CN103305216A - Borate red fluorescent powder and preparation method and application thereof - Google Patents
Borate red fluorescent powder and preparation method and application thereof Download PDFInfo
- Publication number
- CN103305216A CN103305216A CN2013102631314A CN201310263131A CN103305216A CN 103305216 A CN103305216 A CN 103305216A CN 2013102631314 A CN2013102631314 A CN 2013102631314A CN 201310263131 A CN201310263131 A CN 201310263131A CN 103305216 A CN103305216 A CN 103305216A
- Authority
- CN
- China
- Prior art keywords
- fluorescent powder
- red fluorescent
- compound
- preparation
- borate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 33
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 13
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 7
- 230000005284 excitation Effects 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229910052810 boron oxide Inorganic materials 0.000 claims description 6
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 6
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 5
- 235000015320 potassium carbonate Nutrition 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000003836 solid-state method Methods 0.000 claims description 2
- 150000001642 boronic acid derivatives Chemical group 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 abstract 1
- 239000002574 poison Substances 0.000 abstract 1
- 231100000614 poison Toxicity 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- -1 rare-earth ions Chemical class 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 239000002585 base Substances 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 9
- FVIGODVHAVLZOO-UHFFFAOYSA-N Dixanthogen Chemical compound CCOC(=S)SSC(=S)OCC FVIGODVHAVLZOO-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 238000013459 approach Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses borate red fluorescent powder and a preparation method and application thereof. The fluorescent powder is a borate material activated by rare-earth ions, wherein the chemical formula of the fluorescent powder is K3M1-xEUxB6O12; M is one of elements La, Gd and Y; and x is smaller than or equal to 1.0 and greater than or equal to 0.001. According to the borate red fluorescent powder prepared by a high-temperature solid-phase method, the position of a main emission peak is near 612 nanometers and coincided with an emission wavelength of a near ultraviolet semiconductor chip under excitation of near ultraviolet light. The red fluorescent powder disclosed by the invention is good in optical stability, high in red luminescent intensity, and ideal in color purity. The borate red fluorescent powder disclosed by the invention is low in cost, free of poison, free of pollution, and easy to operate and carry out industrial production.
Description
Technical field
The present invention relates to a kind ofly under near ultraviolet excitation, launch a kind of borate base fluorescent powder of red fluorescence, can apply and be packaged in outside the InGaN diode, preparation White-light LED illumination device belongs to the fluorescent material technical field.
Background technology
The plurality of advantages such as that white light LEDs (Light Emitting Diode) has is nontoxic, energy-efficient, the life-span long, shock resistance and safety are decided.Can be widely used on the various lighting installations, be a kind of environmental protection, energy-conservation green illumination light source, therefore is generally considered the new light sources that substitutes traditional lighting.
At present, realize that White-light LED illumination mainly contains 3 kinds of approach, the first approach is to be combined to form white light by red, green and blue look led chip; The second approach is to use quantum effect to realize Single chip white light; The third is to add that with the chip of sending out UV-light or blue light fluorescent material realizes white light.The third method be cost minimum, simple, simultaneously also be the most ripe method, this fluorescent material mainly is the YAG yttrium aluminum garnet, its chemical formula is Y
3Al
5O
12: Ce
3+, the white light LEDs that this fluorescent material is made has very high luminous efficiency, but owing to the few colour rendering index that makes of ruddiness comparison of ingredients in the emmission spectrum is on the low side, colour temperature is higher.This has just reduced the application of white light LEDs at low colour temperature, warm white lighting field.At present, LED mainly is Y with commercial red fluorescence powder
2O
2S:Eu
3+, this red fluorescence powder is sulfide, and the preparation method is complicated, and luminous efficiency is low.Therefore develop a kind of stable performance, low price, can have been become by the red fluorescence powder that UV-light, purple light or blue-light LED chip efficiently excite at present the focus of research both at home and abroad.
Summary of the invention
The object of the present invention is to provide that a kind of luminous efficiency is high, stable chemical nature, and the simple borate base red fluorescent powder of preparation method, preparation method and application thereof.
The present invention is achieved through the following technical solutions: a kind of borate base red fluorescent powder is provided, and its chemical formula is K
3M
1-xEu
xB
6O
12, wherein, the M element is a kind of among La, Gd, the Y,
xBe Eu
3+The molecular fraction of mixing, 0.001≤
x≤ 1.0; Described fluorescent material is launched the red fluorescence that wavelength is 590～720 nanometers under near ultraviolet excitation.
Borate base red fluorescent powder of the present invention, its preparation method comprises the steps: for adopting high temperature solid-state method
1, with contain the K element compound, contain the compound of M element, contain the Eu element compound, contain the B element compound be raw material, press chemical formula K
3M
1-xEu
xB
6O
12The stoichiometric ratio of middle corresponding element takes by weighing each raw material, and in the formula, the M element is a kind of among La, Gd, the Y, 0.001≤
x≤ 1.0; Mix after grinding respectively, obtain mixing raw material;
2, with the presintering 1～2 time in air of the mixing raw material that obtains, sintering temperature is 300～650 ℃, and sintering time is 2～10 hours;
3, the product after the presintering is ground and mixes, calcine in air atmosphere, calcining temperature is 700～1200 ℃, and calcination time is 2～18 hours, obtains a kind of borate base red fluorescent powder.
The compound of the K of containing element of the present invention is a kind of in potassium hydroxide, salt of wormwood, the saltpetre; The compound that contains the M element is a kind of in oxide compound, the nitric acid thing, and the M element is a kind of among La, Gd, the Y; The compound that contains the Eu element is a kind of in europium sesquioxide, the europium nitrate; The compound that contains the B element is a kind of in boron oxide, the boric acid.
A kind of preferred version of above-mentioned preparation method is: the described sintering temperature of step 2 is 350～600 ℃, and sintering time is 3～8 hours; The described calcining temperature of step 3 is 750～1100 ℃, and calcination time is 3～15 hours.
A kind of borate base red fluorescent powder provided by the invention can cooperate an amount of blueness and green emitting phosphor, applies and is packaged in outside the diode, for the preparation of the White-light LED illumination device.
Compared with prior art, the advantage of technical solution of the present invention is:
1, Eu provided by the invention
3+The borate base red fluorescent powder that activates sends the ruddiness that main peak is 612 nanometers under the exciting of 350～400 nanometer light, red degree is pure, cooperates with green emitting phosphor, is coated on the blue-light LED chip to prepare novel white light LEDs.
2, can cooperate with ultraviolet or near ultraviolet LED chip, prepare white light LEDs as red fluorescence powder; Also can cooperate with blue light, purple light, ultraviolet leds, or mix the fluorescent material of other type, the preparation multi-color LED.
3, the borate base red fluorescent powder of the present invention's preparation is compared with other sulfide, halogenide, and its base starting material source is abundant, cheap, and preparation technology is simple, and is without the waste water and gas discharging, environmentally friendly.Have good thermostability, color developing and granularity are conducive to realize the high-power LED of preparation.
Description of drawings
Fig. 1 is the embodiment of the invention 1 prepared K
3Y
0.95Eu
0.05B
6O
12The X-ray powder diffraction collection of illustrative plates of material sample;
Fig. 2 is the embodiment of the invention 1 prepared K
3Y
0.95Eu
0.05B
6O
12The exciting light spectrogram of material sample under monitoring wavelength 612 nanometers;
Fig. 3 is the embodiment of the invention 1 prepared K
3Y
0.95Eu
0.05B
6O
12The luminescent spectrum figure of material sample under 396 nano wave lengths excite;
Fig. 4 is the embodiment of the invention 5 prepared K
3La
0.75Eu
0.25B
6O
12The exciting light spectrogram of material sample under monitoring wavelength 612 nanometers;
Fig. 5 is the embodiment of the invention 5 prepared K
3La
0.75Eu
0.25B
6O
12The luminescent spectrum figure of material sample under 396 nano wave lengths excite.
Embodiment
Technical solution of the present invention is further elaborated below in conjunction with drawings and Examples.
Embodiment 1:
Preparation K
3Y
0.95Eu
0.05B
6O
12
According to chemical formula K
3Y
0.95Eu
0.05B
6O
12, take by weighing respectively: salt of wormwood K
2CO
3: 1.38191 grams, yttrium oxide Y
2O
3: 0.7151 gram, europium sesquioxide Eu
2O
3: 0.0587 gram, boric acid H
3BO
3: 2.4732 grams, after in agate mortar, grinding and mixing, in air atmosphere, carry out presintering, pre-sintering temperature is 500 ℃, sintering time 7 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 750 ℃, and calcination time is 15 hours, namely obtains powder shaped boric acid alkali red illuminating material.
Referring to accompanying drawing 1, it is the X-ray powder diffraction collection of illustrative plates for preparing sample by the present embodiment technical scheme, and the XRD test result shows, prepared borate K
3Y
0.95Eu
0.05B
6O
12Be monophase materials, without any other impurity phase existence, and degree of crystallinity is better.
Referring to accompanying drawing 2, it is the lower exciting light spectrogram that obtains of the prepared sample 612 nanometers monitoring of the present embodiment; As can be seen from the figure, the emitting red light of this material excite the source mainly near ultraviolet 396 nanometers, can mate well the White-light LED chip of near ultraviolet excitation.
Referring to accompanying drawing 3, it is that the prepared sample of the present embodiment excites the lower luminescent spectrum figure that obtains at 396 nano wave lengths; The main luminescence center of this material is at the emitting red light wave band of 612 nanometers.
Embodiment 2:
Preparation K
3Gd
0.9Eu
0.1B
6O
12
According to chemical formula K
3Gd
0.9Eu
0.1B
6O
12, take by weighing respectively: saltpetre KNO
3: 2.022 grams, gadolinium sesquioxide Gd
2O
3: 1.0875 grams, europium nitrate Eu (NO
3)
3-6H
2The O:0.1487 gram, boron oxide B
2O
3: 1.3924 grams, after in agate mortar, grinding and mixing, select air atmosphere to carry out presintering, pre-sintering temperature is 350 ℃, sintering time 8 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 900 ℃, and calcination time is 12 hours, namely obtains the powder shaped borate red luminescent material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 3:
Preparation K
3La
0.999Eu
0.001B
6O
12
According to chemical formula K
3La
0.999Eu
0.001B
6O
12, take by weighing respectively potassium hydroxide KOH:1.122 gram, lanthanum trioxide La
2O
3: 1.0849 grams, europium nitrate Eu (NO
3)
3-6H
2The O:0.0015 gram, boron oxide B
2O
3: 1.3924 grams, after in agate mortar, grinding and mixing, select air atmosphere to carry out presintering, pre-sintering temperature is 600 ℃, then sintering time 3 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 850 ℃, and calcination time is 16 hours, namely obtains the powder shaped borate red luminescent material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 4:
Preparation K
3Gd
0.8Eu
0.2B
6O
12
According to chemical formula K
3Gd
0.8Eu
0.2B
6O
12, take by weighing respectively: salt of wormwood K
2CO
3: 1.3819 grams, Gadolinium trinitrate Gd (NO
3)
3-6H
2The O:2.407 gram, europium nitrate Eu (NO
3)
3-6H
2The O:1.7842 gram, boron oxide B
2O
3: 1.3924 grams, after in agate mortar, grinding and mixing, select air atmosphere to carry out presintering, pre-sintering temperature is 400 ℃, then sintering time 8 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 950 ℃, and calcination time is 10 hours, namely obtains the powder shaped borate red luminescent material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 5:
Preparation K
3La
0.75Eu
0.25B
6O
12
According to chemical formula K
3La
0.75Eu
0.25B
6O
12, take by weighing respectively: saltpetre KNO
3: 2.022 grams, lanthanum nitrate La (NO
3)
3-6H
2The O:2.165 gram, europium nitrate Eu (NO
3)
3-6H
2The O:0.7434 gram, boric acid H
3BO
3: 2.4732 grams, after in agate mortar, grinding and mixing, select air atmosphere to carry out presintering, pre-sintering temperature is 450 ℃, sintering time 7 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 1000 ℃, and calcination time is 15 hours, namely obtains the powder shaped borate red luminescent material.
Referring to accompanying drawing 4, it is the lower exciting light spectrogram that obtains of the prepared sample 612 nanometers monitoring of the present embodiment; As can be seen from the figure, the emitting red light of this material excite the source mainly near ultraviolet 396 nanometers, can mate well the White-light LED chip of near ultraviolet excitation.
Referring to accompanying drawing 5, it is that the prepared sample of the present embodiment excites the lower luminescent spectrum figure that obtains at 396 nano wave lengths; The main luminescence center of this material is at the emitting red light wave band of 612 nanometers.
Embodiment 6:
Preparation K
3Y
0.6Eu
0.4B
6O
12
According to chemical formula Na
2Y
0.6Eu
0.4PO
4F
2, take by weighing respectively salt of wormwood K
2CO
3: 1.3819 grams, yttrium oxide Y
2O
3: 0.4517 gram, europium sesquioxide Eu
2O
3: 0.4692 gram, boron oxide B
2O
3: 1.3924 grams, after in agate mortar, grinding and mixing, select air atmosphere to carry out presintering, pre-sintering temperature is 500 ℃, sintering time 5 hours is cooled to room temperature, takes out sample; It fully is placed in the retort furnace after the grinding again, calcines under air atmosphere, calcining temperature is 1100 ℃, and calcination time is 13 hours, namely obtains the powder shaped borate red luminescent material.Its main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Claims (6)
1. borate base red fluorescent powder, it is characterized in that: its chemical formula is K
3M
1-xEu
xB
6O
12, wherein, the M element is a kind of among La, Gd, the Y,
xBe Eu
3+The molecular fraction of mixing, 0.001≤
x≤ 1.0; Described fluorescent material is launched the red fluorescence that wavelength is 590～720 nanometers under near ultraviolet excitation.
2. the preparation method of borate base red fluorescent powder as claimed in claim 1 is characterized in that adopting high temperature solid-state method, comprises the steps:
(1) with contain the K element compound, contain the compound of M element, contain the Eu element compound, contain the B element compound be raw material, press chemical formula K
3M
1-xEu
xB
6O
12The stoichiometric ratio of middle corresponding element takes by weighing each raw material, and in the formula, the M element is a kind of among La, Gd, the Y, 0.001≤
x≤ 1.0; Mix after grinding respectively, obtain mixing raw material;
(2) with the presintering 1～2 time in air of the mixing raw material that obtains, sintering temperature is 300～650 ℃, and sintering time is 2～10 hours;
(3) product after the presintering is ground and mixes, calcine in air atmosphere, calcining temperature is 700～1200 ℃, and calcination time is 2～18 hours, obtains a kind of borate base red fluorescent powder.
3. the preparation method of a kind of borate base red fluorescent powder according to claim 2 is characterized in that: the compound of the described K of containing element is a kind of in potassium hydroxide, salt of wormwood, the saltpetre; The compound that contains the M element is a kind of in oxide compound, the nitric acid thing, and the M element is a kind of among La, Gd, the Y; The compound that contains the Eu element is a kind of in europium sesquioxide, the europium nitrate; The compound that contains the B element is a kind of in boron oxide, the boric acid.
4. the preparation method of a kind of borate base red fluorescent powder according to claim 2, it is characterized in that: the described sintering temperature of step (2) is 350～600 ℃, and sintering time is 3～8 hours.
5. the preparation method of a kind of borate base red fluorescent powder according to claim 2, it is characterized in that: the described calcining temperature of step (3) is 750～1100 ℃, and calcination time is 3～15 hours.
6. by the application of a kind of borate base red fluorescent powder claimed in claim 1, it is characterized in that: cooperate an amount of blueness and green emitting phosphor, apply and be packaged in outside the diode, for the preparation of the White-light LED illumination device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310263131.4A CN103305216B (en) | 2013-06-27 | 2013-06-27 | Borate red fluorescent powder and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310263131.4A CN103305216B (en) | 2013-06-27 | 2013-06-27 | Borate red fluorescent powder and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103305216A true CN103305216A (en) | 2013-09-18 |
| CN103305216B CN103305216B (en) | 2015-01-28 |
Family
ID=49130942
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310263131.4A Expired - Fee Related CN103305216B (en) | 2013-06-27 | 2013-06-27 | Borate red fluorescent powder and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103305216B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885836A (en) * | 2014-12-17 | 2016-08-24 | 温州大学 | Multi-wavelength emission Eu3+ uni-doped borate luminescent material and preparing method thereof |
| CN106544029A (en) * | 2016-11-05 | 2017-03-29 | 桂林理工大学 | fluorine-containing phosphate red fluorescent powder and preparation method thereof |
| CN107858146A (en) * | 2017-09-30 | 2018-03-30 | 西安建筑科技大学 | A kind of Eu3+Ion doping borate（K6Ba4B8O19）The synthetic method of base red fluorescent powder |
| WO2018098690A1 (en) * | 2016-11-30 | 2018-06-07 | 深圳市耀铭豪智能科技有限公司 | Led illuminating device and preparation method therefor |
| CN108822836A (en) * | 2018-06-08 | 2018-11-16 | 南通纺织丝绸产业技术研究院 | A kind of Eu2+And Eu3+The fluorescent powder of europium ion mixing activation, preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004123764A (en) * | 2002-08-07 | 2004-04-22 | Nec Lighting Ltd | Red light-emitting phosphor and light-emitting element using the same |
-
2013
- 2013-06-27 CN CN201310263131.4A patent/CN103305216B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004123764A (en) * | 2002-08-07 | 2004-04-22 | Nec Lighting Ltd | Red light-emitting phosphor and light-emitting element using the same |
Non-Patent Citations (2)
| Title |
|---|
| SANGEN ZHAO, ET AL.: "K3YB6O12: A new nonlinear optical crystal with a short UV cutoff edge", 《MATERIALS RESEARCH BULLETIN》 * |
| 张鲁宁等: "Na3La9B8O27:Ln3+(Ln=Eu或Tb)荧光体的制备与发光性能", 《华东交通大学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885836A (en) * | 2014-12-17 | 2016-08-24 | 温州大学 | Multi-wavelength emission Eu3+ uni-doped borate luminescent material and preparing method thereof |
| CN106544029A (en) * | 2016-11-05 | 2017-03-29 | 桂林理工大学 | fluorine-containing phosphate red fluorescent powder and preparation method thereof |
| WO2018098690A1 (en) * | 2016-11-30 | 2018-06-07 | 深圳市耀铭豪智能科技有限公司 | Led illuminating device and preparation method therefor |
| KR20190032490A (en) | 2016-11-30 | 2019-03-27 | 선전 와이엠에이치 인텔리전트 테크놀러지 컴퍼니 리미티드 | Led illuminating device and preparation method therefor |
| US10920135B2 (en) | 2016-11-30 | 2021-02-16 | Shenzhen Ymh Intelligent Technology Co., Ltd. | Preparation method of an LED illuminating device |
| CN107858146A (en) * | 2017-09-30 | 2018-03-30 | 西安建筑科技大学 | A kind of Eu3+Ion doping borate（K6Ba4B8O19）The synthetic method of base red fluorescent powder |
| CN108822836A (en) * | 2018-06-08 | 2018-11-16 | 南通纺织丝绸产业技术研究院 | A kind of Eu2+And Eu3+The fluorescent powder of europium ion mixing activation, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103305216B (en) | 2015-01-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101475802B (en) | Multiple antimonate luminescent materials for white light LED and preparation thereof | |
| CN102250616B (en) | Double-perovskite structured red fluorescent powder as well as preparation method and application thereof | |
| CN101921589A (en) | Niobate or tantalite fluorescent material used for white light LED and preparation method thereof | |
| CN103627392B (en) | A kind of stibnate base red fluorescent powder and its preparation method and application | |
| CN102533266A (en) | Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder | |
| CN103205253A (en) | Columbate or tantalate fluorescence material used in white-light LED, and its preparation method | |
| CN103305216B (en) | Borate red fluorescent powder and preparation method and application thereof | |
| CN103242830B (en) | Fluorosilicate-based blue-green fluorescent powder as well as preparation method and applications of fluorescent powder | |
| CN102585831B (en) | Europium-ion-excited fluoromolybdate red fluorescent powder and preparation method and application thereof | |
| CN102585819B (en) | Lanthanum boron tungstate red fluorescent powder and preparation method thereof | |
| CN102492425A (en) | Aluminate red phosphor, preparation method and application | |
| CN103305221A (en) | Eu<3+>-doped vanadate fluorescent material, and preparation method and application thereof | |
| CN103031125A (en) | Niobate or tantalite fluorescent material for white LED (Light-Emitting Diode), and preparation method of niobate or tantalite fluorescent material | |
| CN103059849B (en) | Silicophosphate green fluorescent powder activated by Eu<2+> and preparation method as well as application thereof | |
| CN103289698B (en) | A kind of europium ion Eu 3+the phosphate base red fluorescence powder activated, preparation method and application | |
| CN103396800B (en) | Boron aluminate-based blue fluorescent powder, preparation method and application | |
| CN103275713A (en) | Rare earth molybdate red phosphor, and preparation method and application thereof | |
| CN102942928B (en) | Zirconate-base red phosphor, method for preparing same and application | |
| CN102604633A (en) | Tetratungstate red phosphor powder and preparation method thereof | |
| CN102925150B (en) | Tungstate fluorescent powder as well as preparation method and application thereof | |
| CN102373062B (en) | Fluosilicate red fluorescent powder suitable for white-light LED (Light-Emitting Diode) and preparation method thereof | |
| CN103320131B (en) | Phosphate based red phosphor, preparation method and application thereof | |
| CN105062472B (en) | A kind of preparation method and application of the blue colour fluorescent powder for warm white LED | |
| CN103992795B (en) | A kind of LED red fluorescence powder and preparation method thereof | |
| CN102433118A (en) | Niobate red fluorescent powder, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171221 Address after: 511430 1402 room 1402, No. 383 office building, North 383 Panyu Avenue, Panyu District South Village, Panyu District, Guangdong Patentee after: Guangzhou Intellectual Property Service Co., Ltd. Address before: 215123 Suzhou City, Suzhou Province Industrial Park, No. love road, No. 199 Patentee before: Soochow University |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20181120 Address after: 401120 3rd floor, Building 11, Jingkai District, Guanyan Village, Lianglu Road, Yubei District, Chongqing Patentee after: CHONGQING GOLUTE NEW MATERIAL TECHNOLOGY CO., LTD. Address before: 511430 1402 office building, 383 office building, Panyu Avenue North, Panyu District Town, Guangzhou, Guangdong, Panyu, China Patentee before: Guangzhou Intellectual Property Service Co., Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200429 Address after: 236000 south side of Pao Road, industrial park, Yingshang County, Fuyang, Anhui Patentee after: ANHUI RONGZE TECHNOLOGY Co.,Ltd. Address before: 401120, Chongqing, Yubei District two road view of the village through the Camp Camp No. 11, building 3 Patentee before: CHONGQING GOLUTE NEW MATERIAL TECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150128 Termination date: 20200627 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |