CN1995277A - Single component white light fluorescent powder for LED lamp and its preparation method - Google Patents

Single component white light fluorescent powder for LED lamp and its preparation method Download PDF

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Publication number
CN1995277A
CN1995277A CNA2006101679354A CN200610167935A CN1995277A CN 1995277 A CN1995277 A CN 1995277A CN A2006101679354 A CNA2006101679354 A CN A2006101679354A CN 200610167935 A CN200610167935 A CN 200610167935A CN 1995277 A CN1995277 A CN 1995277A
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powder
led lamp
fluorescent powder
single component
white light
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CN100554373C (en
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田一光
龚兵勇
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Wenzhou University
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Wenzhou University
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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 discloses a single-component white fluorescent powder and making method of LED lamp, wherein the molecular formula of fluorescent powder is MO .aAl2O3 .bSiO2 .cL:dX (MO is random two composition of MgO, CaO, SrO or BaO; L is boracic acid mineralizer; X is activator with manganese and europium; a, b, c, d represents the molar number of Al2O3, SiO2, mineralizer L and activator X when the molar number of MO is 1; 2<=(a+b)<=5; b=(1-5) a; c=0.1-0.4; d=0.01-0.4). The making method comprises the following steps: weighing raw material; grinding to grain size at 1-5um; milling; moulding through bidirection to form blank; sintering; insulating under reducing condition with carbon particle; cooling to indoor temperature at certain velocity; repeating the heat disposal step to obtain the sintered material with luminance over 40cd/m2 and main peak between 400 and 500 nm.

Description

A kind of LED lamp single component white light fluorescent powder and preparation method thereof
Technical field
The invention belongs to material science, particularly a kind of near ultraviolet excitated one-component LED lamp preparation method of white emitting fluorescent powder.
Background technology
1993, Japanese Ri Ya chemical company acquisition of technology broke through, and successfully develops blue light GaN photodiode (LED), for the arrival in semiconductor solid lighting epoch has brought hope.Semiconductor lighting is compared with incandescent osram lamp and luminescent lamp, have nontoxic, overlong service life (100,000 hours), energy-efficient, all solid state, plurality of advantages such as operating voltage is low, shock resistance and security are good, will become the new light sources that 21 century substitutes the traditional lighting device.1997, Ri Ya chemical company utilized the rear-earth-doped YAG:Ce of blue light tube core pumping 3+Gold-tinted fluorescent material is developed white LED lamp and is also put goods on the market very soon.Because white light is to be formed by the yellow fluorescence of fluorescent material and the blue light of LED, the glow color of ubiquity device changes with the variation of driving voltage and fluorescent coating thickness, color reducibility is poor, and colour rendering index is low, and the junction temperature of chip rising causes problems such as look drift.For addressing the above problem, adopt near-ultraviolet light (380～410 nanometer) InGaN tube core to excite three primary colors fluorescent powder to realize that white LED lamp has become at present one of focus of these field research and development in the world.Because vision is to the insensitivity of near-ultraviolet light, the color of this class white light LEDs is only determined by fluorescent material.Therefore, the white emitting fluorescent powder that colour stable, color reducibility and colour rendering index are high is considered to the leading material of White-light LED illumination of new generation.
At present, the white emitting fluorescent powder that is complementary with the near-ultraviolet light tube core lacks, and luminescent properties is undesirable, and this white emitting fluorescent powder generally adopts the way of mixing three kinds of primary colours fluorescent material of red, green, blue to make.Because exist color to absorb and proportioning regulation and control problem between the mixture, luminous efficiency and color rendition performance are a greater impact again.Therefore developing panchromatic one-component LED lamp is of great significance with white emitting fluorescent powder.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of LED lamp single component white light fluorescent powder and preparation method thereof is provided.
The objective of the invention is to be achieved through the following technical solutions:
It is alkaline earth metal aluminosilicate that LED lamp of the present invention is formed with single component white light fluorescent powder matrix, and general expression is MOaAl 2O 3BSiO 2CL:dX, wherein MO is any two kinds of compositions of MgO, CaO, SrO or BaO; L is the boric acid mineralizer, and X is the activator that different ratios manganese and europium are formed, and a, b, c, d are representative Al when the mole number of MO is 1 2O 3, SiO 2, mineralizer L and activator X mole number, 2≤(a+b)≤5, b=(1～5) a, c=0.1～0.4, d=0.01～0.4.
LED lamp of the present invention comprises the steps: with the preparation method of single component white light fluorescent powder
1. the burning raw material can be selected alkaline earth metal carbonate or subcarbonate or oxide compound, aluminum oxide or aluminium hydroxide, SiO 2 powder or metasilicic acid or orthosilicic acid in the fluorescent material;
2. adopting planetary ball mill that the raw material of aluminium, silicon and europium is carried out ball milling to particle diameter is 1～5 micron;
3. the raw material of the aluminium behind the ball milling, silicon and europium is carried out abundant ball milling with the raw material and the boric acid of calcium, magnesium, strontium, barium, manganese, the ball milling time is 10～25 hours;
4. adopt metal die to press knot to obtain biscuit on hydropress with two-way press moulding mode, pressing knot pressure is 1000～5000kg/cm 2
5. biscuit is put into corundum crucible, use high temperature resistance furnace, under the reductive condition of gac, be heated to 1100～1400 ℃, and be incubated 1～5 hour, reduce to room temperature with 2～10 ℃/minute rate of temperature fall subsequently with 300～500 ℃/hour rate of heating;
6. repetitive operation step 5. 2～5 times obtains sintered material;
7. adopt hand lapping and planetary ball mill ball milling method to combine particle size in the sintered compact is milled to 1～5 micron;
8. remove the impurity that remains in the powder with deionized water and washing with alcohol,, obtain powdered material in 80～150 ℃ of oven dry 10～30 hours;
9. adopt x-ray powder diffraction instrument to measure the crystalline phase of the XRD figure spectrum of fluorescent material with the checking powder, shine luminosity and the glow color of verifying fluorescent material with 365 nanometer ultraviolet lamps, measure the excitation spectrum and the emmission spectrum of fluorescent material with the ultraviolet-visible spectrophotometer.
The test of the luminosity of luminescent material of the present invention is undertaken by the GB/T14633-93 standard-required.
The present invention has successfully prepared a kind of LED lamp single component white light fluorescent powder by selecting suitable aluminosilicate body material, activator ion collocation, mineralizer and preparation method, is suitable near ultraviolet-purple LED and excites.The luminosity of fluorescent material of the present invention (under the 365 nanometer ultra violet lamps) has surpassed 40cd/m 2, its emmission spectrum is distributed in whole visible region, and main peak can change in 400～500 nanometer range according to composition, and at yellow light area once peak (accompanying drawing 2); Sintered compact has loosely organized, is easy to fragmentation, and particle diameter is less than 5 microns, advantage such as brightness height, glow color are pure.
Description of drawings
Fig. 1 is the powder crystal diffracting spectrum (XRD) of fluorescent material.
Fig. 2 is excitation spectrum and the emmission spectrum that fluorescent material records with ultraviolet-visible pectrophotometer.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but be not limited to these embodiment.
Embodiment 1:
LED lamp single component white light fluorescent powder, expression MOaAl 2O 3BSiO 2CL:dX, wherein MO is CaO, BaO; L is a boric acid, and X is 1: 1 europium sesquioxide of mol ratio and manganese oxide, a=1.0, b=1.0, c=0.2, d=0.02.
The preparation method is as follows:
Take by weighing CaCO 33.0027 gram, BaCO 313.4191 gram, A1 2O 3Micro mist 10.2007 grams, SiO 2Fine powder 6.0100 grams, Eu 2O 30.3579 gram, MnCO 30.1149 gram, boric acid 1.236 grams.Adopt planetary ball mill with Al 2O 3, SiO 2And Eu 2O 3Carrying out ball milling to particle diameter is about 1 micron, subsequently with the oxide compound mixed powder and the CaCO that obtain 3, BaCO 3, MnCO 3Carry out the thorough mixing ball milling about 10 hours with boric acid, use metal die with two-way press moulding mode with 1000kg/cm 2Pressure be pressed into the biscuit that diameter is 13mm, this biscuit is put into corundum crucible, use high temperature resistance furnace; under the active carbon granule reductive condition; be heated to 1250 ℃ with 300 ℃/hour speed, and under this temperature, be incubated 5h, reduce to room temperature with 10 ℃/hour rate of temperature fall subsequently.Repeat intensification, insulation and temperature-fall period 2 times, obtain sintered material, the mode that adopts hand lapping and planetary type ball-milling to combine is milled to particle size in the sintered compact about 1 micron, remove remaining impurities with deionized water and washing with alcohol, in 120 ℃ of oven dry 30 hours, make particles dispersed uniformly light-emitting material powder, it is luminous that fluorescent material is inclined to one side pearl opal under the 365nm ultra violet lamp, adopt x-ray powder diffraction instrument to measure the diffracting spectrum of fluorescent material, adopt ultraviolet-visible spectrophotometer to measure the excitation spectrum and the luminescent spectrum of fluorescent material.
Embodiment 2:
LED lamp single component white fluorescent powder, expression MOaAl 2O 3BSiO 2CL:dX, wherein MO is SrO, CaO; L is a boric acid, and X is 1: 3 europium sesquioxide of mol ratio and manganese oxide, a=1.1, b=2.0, c=0.3, d=0.06.
The preparation method is as follows:
Take by weighing SrCO 32.9526 gram, CaCO 37.4067 gram, Al 2O 3Micro mist 12.2408 grams, SiO 2Fine powder 12.0200 grams, Eu 2O 30.5369 gram, MnCO 30.5172 gram, boric acid 1.854 grams.Adopt planetary ball mill with Al 2O 3, SiO 2And Eu 2O 3Carrying out ball milling to particle diameter is about 2 microns, subsequently with the oxide compound mixed powder and the SrCO that obtain 3, CaCO 3, MnCO 3Carry out the thorough mixing ball milling about 15 hours with boric acid, use metal die with two-way press moulding mode with 2000kg/cm 2Pressure be pressed into the biscuit that diameter is 13mm, this biscuit is put into corundum crucible, use high temperature resistance furnace; under the active carbon granule reductive condition; be heated to 1200 ℃ with 350 ℃/hour speed, and under this temperature, be incubated 4h, reduce to room temperature with 8 ℃/hour rate of temperature fall subsequently.Repeat intensification, insulation and temperature-fall period 3 times, obtain sintered material, the mode that adopts hand lapping and planetary type ball-milling to combine is milled to particle size in the sintered compact about 2 microns, remove remaining impurities with deionized water and washing with alcohol, in 120 ℃ of oven dry 30 hours, make particles dispersed uniformly light-emitting material powder, it is luminous that fluorescent material is inclined to one side pearl opal under the 365nm ultra violet lamp, adopt x-ray powder diffraction instrument to measure the diffracting spectrum of fluorescent material, adopt the excitation spectrum and the luminescent spectrum of ultraviolet-visible spectrophotometry fluorescent material.。
Embodiment 3.:
LED lamp single component white fluorescent powder, expression MOaAl 2O 3BSiO 2CL:dX, wherein MO is MgO, CaO; L is a boric acid, and X is 1: 5 europium sesquioxide of mol ratio and manganese oxide, a=1.0, b=2.5, c=0.1, d=0.09.
The preparation method is as follows:
Take by weighing (MgCO 3) 4Mg (OH) 25H 2The O1.9432 gram, CaCO 37.1064 gram, Al 2O 3Micro mist 10.2007 grams, SiO 2Fine powder 15.0250 grams, Eu 2O 30.5369 gram, MnCO 30.8620 gram, boric acid 0.618 gram.Adopt planetary ball mill with Al 2O 3, SiO 2And Eu 2O 3Carrying out ball milling to particle diameter is about 3 microns, subsequently with the oxide compound mixed powder and (the Mg CO that obtain 3) 4Mg (OH) 25H 2O, CaCO 3, MnCO 3Carry out the thorough mixing ball milling about 20 hours with boric acid, use metal die with two-way press moulding mode with 3000kg/cm 2Pressure be pressed into the biscuit that diameter is 13mm, this biscuit is put into corundum crucible, use high temperature resistance furnace; under the active carbon granule reductive condition; be heated to 1300 ℃ with 400 ℃/hour speed, and under this temperature, be incubated 3h, reduce to room temperature with 6 ℃/hour rate of temperature fall subsequently.Repeat intensification, insulation and temperature-fall period 4 times, obtain sintered material, the mode that adopts hand lapping and planetary type ball-milling to combine is milled to particle size in the sintered compact about 4 microns, remove remaining impurities with deionized water and washing with alcohol, in 120 ℃ of oven dry 30 hours, make particles dispersed uniformly light-emitting material powder, it is luminous that fluorescent material is inclined to one side pearl opal under the 365nm ultra violet lamp, with the diffracting spectrum of x-ray powder diffraction instrument measurement fluorescent material, measure the excitation spectrum and the luminescent spectrum of fluorescent material with ultraviolet-visible spectrophotometer.
Embodiment 4:
LED lamp single component white fluorescent powder, expression MOaAl 2O 3BSiO 2CL:dX, wherein MO is MgO, BaO; L is a boric acid, and X is 1: 9 europium sesquioxide of mol ratio and manganese oxide, a=1.1, b=3, c=0.2, d=0.2.
The preparation method is as follows:
Take by weighing (MgCO 3) 4Mg (OH) 25H 2O 0.9716 gram, BaCO 313.8138 gram, Al 2O 3Micro mist 11.2207 grams, SiO 2Fine powder 18.03 grams, Eu 2O 30.7158 gram, MnCO 32.0689 gram, boric acid 1.236 grams.Adopt planetary ball mill with Al 2O 3, SiO 2And Eu 2O 3Carrying out ball milling to particle diameter is about 4 microns, subsequently with the oxide compound mixed powder and the (MgCO that obtain 3) 4Mg (OH) 25H 2O, BaCO 3, MnCO 3Carry out the thorough mixing ball milling about 20 hours with boric acid, use metal die with two-way press moulding mode with 4000kg/cm 2Pressure be pressed into the biscuit that diameter is 13mm, this biscuit is put into corundum crucible, use high temperature resistance furnace, under the reductive condition of activated carbon, be heated to 1350 ℃ with 450 ℃/hour speed, and under this temperature, be incubated 2h, reduce to room temperature with 4 ℃/hour rate of temperature fall subsequently.Repeat intensification, insulation and temperature-fall period 4 times, obtain sintered material, the mode that adopts hand lapping and planetary ball mill to combine is milled to particle size in the sintered compact about 4 microns, remove remaining impurities with deionized water and washing with alcohol, in 120 ℃ of oven dry 30 hours, make particles dispersed uniformly light-emitting material powder, it is luminous that fluorescent material is inclined to one side pearl opal under the 365nm ultra violet lamp, with the diffracting spectrum of x-ray powder diffraction instrument measurement fluorescent material, measure the excitation spectrum and the luminescent spectrum of fluorescent material with ultraviolet-visible spectrophotometer.
Embodiment 5:
LED lamp single component white fluorescent powder, expression MOaAl 2O 3BSiO 2CL:dX, wherein MO is MgO, SrO; L is a boric acid, and X is 1: 15 europium sesquioxide of mol ratio and manganese oxide, a=1.5, b=3.2, c=0.40, d=0.32.
The preparation method is as follows:
Take by weighing (MgCO 3) 4Mg (OH) 25H 2O 0.4858 gram, SrCO 39.3007 gram, Al 2O 3Micro mist 15.3010 grams, SiO 2Fine powder 19.2320 grams, Eu 2O 30.7158 gram, MnCO 33.4481 gram, boric acid 2.472 grams.Adopt planetary ball mill with Al 2O 3, SiO 2And Eu 2O 3Carrying out ball milling to particle diameter is about 5 microns, subsequently with the oxide compound mixed powder and the (MgCO that obtain 3) 4Mg (OH) 25H 2O, SrCO 3, MnCO 3Carry out the thorough mixing ball milling about 25 hours with boric acid, use metal die with two-way press moulding mode with 5000kg/cm 2Pressure be pressed into the biscuit that diameter is 13mm, this biscuit is put into corundum crucible, use high temperature resistance furnace, under the reductive condition of activated carbon, be heated to 1100 ℃ with 500 ℃/hour speed, and under this temperature, be incubated 2h, reduce to room temperature with 2 ℃/hour rate of temperature fall subsequently.Repeat intensification, insulation and temperature-fall period 5 times, obtain sintered material, the mode that adopts hand lapping and planetary type ball-milling to combine is milled to particle size in the sintered compact about 5 microns, remove remaining impurities with deionized water and washing with alcohol, in 120 ℃ of oven dry 30 hours, make particles dispersed uniformly light-emitting material powder, under the 365nm ultra violet lamp, it is luminous that fluorescent material is inclined to one side pearl opal, with the diffracting spectrum of x-ray powder diffraction instrument measurement fluorescent material, measure the excitation spectrum and the luminescent spectrum of fluorescent material with ultraviolet-visible spectrophotometer.

Claims (6)

1. LED lamp single component white light fluorescent powder is characterized in that: it is alkaline earth metal aluminosilicate that white emitting fluorescent powder matrix is formed, and general expression is MOaAl 2O 3BSiO 2CL:dX, wherein MO is any two kinds of compositions of MgO, CaO, SrO or BaO; L is a mineralizer, and X is an activator, and a, b, c, d are representative Al when the mole number of MO is 1 2O 3, SiO 2, mineralizer L and activator X mole number, 2≤(a+b)≤5, b=(1～5) a, c=0.1～0.4, d=0.01～0.4.
2. LED lamp single component white light fluorescent powder as claimed in claim 1 is characterized in that: mineralizer is a boric acid.
3. LED lamp single component white light fluorescent powder as claimed in claim 2, it is characterized in that: activator X is formed according to different ratios by manganese and europium.
4. LED lamp single component white light fluorescent powder as claimed in claim 3 is characterized in that: the luminosity of fluorescent material has surpassed 40cd/m under 365 nanometer ultra violet lamps 2, luminescent spectrum is distributed in whole visible region, and main peak can change in 400～500 nanometer range according to composition.
5. LED lamp single component white light fluorescent powder as claimed in claim 3, it is characterized in that: the GB/T14633-93 standard-required is pressed in the test of the luminosity of luminescent material.
6. as the preparation method of each described LED lamp of claim 1～5, formed by following processing step with single component white light fluorescent powder:
1. the burning raw material can be selected alkaline earth metal carbonate or subcarbonate or oxide compound, aluminum oxide or aluminium hydroxide, SiO 2 powder or metasilicic acid or orthosilicic acid in the fluorescent material;
2. adopting planetary ball mill that the raw material of aluminium, silicon and europium is carried out ball milling to particle diameter is 1～5 micron;
3. the raw material of the aluminium behind the ball milling, silicon and europium is carried out abundant ball milling with the raw material and the boric acid of calcium, magnesium, strontium, barium, manganese, the ball milling time is 10～25 hours;
4. adopt metal die to press knot to obtain biscuit on hydropress with two-way press moulding mode, pressing knot pressure is 1000～5000kg/cm 2
5. biscuit is put into corundum crucible, use high temperature resistance furnace, under the reductive condition of gac, be heated to 1100～1400 ℃, and be incubated 1～5 hour, reduce to room temperature with 2～10 ℃/minute rate of temperature fall subsequently with 300～500 ℃/hour speed;
6. repetitive operation step 5. 2～5 times obtains sintered material;
7. adopt hand lapping and planetary ball mill ball milling method to combine particle size in the sintered compact is milled to 1～5 micron;
8. remove the impurity that remains in the powder with deionized water and washing with alcohol,, obtain powdered material in 80～150 ℃ of oven dry 10～30 hours;
9. adopt x-ray powder diffraction instrument to measure the crystalline phase of the XRD figure spectrum of fluorescent material with the checking powder, under the 365nm ultraviolet lamp, shine the luminosity and the glow color of checking fluorescent material, measure the excitation spectrum and the emmission spectrum of fluorescent material with ultraviolet-visible spectrophotometer.
CNB2006101679354A 2006-12-21 2006-12-21 A kind of LED lamp single component white light fluorescent powder and preparation method thereof Expired - Fee Related CN100554373C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134895B (en) * 2006-08-15 2011-05-04 大连路明发光科技股份有限公司 Wide-spectrum excitation fluorescent material and synthesizing method and light-emitting apparatus using the same
CN101565620B (en) * 2009-06-05 2012-04-11 中国科学院长春光学精密机械与物理研究所 Single-phase white-emitting phosphor based on near ultraviolet excitation and preparation method thereof
CN103059840A (en) * 2012-11-01 2013-04-24 宁波南车新能源科技有限公司 White ultra-long afterglow luminescent material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134895B (en) * 2006-08-15 2011-05-04 大连路明发光科技股份有限公司 Wide-spectrum excitation fluorescent material and synthesizing method and light-emitting apparatus using the same
CN101565620B (en) * 2009-06-05 2012-04-11 中国科学院长春光学精密机械与物理研究所 Single-phase white-emitting phosphor based on near ultraviolet excitation and preparation method thereof
CN103059840A (en) * 2012-11-01 2013-04-24 宁波南车新能源科技有限公司 White ultra-long afterglow luminescent material and preparation method thereof
CN103059840B (en) * 2012-11-01 2015-03-25 宁波南车新能源科技有限公司 White ultra-long afterglow luminescent material and preparation method thereof

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