light) of the shorter wavelength sent by LED chip by fluorescent material is transformed into the longer visible ray of wavelength (as ruddiness, green glow, blue light etc.), then forms white light by the photorecombination of different colours.According to the difference of LED chip emission wavelength, two kinds of modes can be divided into again: blue-ray LED+yellow fluorescent powder and purple LED+red/green/blue three primary colors fluorescent powder.Therefore the development of progress to white light LEDs of phosphor technologies has very important effect, and the fluorescent material of research and development near ultraviolet excitation is very necessary.
Summary of the invention
One of the object of the invention is to provide a kind of silicate fluorescent powder of white light LEDs blue green light, La
6-x-yba
2ca
2(SiO
4)
6f
2: xCe
3+, yTb
3+, wherein x and y is doped matrix material La respectively
6ba
2ca
2(SiO
4)
6f
2in rare earth ion Ce
3+and Tb
3+molar percentage, and 0.05≤x≤0.20,0.00≤y≤0.30.This fluor has good color tunability.
Two of the object of the invention is to provide a kind of preparation method preparing above-mentioned novel blue green light silicate luminescent material.This preparation method is simple, easy handling and free from environmental pollution.Concrete technology of preparing plan explanation is as follows:
1) by chemical constitution formula La
6-x-yba
2ca
2(SiO
4)
6f
2: xCe
3+, yTb
3+stoichiometric ratio takes lanthanum trioxide, barium carbonate, calcium carbonate, silicon-dioxide, cerium dioxide, terbium peroxide, and fully porphyrize mixing;
2) by step 1) mixture that obtains inserts crucible, in 1300 DEG C ~ 1450 DEG C temperature lower calcinations 4 hours ~ 6 hours in the High Temperature Furnaces Heating Apparatus of reducing atmosphere, thus obtains the sintered compact that burns till;
3) by step 2) grinding of the sintered compact that obtains becomes powder.
The invention provides a kind of white light LEDs silicate blue powder look fluor La
6-x-yba
2ca
2(SiO
4)
6f
2: xCe
3+, yTb
3+(wherein x and y is doped matrix material La respectively
6ba
2ca
2(SiO
4)
6f
2in rare earth ion Ce
3+and Tb
3+molar percentage, and 0.05≤x≤0.20,0.00≤y≤0.30).Fluorescent material has following characteristics:
1, can effectively be excited by near-ultraviolet light and send blue green light, change rare earth ion Ce
3+and Tb
3+doping can realize radiative luminous intensity and glow color adjustable.
2, the preparation method of material of the present invention is simple, easy handling and free from environmental pollution.
Accompanying drawing explanation
Fig. 1 (a) and (b) are the fluorescent material La prepared by embodiment 1 respectively
5.90ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+and the La prepared by embodiment 2
5.70ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.20Tb
3+powder x-ray diffraction (XRD) figure.La
6ba
4(SiO
4)
6f
2the XRD figure of reference material also provides in FIG as a reference.
The fluorescent material La of Fig. 2 prepared by embodiment 4
5.70ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.20Tb
3+excitation spectrum (monitoring spectrum lambda
emfor 418nm and 545nm) and emmission spectrum (excitation spectrum λ
exfor 282nm) curve synoptic diagram.
Embodiment
With reference to following specific embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited to following specific embodiment.
Embodiment 1: material consists of La
5.90ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+(x=0.10, y=0.00)
By La
5.90ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+in the stoichiometric ratio of each element, accurately take the La of 0.9611g
2o
3, 0.3605g SiO
2, 0.3947g BaCO
3, 0.2002g CaCO
3, 0.0570g NH
4hF
2and the CeO of 0.0172g
2high purity powdered form raw material, is placed in agate mortar grinding about 20 minutes, raw material is fully mixed.Mixing raw material is transferred in alumina crucible, put into High Temperature Furnaces Heating Apparatus.5%H at 1400 DEG C
2with 95%N
2calcine 5 hours in mixed gas, take out after naturally cooling, again grind about 10 minutes, obtain single-phase La
5.90ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+fluorescent material.
Embodiment 2: material consists of La
5.85ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.05Tb
3+(x=0.10, y=0.05)
By La
5.70ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.05Tb
3+in the stoichiometric ratio of each element, accurately take the La of 0.9530g
2o
3, 0.3605g SiO
2, 0.3947g BaCO
3, 0.2002g CaCO
3, 0.0570g NH
4hF
2, 0.0172g CeO
2and 0.0093g Tb
4o
7high purity powdered form raw material, is placed in agate mortar grinding about 20 minutes, raw material is fully mixed.Mixing raw material is transferred in alumina crucible, put into High Temperature Furnaces Heating Apparatus.5%H at 1400 DEG C
2with 95%N
2calcine 5 hours in mixed gas, take out after naturally cooling, again grind about 10 minutes, obtain single-phase La
5.85ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.05Tb
3+fluorescent material.
Embodiment 3: material consists of La
5.80ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.10Tb
3+(x=0.10, y=0.10)
By La
4.850si
2bO
13: 0.050Ce
3+, 0.100Mn
2+in the stoichiometric ratio of each element, accurately take the La of 0.9448g
2o
3, 0.3605g SiO
2, 0.3947g BaCO
3, 0.2002g CaCO
3, 0.0570g NH
4hF
2, 0.0172g CeO
2and 0.0187g Tb
4o
7high purity powdered form raw material, is placed in agate mortar grinding about 20 minutes, raw material is fully mixed.Mixing raw material is transferred in alumina crucible, put into High Temperature Furnaces Heating Apparatus.5%H at 1400 DEG C
2with 95%N
2calcine 5 hours in mixed gas, take out after naturally cooling, again grind about 10 minutes, obtain single-phase La
5.80ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.10Tb
3+fluorescent material.
Embodiment 4: material consists of La
5.70ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.20Tb
3+(x=0.10, y=0.20)
By La
4.800si
2bO
13: 0.050Ce
3+, 0.150Mn
2+in the stoichiometric ratio of each element, accurately take the La of 0.9286g
2o
3, 0.3605g SiO
2, 0.3947g BaCO
3, 0.2002g CaCO
3, 0.0570g NH
4hF
2, 0.0172g CeO
2and 0.0374g Tb
4o
7high purity powdered form raw material, is placed in agate mortar grinding about 20 minutes, raw material is fully mixed.Mixing raw material is transferred in alumina crucible, put into High Temperature Furnaces Heating Apparatus.5%H at 1400 DEG C
2with 95%N
2calcine 5 hours in mixed gas, take out after naturally cooling, again grind about 10 minutes, obtain single-phase La
5.70ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.20Tb
3+fluorescent material.
Embodiment 5: material consists of La
5.60ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.30Tb
3+(x=0.10, y=0.30)
By La
4.750si
2bO
13: 0.050Ce
3+, 0.200Mn
2+in the stoichiometric ratio of each element, accurately take the La of 0.9123g
2o
3, 0.3605g SiO
2, 0.3947g BaCO
3, 0.2002g CaCO
3, 0.0570g NH
4hF
2, 0.0172g CeO
2and 0.0561g Tb
4o
7high purity powdered form raw material, is placed in agate mortar grinding about 20 minutes, raw material is fully mixed.Mixing raw material is transferred in alumina crucible, put into High Temperature Furnaces Heating Apparatus.5%H at 1400 DEG C
2with 95%N
2calcine 5 hours in mixed gas, take out after naturally cooling, again grind about 10 minutes, obtain single-phase La
5.60ba
2ca
2(SiO
4)
6f
2: 0.10Ce
3+, 0.30Tb
3+fluorescent material.
Claims (4)
1. can the fluorescent material of excited blue-green fluorescence, it is characterized in that, the chemical constitution formula of this fluorescent material is La
6-x-yba
2ca
2(SiO
4)
6f
2: xCe
3+, yTb
3+, wherein x and y is doped matrix material La respectively
6ba
2ca
2(SiO
4)
6f
2in rare earth ion Ce
3+and Tb
3+molar percentage, and 0.05≤x≤0.20,0.00≤y≤0.30.
2. prepare the method that white light LEDs according to claim 1 uses the fluorescent material that can excite blue powder look fluorescence, comprising:
1) by chemical constitution formula La
6-x-yba
2ca
2(SiO
4)
6f
2: xCe
3+, yTb
3+stoichiometric ratio takes lanthanum trioxide, barium carbonate, calcium carbonate, silicon-dioxide, ammonium bifluoride, cerium oxide and terbium peroxide, and fully porphyrize mixing;
2) by step 1) mixture that obtains inserts crucible, in 1350 DEG C ~ 1450 DEG C temperature lower calcinations 4 hours ~ 6 hours in the High Temperature Furnaces Heating Apparatus of reducing atmosphere, thus obtains the sintered compact that burns till;
3) by step 2) grinding of the sintered compact that obtains becomes powder.
3. method as claimed in claim 2, it is characterized in that, the phosphorus source of employing is the compound Secondary ammonium phosphate of phosphoric acid, primary ammonium phosphate at least one.The silicon source adopted can be silicon-dioxide, the compound silicic acid at least one that can be converted into silicon-dioxide.
4. method as claimed in claim 2, it is characterized in that, by placing solid carbon or graphite in high temperature process furnances, under making to be in reducing atmosphere in high temperature process furnances, or be the H of 1 ~ 10%: 99 ~ 90% by volume ratio
2and N
2the reaction atmosphere of mixed gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510188151.9A CN104830342A (en) | 2015-04-21 | 2015-04-21 | Silicate fluorescent powder capable of exciting blue-green light and preparation method therefor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510188151.9A CN104830342A (en) | 2015-04-21 | 2015-04-21 | Silicate fluorescent powder capable of exciting blue-green light and preparation method therefor |
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|---|---|
| CN104830342A true CN104830342A (en) | 2015-08-12 |
Family
ID=53808549
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510188151.9A Pending CN104830342A (en) | 2015-04-21 | 2015-04-21 | Silicate fluorescent powder capable of exciting blue-green light and preparation method therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033909A (en) * | 2017-04-27 | 2017-08-11 | 中国科学院长春光学精密机械与物理研究所 | It is a kind of suitable for fluosilicate green emitting phosphor of ultraviolet excitation and preparation method thereof |
| CN116396756A (en) * | 2023-05-01 | 2023-07-07 | 陕西师范大学 | Broad-spectrum cyan-emission oxyfluoride fluorescent powder and preparation method thereof |
| CN116396756B (en) * | 2023-05-01 | 2024-05-03 | 烟台布莱特光电材料有限公司 | Broad-spectrum cyan-emission oxyfluoride fluorescent powder and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740370A (en) * | 2013-12-11 | 2014-04-23 | 中国地质大学（北京） | Apatite-structure fluorescent powder capable of exciting blue green light and preparation method thereof |
| CN103740368A (en) * | 2013-12-11 | 2014-04-23 | 中国地质大学（北京） | Silicon borate fluorescent powder capable of exciting blue pink light and preparation method thereof |
-
2015
- 2015-04-21 CN CN201510188151.9A patent/CN104830342A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740370A (en) * | 2013-12-11 | 2014-04-23 | 中国地质大学（北京） | Apatite-structure fluorescent powder capable of exciting blue green light and preparation method thereof |
| CN103740368A (en) * | 2013-12-11 | 2014-04-23 | 中国地质大学（北京） | Silicon borate fluorescent powder capable of exciting blue pink light and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| QINGFENG GUO ET AL.: "Luminescence properties and energy transfer in La6Ba4(SiO4)6F2:Ce3+,Tb3+ phosphors", 《JOURNAL OF LUMINESCENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033909A (en) * | 2017-04-27 | 2017-08-11 | 中国科学院长春光学精密机械与物理研究所 | It is a kind of suitable for fluosilicate green emitting phosphor of ultraviolet excitation and preparation method thereof |
| CN116396756A (en) * | 2023-05-01 | 2023-07-07 | 陕西师范大学 | Broad-spectrum cyan-emission oxyfluoride fluorescent powder and preparation method thereof |
| CN116396756B (en) * | 2023-05-01 | 2024-05-03 | 烟台布莱特光电材料有限公司 | Broad-spectrum cyan-emission oxyfluoride fluorescent powder and preparation method thereof |
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Application publication date: 20150812 |