CN103013505A - Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes) - Google Patents

Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes) Download PDF

Info

Publication number
CN103013505A
CN103013505A CN2012105452913A CN201210545291A CN103013505A CN 103013505 A CN103013505 A CN 103013505A CN 2012105452913 A CN2012105452913 A CN 2012105452913A CN 201210545291 A CN201210545291 A CN 201210545291A CN 103013505 A CN103013505 A CN 103013505A
Authority
CN
China
Prior art keywords
solution
preparation
fluorescent material
white light
light leds
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
Application number
CN2012105452913A
Other languages
Chinese (zh)
Other versions
CN103013505B (en
Inventor
宁青菊
郭芳芳
乔畅君
李向龙
史永胜
于成龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201210545291.3A priority Critical patent/CN103013505B/en
Publication of CN103013505A publication Critical patent/CN103013505A/en
Application granted granted Critical
Publication of CN103013505B publication Critical patent/CN103013505B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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)
  • Silicon Compounds (AREA)

Abstract

The invention provides a preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes), which comprises the following steps: after completely dissolving Tb4O7 in a concentrated nitric acid solution, regulating the pH value to 4-7 with ammonia water, sequentially adding anhydrous CaCl2, Ca(NO3)2.4H2O and anhydrous ethanol, uniformly stirring, adding a slow release agent citric acid solution, continuously stirring until the slow release agent is uniformly dispersed in the solution, adding ethyl silicate, and stirring to form a uniform and transparent solution; and regulating the pH value of the uniform and transparent solution to 6-8 with ammonia water to form a gel, drying the gel, grinding to form powder, putting the dry gel powder in a resistance furnace, and sintering in a weak reducing atmosphere. The preparation method provided by the invention implements activation of the Ca2SiO3Cl2 substrate to emit white light by using the single Tb<3+>.

Description

The white light LEDs preparation method of single-matrix fluorescent material
Technical field
The present invention relates to a kind of white light LEDs with the preparation method of single-matrix fluorescent material, be specifically related to the preparation method that a kind of white light LEDs is used single-matrix fluorescent material.
Background technology
White light LEDs is once extensive concern occurring just being subject to, have the characteristics such as environmental protection, energy-conservation, efficient, life-span length, easy care as the illumination of light source, be called as and surmount incandescent light, luminescent lamp and high-voltage gas discharging light (High intensity dis-charge, HID) the 4th generation lighting source, be the first-selection of pursuing the society of low-carbon economy.
The realization of white light LEDs mainly is to adopt a led chip and phosphor combination, and the short wavelength's who chip is sent by fluorescent material light partly or entirely converts visible light to, is combined at last white light.What current research was maximum and the most ripe is blue led/yellow fluorescence powder system, but the luminous efficiency of this fluorescent material is lower, and the photoelectric transformation efficiency of ultraviolet conversion hysteria fluorescent material system is lower, therefore studies near ultraviolet conversion hysteria fluorescent material tool and is of great significance.
Near ultraviolet conversion hysteria fluorescent material can be divided into single-matrix white fluorescent powder and multiple matrix white fluorescent powder.The direct transmitting white of single-matrix white fluorescent powder energy under the exciting of near-ultraviolet light wherein, compare with other system fluorescent material, its outstanding feature is arranged: (1) is owing to the insensitivity of vision to near-ultraviolet light, the color of this class white light LEDs is determined by fluorescence, so colour stable, color reducibility is higher; (2) owing to being the single-matrix compound, can reduce energy waste, be conducive to improve luminous efficiency; (3) can avoid because the color imbalance that multiple matrix compounds interphase interaction causes is conducive to improve color developing; (4) cost.Therefore single-matrix white fluorescent powder more and more receives people's concern recent years, becomes the study hotspot of White-light LED illumination of new generation, and the research of relevant this system material also gradually deeply.
In recent years, the research of relevant single-matrix white fluorescent powder, existing lot of documents report, the matrix compounds scope that relates to is very wide, comprises silicate, phosphoric acid salt, borate, vanadate, aluminate etc.Wherein the compound alkaline earth halogen silicate of alkaline-earth silicate and alkali-earth halide has lower synthesis temperature, stable physical and chemical performance, thereby obtains broad research.Alkaline earth chloride silicate is a kind of substrate material of luminescent properties excellence.Active ions are except common Eu 2+And Ce 3+Outward, Mn 2+, Eu 3+, Dy 3+, Tb 3+Deng the active ions that also often are used as in the single-matrix white fluorescence system.Wherein modal is two kinds of ion co-doped single-matrix white fluorescent powders, such as Eu 2+-Mn 2+, Ce 3+-Mn 2+Deng, single excited ion is difficult to realize white light emission.
Summary of the invention
Technical problem to be solved by this invention provides a kind of white light LEDs with the preparation method of single-matrix fluorescent material, has realized Tb 3+Single excitation-emission white light.
For achieving the above object, the invention provides the preparation method that a kind of white light LEDs is used single-matrix fluorescent material, its chemical constitution formula is Ca 2SiO 3Cl 2: xTb 3+, wherein the span of x is 0.001～0.004, at first with Tb 4O 7Be dissolved in the salpeter solution to Tb 4O 7After the dissolving, regulating the pH value is 4～7, then adds successively anhydrous CaCl fully 2, Ca (NO 3) 24H 2O and dehydrated alcohol after stirring, add the sustained release dosage citric acid solution again and constantly stir and make sustained release dosage Uniform Dispersion in solution, add at last tetraethyl silicate, stir and form homogeneous transparent solution; The pH value of regulating homogeneous transparent solution is 6～8, until form gel, will grind to form powder behind the gel drying, and the powder with xerogel places resistance furnace to get final product in the weakly reducing atmosphere sintering at last.
As the preferred embodiments of the present invention, described Tb 4O 7Under 75～98 ℃ condition, constantly to stir and consoluet;
As the preferred embodiments of the present invention, described dissolving Tb 4O 7The nitric acid weight concentration be 50～58%;
As the preferred embodiments of the present invention, the concentration of described citric acid is 0.3mol/L, and add-on is 0.5～1.5ml;
As the preferred embodiments of the present invention, the add-on of described tetraethoxy is 4.48ml;
As the preferred embodiments of the present invention, form in the process of gel at clear solution, be that the pH value that the ammoniacal liquor of 0.1mol/L is regulated homogeneous transparent solution is 6～8 with concentration, the formation gel;
As the preferred embodiments of the present invention, in the weakly reducing atmosphere of sintering be: the powder of xerogel is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite are housed, the ratio of described carbon dust and graphite is 1:1;
As the preferred embodiments of the present invention, described sintering schedule is: be heated to 320 ℃ with 6 ℃/min speed, insulation 5～8h; Be warming up to 550～600 ℃ with 15 ℃/min again, insulation 5～10h, last furnace cooling.
The Ca that the present invention adopts wet chemistry method to prepare 2SiO 3Cl 2: xTb 3+Fluorescent material, crystalline phase purity is high, and particle diameter is even, is of a size of 1～3 μ m, this fluorescent material is with 365～375nm optical excitation, 8 spike emission peaks can occur at visible light part, present white light emission after the mixing, chromaticity coordinates is (0.3174,0.3485), very approaching with standard white light (0.33,0.33), and colour temperature Tc=6161K is positioned at positive white light reference color temperature.The Ca that the method is prepared 2SiO 3Cl 2: xTb 3+Fluorescent material is a kind of very potential white light LEDs single-matrix fluorescent material.
Description of drawings
Fig. 1 is embodiment of the invention 2Ca 2SiO 3Cl 2: 0.002Tb 3+Scanning electron microscope (SEM) photograph;
Fig. 2 is embodiment of the invention 3Ca 2SiO 3Cl 2: 0.003Tb 3+The utilizing emitted light spectrogram;
Fig. 3 is embodiment of the invention 4Ca 2SiO 3Cl 2: 0.003Tb 3+Chromaticity coordinates figure.
Embodiment
For achieving the above object, the invention provides a kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula is Ca 2SiO 3Cl 2: xTb 3+, wherein the span of x is 0.001～0.004.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is that 0.00002～0.00008mol takes by weighing Tb 4O 7, measure respectively 5～8ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 75～98 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=4～7, till white insolubles will occurring, adds at last distilled water 2～4ml, forms solution A.In solution A, add anhydrous CaCl 2, add again Ca (NO after the dissolving 3) 24H 2O, citric acid sustained release dosage solution 0.5ml～1.5ml that the dehydrated alcohol that adds at last and concentration are 0.3mol/L stirs 3～5min, forms solution B.In solution B, add TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=6 of regulator solution～8, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 4～7h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 5～8h; Be warming up to 550～600 ℃ with 15 ℃/min again, insulation 5～10h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
Below in conjunction with specific embodiment the inventive method is further elaborated:
Embodiment 1:
A kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula are Ca 2SiO 3Cl 2: xTb 3+, wherein the value of x is 0.001.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is that 0.00002mol takes by weighing Tb 4O 7, measure respectively 5ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 75 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=4, and till white insolubles will occurring, adding at last distilled water is 2～4ml, forms solution A.In solution A, add anhydrous CaCl 2, add again Ca (NO after the dissolving 3) 24H 2O adds the dehydrated alcohol of 5～8ml and the citric acid sustained release dosage solution 0.5ml that concentration is 0.3mol/L at last, stirs 3～5min, forms solution B.In solution B, add ml TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=6 of regulator solution, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 4h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 8h; Be warming up to 550 ℃ with 15 ℃/min again, insulation 10h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
Embodiment 2
A kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula are Ca 2SiO 3Cl 2: xTb 3+, wherein the value of x is 0.002.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is that 0.00004mol takes by weighing Tb 4O 7, measure respectively 6ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 85 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=5, and till white insolubles will occurring, adding at last distilled water is 2～4ml, forms solution A.In solution A, add anhydrous 0.02mol CaCl 2, add again 0.02mol Ca (NO after the dissolving 3) 24H 2O adds the dehydrated alcohol of 5～8ml and the citric acid sustained release dosage solution 1.0ml that concentration is 0.3mol/L at last, stirs 3～5min, forms solution B.In solution B, add 4.48ml TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=6 of regulator solution, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 4h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 7h; Be warming up to 600 ℃ with 15 ℃/min again, insulation 7h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
Embodiment 3
A kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula are Ca 2SiO 3Cl 2: xTb 3+, wherein the value of x is 0.003.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is that 0.00006mol takes by weighing Tb 4O 7, measure respectively 6ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 90 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=5, and till white insolubles will occurring, adding at last distilled water is 2～4ml, forms solution A.In solution A, add anhydrous 0.02molCaCl 2, add again 0.02mol Ca (NO after the dissolving 3) 24H 2O adds the dehydrated alcohol of 5～8ml and the citric acid sustained release dosage solution 1.5ml that concentration is 0.3mol/L at last, stirs 3～5min, forms solution B.In solution B, add 4.48ml TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=7 of regulator solution, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 5h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 7h; Be warming up to 600 ℃ with 15 ℃/min again, insulation 7h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
Embodiment 4
A kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula are Ca 2SiO 3Cl 2: xTb 3+, wherein the value of x is 0.003.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is the Tb that 0.00006mol takes by weighing 4O 7, measure respectively 8ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 98 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=7, and till white insolubles will occurring, adding at last distilled water is 2～4ml, forms solution A.In solution A, add anhydrous 0.02mol CaCl 2, add again 0.02mol Ca (NO after the dissolving 3) 24H 2O adds the dehydrated alcohol of 5～8ml and the citric acid sustained release dosage solution 1.5ml that concentration is 0.3mol/L at last, stirs 3～5min, forms solution B.In solution B, add 4.48ml TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=7 of regulator solution, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 6h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 6h; Be warming up to 620 ℃ with 15 ℃/min again, insulation 6h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
Embodiment 5
A kind of alkaline earth chloride silicate-based white fluorescent powder for white LED, its chemical constitution formula are Ca 2SiO 3Cl 2: xTb 3+, wherein the span of x is 0.004.
1) according to stoichiometric ratio, calculates the Ca of synthetic 0.02mol 2SiO 3Cl 2: xTb 3+The quality of required medicine: the anhydrous CaCl of weighing 0.02mol 2, 0.02mol Ca (NO 3) 24H 2The molar weight that O reaches according to Tb is the Tb that takes by weighing of 0.00008mol 4O 7, measure respectively 8ml dehydrated alcohol, 4.48ml tetraethyl silicate (TEOS).With Tb 4O 7Be dissolved in an amount of weight concentration and be in 50～58% the concentrated nitric acid solution, be heated to 90 ℃, until Tb 4O 7Powder dissolves fully, and the amount of nitric acid is with dissolving Tb 4O 7Powder is advisable, and then is first rare NH of 0.1mol/L with concentration 3H 2O regulator solution pH value is to pH=7, and till white insolubles will occurring, adding at last distilled water is 2～4ml, forms solution A.In solution A, add anhydrous 0.02mol CaCl 2, add again 0.02mol Ca (NO after the dissolving 3) 24H 2O adds the dehydrated alcohol of 5～8ml and the citric acid sustained release dosage solution 1.0ml that concentration is 0.3mol/L at last, stirs 3～5min, forms solution B.In solution B, add 4.48ml TEOS, rapid stirring 5～10min, the solution C of formation homogeneous transparent.
2) the above-mentioned homogeneous phase solution C that is made into is stirred at ambient temperature, and drip rare NH of 0.1mol/L 3H 2O, the pH=8 of regulator solution, rapid stirring is until form gel.The gel of gained is placed 120 ℃ of constant temperature, and oven dry 7h obtains xerogel, with mortar xerogel is ground to form powder.
3) the xerogel powder that grinds is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite (its ratio is 1:1) are housed, put it at last in the chamber type electric resistance furnace, be heated to 320 ℃ with 6 ℃/min speed, insulation 5h; Be warming up to 620 ℃ with 15 ℃/min again, insulation 5h furnace cooling obtains Ca 2SiO 3Cl 2: xTb 3+Fluorescent material.
The present invention adopts wet chemistry method to prepare the presoma of sample, and take citric acid as sustained release dosage, slows down gelation process, reduces crystalline size.The Ca for preparing 2SiO 3Cl 2: xTb 3+Fluorescent material, crystalline phase purity is high, particle diameter is 1～3 μ m, and particle diameter is even, with 365～375nm optical excitation, 8 spike emission peaks can appear at visible light part, present white light emission after the mixing, chromaticity coordinates is (0.3174,0.3485) and standard white light (0.33,0.33) very approaching, and colour temperature Tc=6161K is positioned at positive white light reference color temperature.The Ca that the method is prepared 2SiO 3Cl 2: xTb 3+Fluorescent material is a kind of very potential white light LEDs single-matrix fluorescent material.

Claims (8)

1. a white light LEDs is with the preparation method of single-matrix fluorescent material, and it is characterized in that: its chemical constitution formula is Ca 2SiO 3Cl 2: xTb 3+, wherein the span of x is 0.001～0.004, at first with Tb 4O 7Be dissolved in the salpeter solution to Tb 4O 7After the dissolving, regulating the pH value is 4～7, then adds successively anhydrous CaCl fully 2, Ca (NO 3) 24H 2O and dehydrated alcohol after stirring, add the sustained release dosage citric acid solution again and constantly stir and make sustained release dosage Uniform Dispersion in solution, add at last tetraethyl silicate, stir and form homogeneous transparent solution; The pH value of regulating homogeneous transparent solution is 6～8, until form gel, will grind to form powder behind the gel drying, and the powder with xerogel places resistance furnace to get final product in the weakly reducing atmosphere sintering at last.
2. a kind of white light LEDs as claimed in claim 1 is characterized in that: described Tb with the preparation method of single-matrix fluorescent material 4O 7Under 75～98 ℃ condition, constantly to stir and consoluet.
3. a kind of white light LEDs as claimed in claim 1 or 2 is characterized in that: described dissolving Tb with the preparation method of single-matrix fluorescent material 4O 7The nitric acid weight concentration be 50～58%.
4. a kind of white light LEDs as claimed in claim 1 is with the preparation method of single-matrix fluorescent material, and it is characterized in that: the concentration of described citric acid is 0.3mol/L, and add-on is 0.5～1.5ml.
5. a kind of white light LEDs as claimed in claim 1 is with the preparation method of single-matrix fluorescent material, and it is characterized in that: the add-on of described tetraethoxy is 4.48ml.
6. a kind of white light LEDs as claimed in claim 1 is characterized in that with the preparation method of single-matrix fluorescent material: forming in the process of gel at clear solution, is that the pH value that the ammoniacal liquor of 0.1mol/L is regulated homogeneous transparent solution is 6～8 with concentration, the formation gel.
7. a kind of white light LEDs as claimed in claim 1 is with the preparation method of single-matrix fluorescent material, it is characterized in that: in the weakly reducing atmosphere of sintering be: the powder of xerogel is placed alumina crucible, then crucible is put into zirconium white tank and sealing that carbon dust and graphite are housed, the ratio of described carbon dust and graphite is 1:1.
8. such as the preparation method of claim 1 or 7 described a kind of white light LEDs usefulness single-matrix fluorescent material, it is characterized in that: described sintering schedule is: be heated to 320 ℃ with 6 ℃/min speed, insulation 5～8h; Be warming up to 550～600 ℃ with 15 ℃/min again, insulation 5～10h, last furnace cooling.
CN201210545291.3A 2012-12-14 2012-12-14 Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes) Expired - Fee Related CN103013505B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210545291.3A CN103013505B (en) 2012-12-14 2012-12-14 Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210545291.3A CN103013505B (en) 2012-12-14 2012-12-14 Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes)

Publications (2)

Publication Number Publication Date
CN103013505A true CN103013505A (en) 2013-04-03
CN103013505B CN103013505B (en) 2014-04-16

Family

ID=47962628

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210545291.3A Expired - Fee Related CN103013505B (en) 2012-12-14 2012-12-14 Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes)

Country Status (1)

Country Link
CN (1) CN103013505B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923646A (en) * 2014-04-10 2014-07-16 上海应用技术学院 Yellow fluorescent powder and preparation method thereof
CN107936960A (en) * 2017-12-06 2018-04-20 河北工业大学 A kind of Tb3+Adulterate the preparation method of calcium silicate luminescent material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040159846A1 (en) * 2003-02-18 2004-08-19 Doxsee Daniel Darcy White light LED device
CN101892049A (en) * 2010-07-30 2010-11-24 陕西科技大学 Single matrix white light fluorescent powder for white light LED and preparation method thereof
CN101892054A (en) * 2010-07-30 2010-11-24 陕西科技大学 White emitting fluorescent powder for LED and preparation method thereof
CN101892048A (en) * 2010-07-30 2010-11-24 陕西科技大学 Alkaline earth chloride silicate-based white fluorescent powder for white LED and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040159846A1 (en) * 2003-02-18 2004-08-19 Doxsee Daniel Darcy White light LED device
CN101892049A (en) * 2010-07-30 2010-11-24 陕西科技大学 Single matrix white light fluorescent powder for white light LED and preparation method thereof
CN101892054A (en) * 2010-07-30 2010-11-24 陕西科技大学 White emitting fluorescent powder for LED and preparation method thereof
CN101892048A (en) * 2010-07-30 2010-11-24 陕西科技大学 Alkaline earth chloride silicate-based white fluorescent powder for white LED and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
宁青菊: "Ca2SiO3Cl2:Dy3+单一基质白光荧光粉的制备及发光特性", 《功能材料》 *
杨志平，等: "用于白光LED的单一基质白光荧光粉Ca2SiO3Cl2:Eu2+,Mn2+的发光性质", 《物理学报》 *
杨志平，等: "用于白光LED的高亮度蓝白色荧光粉Ca2SiO3Cl2:Eu2+的发光性质", 《发光学报》 *
陈茜等: "Sr2MgSi2O7:Tb3+,Li+荧光粉的合成和发光机理", 《无机化学学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923646A (en) * 2014-04-10 2014-07-16 上海应用技术学院 Yellow fluorescent powder and preparation method thereof
CN103923646B (en) * 2014-04-10 2015-06-10 上海应用技术学院 Yellow fluorescent powder and preparation method thereof
CN107936960A (en) * 2017-12-06 2018-04-20 河北工业大学 A kind of Tb3+Adulterate the preparation method of calcium silicate luminescent material

Also Published As

Publication number Publication date
CN103013505B (en) 2014-04-16

Similar Documents

Publication Publication Date Title
CN101962542B (en) Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof
CN103627392B (en) A kind of stibnate base red fluorescent powder and its preparation method and application
CN102260498B (en) Nitric oxide orange red fluorescent powder for white LED (light-emitting diode) and preparation method thereof
CN103484112B (en) Rare-earth europium-activated single-component white-light fluorescent powder and preparation method thereof
CN109536168B (en) Eu (Eu)2+Ion-doped high-luminous-efficiency blue fluorescent powder and preparation method and application thereof
CN102093888A (en) Preparation method and application of warm white fluorescent powder
CN111154488A (en) Terbium-doped germanate green fluorescent powder for white light LED and preparation method thereof
CN103725285B (en) Single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof
Han et al. Single-phase and warm white-light-emitting phosphors CaLa2− x− y (MoO4) 4: xDy3+, yEu3+: synthesis, luminescence and energy transfer
TWI359857B (en) White light illumination device
CN102585831B (en) Europium-ion-excited fluoromolybdate red fluorescent powder and preparation method and application thereof
CN103059849B (en) Silicophosphate green fluorescent powder activated by Eu&lt;2+&gt; and preparation method as well as application thereof
CN101412911A (en) Aluminosilicate blue fluorescent powder and preparation thereof
CN103965897B (en) A kind of LED aluminosilicate yellowish green fluorescent powder and preparation method thereof
CN103013505B (en) Preparation method of single-substrate fluorescent powder for white-light LEDs (light-emitting diodes)
CN102936495B (en) The synthetic method of silicate orange red fluorescence powder for a kind of white light LEDs
CN103694999A (en) Europium ion activated phosphate red fluorescent powder and preparation method thereof
CN104212457B (en) Fluoroborosilicate-based red phosphor, and preparation method and application thereof
CN104830335A (en) Europium-doped borate fluorescent powder and preparing method thereof
CN105199729A (en) NaSrPO4:xEu&lt;3+&gt; red phosphor powder for LED (Light Emitting Diode) and preparation method thereof
Yang et al. The effect of doping Mg2+ on structure and properties of Sr (1.992-x) MgxSiO4: 0.008 Eu2+ blue phosphor synthesized by co-precipitation method
CN103409137A (en) An ultraviolet ray excited SrMgAl10O17: eu2+, mn2+blue-green phosphor
CN107686726A (en) A kind of white light LEDs lithium fluorosilicate sodium red light material and preparation method thereof
CN103849386B (en) A kind of colloidal sol auto-combustion method prepares the method for aluminate blue fluorescent powder
CN103773368A (en) Phosphate blue-fluorescence material for white LED (Light Emitting Diode) and preparation method 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
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20140416

Termination date: 20211214