CN103951187A - Light-emitting glass material for white light LED (Light-Emitting Diode) and preparation method thereof - Google Patents

Light-emitting glass material for white light LED (Light-Emitting Diode) and preparation method thereof Download PDF

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CN103951187A
CN103951187A CN201410165081.0A CN201410165081A CN103951187A CN 103951187 A CN103951187 A CN 103951187A CN 201410165081 A CN201410165081 A CN 201410165081A CN 103951187 A CN103951187 A CN 103951187A
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light
white light
glass
glass material
preparation
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陈国华
王家鑫
康晓玲
袁昌来
周昌荣
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Guilin University of Electronic Technology
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Guilin University of Electronic Technology
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Abstract

The invention relates to a light-emitting glass material for a white light LED (Light-Emitting Diode) and a preparation method thereof. The preparation method comprises the following steps of: blending according to a component formula of aZnO-bSrO-cP2O5-dK2O-eTm2O3-fTb4O7-gMnO by taking ammonium dihydrogen phosphate (NH4H2PO4), zinc oxide (ZnO), potassium carbonate (K2CO3), strontium carbonate (SrCO3), manganese carbonate (MnCO3), thulium oxide (Tm2O3) and terbium oxide (Tb4O7); mixing through ball milling for 12 hours, and then drying; keeping temperature at 1150-1200 DEG C for 0.5-1.5 hours to obtain molten glass; then forming and annealing to obtain the uniform and transparent light-emitting glass material. The light-emitting glass material for the white light LED, which is disclosed by the invention, has the advantages of simple preparation process, lower melting temperature and low preparation cost. According to the light-emitting glass material, a light-emitting glass emits white light under the excitation of ultraviolet light, and the color quality regulation and control of the white light can be conveniently realized by regulating glass composition, ion doping concentration and an excitation wavelength, so that the purposes of energy conservation, environment protection and encapsulation process simplification are expected to realize.

Description

A kind of white light LEDs luminous glass material and preparation method thereof
Technical field
The invention belongs to luminous glass material and LED lighting field, be specifically related to a kind of white light LEDs luminous glass material and preparation method thereof.
Background technology
Along with the development of semiconductor lighting technology (LED), LED lamp has become an illumination new lover, gets most of the attention.If incandescent light is replaced to LED lamp, can realize CO 2reduce discharging 90%.LED a kind ofly can change electric energy into the light emitting semiconductor device of luminous energy, belongs to solid state light emitter.White light LEDs, with plurality of advantages such as its long lifetime, energy-efficient, environmental protections, demonstrates huge market potential and application prospect aspect solid-state illumination.Yet, from development, for high-power, high brightness and the high-color rendering light-source angle of general lighting, consider, existing luminescent lamp cost is high, luminous efficiency is low, color developing is lower, the problems such as the low and later stage packaging technology imperfection of stability, do not reach social demand far away, so adopt easily preparation machine-shaping, the transparent luminescent glass with good physical chemistry and thermostability, become LED luminescent device with LED chip direct-assembling, beyond doubt one simple, pursue the first-selection of the society of low-carbon economy.
Summary of the invention
Luminous glass material and preparation method thereof for a kind of white light LEDs that the object of the invention is to solve the deficiency of current material and provide, this material not only cost of manufacture is low, luminous efficiency is high, and this luminous glass material obtains white light under UV-light (300-400nm) excites, and the regulation and control of the color quality of white light can by regulating, glass composition, ion doping concentration and excitation wavelength are convenient to be realized, thereby be expected to realize energy-conservation, environmental protection, simplifies the object of packaging process.
A white light LEDs luminous glass material, its component formula is: aZnO-bSrO-cP 2o 5-dK 2o-eTm 2o 3-fTb 4o 7-gMnO, wherein Tm 2o 3, Tb 4o 7with MnO be extraneous component, a+b+c+d=100.Wherein, by molecular fraction: 40≤a≤42,20≤b≤22,35≤c≤39, d=1.E, f, g are respectively additional Tm 2o 3, Tb 4o 7with the content of MnO, its molecular fraction is: 0.1≤e≤0.2,0.125≤f≤0.5,0.5≤g≤3.
A kind of white light LEDs luminous glass material, comprise following key step: (1) take analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the manganous carbonate that purity is 99.95%, trioxide and the terbium sesquioxide that purity is 99.99% is raw material, according to component formula: aZnO-bSrO-cP 2o 5-dK 2o-eTm 2o 3-fTb 4o 7-gMnO prepares burden.
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 11 ~ 13 h and is made admixtion;
(3) after described admixtion is dry, pour in the clean corundum crucible of previously prepd standby;
(4) crucible of placing glass admixtion is placed in to electric furnace, first at 500 ℃ ~ 700 ℃ insulation 0.5 ~ 1h, is then warming up to the glass metal that 1150-1200 ℃ of insulation 0.5 ~ 1.5h obtains fusing;
(5) subsequently described glass metal is poured into 250 ~ 350 ℃ of preheated copper coin die for molding;
(6) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 400 ~ 450 ℃ and annealed after 7 ~ 9h, furnace cooling, to room temperature, obtains white light LEDs luminescent material.
(7) processing of sample
Block glass, through being cut into the thick sheet glass in 1mm left and right, becomes transparence sheet glass through grinding, polishing.
Described primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood are analytically pure raw material, and manganous carbonate is high pure raw material (purity 99.95%), and rare earths material purity is 99.99%
Described step (4), first at 600 ℃ of insulation 0.5h, is then warming up to 1150-1200 ℃ of insulation 1 h.
In described step (6), getting preheating temperature is 450 ℃, and annealing time is within 8 hours, to be the best.
Tm of the present invention 2o 3, Tb 4o 7the ion of introducing with MnO is Tm 3+, Tb 3+and Mn 2+, Tm wherein 3+in glass, show as the blue emission band that is positioned at 452nm place, Tb 3+main emission peak in glass is positioned at the 542nm in green glow region, also has Tb at 583nm and 485nm simultaneously 3+emission peak.Mn 2+in ruddiness region, present three emission peaks, be respectively 629nm, 670nm and 558nm, wherein 629nm place intensity is the highest.Three kinds of ions are mixed altogether in phosphoric acid zinc strontium glass, under ultraviolet excitation, thereby produce the compound generation white light of bluish-green red trichromatism transmitting.
Advantage of the present invention is:
This white light LEDs is simple by luminous glass material preparation technology, and temperature of fusion is lower, does not need reducing atmosphere just can obtain, and has therefore reduced preparation cost; And phosphate glass dopant ion concentration is higher, the luminous intensity of glass material and luminous efficiency are improved.By regulating glass composition and ionic concn and excitation wavelength can regulate and control easily white color purity.This luminous glass material is expected to become LED luminescent device with the semi-conductor chip direct-assembling of emitting ultraviolet light, can simplify packaging process.
Embodiment
Embodiment 1
A white light LEDs luminous glass material, component formula is: 42ZnO-20SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-xTb 4o 7-1MnO, (x=0.125,0.25,0.5).
Its preparation method, comprise following key step: (1) take analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the manganous carbonate that purity is 99.95%, trioxide and the terbium sesquioxide that purity is 99.99% is raw material, according to component formula: 42ZnO-20SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-xTb 4o 7-1MnO, prepare burden (x=0.125,0.25,0.5).
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 12h and is made admixtion;
(3) after described admixtion is dry, pour in the clean corundum crucible of previously prepd standby;
(4) crucible of placing glass admixtion is placed in to electric furnace, first at 550 ℃ of insulation 0.5h, is then warming up to the glass metal that 1150 ℃ of insulation 0.5h obtain fusing;
(5) subsequently described glass metal is poured into 300 ℃ of preheated copper coin die for molding;
(6) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 450 ℃ and annealed after 9h, furnace cooling, to room temperature, obtains white light LEDs luminescent material.
(7) processing of sample:
Block glass, through being cut into the thick sheet glass in 1mm left and right, becomes transparence sheet glass through grinding, polishing.
Product is after tested: under the exciting of 377nm exciting light, the emmission spectrum of glass sample is by indigo plant red green composition, and blue emission center is 413nm, and green emission peak center is 542nm, and red emission peak center is 618nm.Wherein blue color spectrum is banded transmitting, and green red spectrum is wire transmitting.
The chromaticity coordinates (x, y) that above-mentioned glass is 377nm ultraviolet excitation lower-glass sample at wavelength is respectively (0.306,0.324), (0.310,0.350) and (0.323,0.362), can be adjusted to warm white from cold white light.
embodiment 2
A white light LEDs luminous glass material, component formula is: 42ZnO-22SrO-35P 2o 5-1K 2o-0.2Tm 2o 3-0.5Tb 4o 7-xMnO, (x=0.5,1,2).
Its preparation method, comprise following key step: (1) take analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the manganous carbonate that purity is 99.95%, trioxide and the terbium sesquioxide that purity is 99.99% is raw material, according to component formula: 42ZnO-22SrO-35P 2o 5-1K 2o-0.2Tm 2o 3-0.5Tb 4o 7-xMnO, prepare burden (x=0.5,1,2);
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 12 h and is made admixtion;
(3) after described admixtion is dry, pour in the clean corundum crucible of previously prepd standby;
(4) crucible of placing glass admixtion is placed in to electric furnace, first at 550 ℃ of insulation 0.5h, is then warming up to the glass metal that 1150 ℃ of insulation 0.5h obtain fusing;
(5) subsequently described glass metal is poured into 300 ℃ of preheated copper coin die for molding;
(6) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 450 ℃ and annealed after 9h, furnace cooling, to room temperature, obtains white light LEDs luminescent material.
Raw material primary ammonium phosphate (NH wherein 4h 2pO 4), zinc oxide (ZnO), salt of wormwood (K 2cO 3) and Strontium carbonate powder (SrCO 3) be analytical pure raw material, manganous carbonate is high pure raw material (concentration 99.95%), rare earths material trioxide (Tm 2o 3), terbium sesquioxide (Tb 4o 7) purity be 99.99%.
(7) processing of sample:
Block glass, through being cut into the thick sheet glass in 1mm left and right, becomes transparence sheet glass through grinding, polishing.
Product is after tested: under the exciting of wavelength 377nm excitaton source, the emission spectrum of glass sample is by indigo plant red green composition, and blue emission center is 414nm, and green emission peak center is 542nm, and red emission peak center is 618nm.Wherein blue color spectrum is banded transmitting, and green red spectrum is wire transmitting.
The chromaticity coordinates (x, y) that above-mentioned glass is 377nm ultraviolet excitation lower-glass sample at wavelength is respectively (0.313,0.390), (0.323,0.362) and (0.328,0.360), can be adjusted to white light tone.
Embodiment 3
A white light LEDs luminous glass material, component formula is: 42ZnO-20SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-xTb 4o 7-1MnO, (x=0.5,1,2).
Its preparation method, comprise following key step: (1) take analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the manganous carbonate that purity is 99.95%, trioxide and the terbium sesquioxide that purity is 99.99% is raw material, according to component formula: 42ZnO-20SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-xTb 4o 7-1MnO, prepare burden (x=0.5,1,2);
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 12 h and is made admixtion;
(3) after described admixtion is dry, pour in the clean corundum crucible of previously prepd standby;
(4) crucible of placing glass admixtion is placed in to electric furnace, first at 550 ℃ of insulation 0.5h, is then warming up to the glass metal that 1150 ℃ of insulation 0.5h obtain fusing;
(5) subsequently described glass metal is poured into 300 ℃ of preheated copper coin die for molding;
(6) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 450 ℃ and annealed after 8h, furnace cooling, to room temperature, obtains white light LEDs luminescent material.
Raw material primary ammonium phosphate (NH wherein 4h 2pO 4), zinc oxide (ZnO), salt of wormwood (K 2cO 3) and Strontium carbonate powder (SrCO 3) be analytical pure raw material, manganous carbonate is high pure raw material (concentration 99.95%), rare earths material trioxide (Tm 2o 3), terbium sesquioxide (Tb 4o 7) purity be 99.99%.
4) processing of sample
Block glass, through being cut into the thick sheet glass in 1mm left and right, becomes transparence sheet glass through grinding, polishing.
Product is after tested: under 351nm excites, the emission spectrum of glass sample is by indigo plant red green composition, and blue emission center is 450nm, and green peak center is 542nm, and red peak center is 668nm.Wherein blue color spectrum is banded transmitting, and green red spectrum is wire transmitting.
The chromaticity coordinates (x, y) that above-mentioned glass is 358nm ultraviolet excitation lower-glass sample at wavelength is respectively (0.314,0.339), (0.315,0.338) and (0.333,0.330), when MnO increases, close to the photochromic coordinate of standard white (0.333,0.333).
Embodiment 4
A white light LEDs luminous glass material, its component formula is 41ZnO-21SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-0.5Tb 4o 7-xMnO, (x=0.5,1,2).
Its preparation method, comprises following key step: take analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the manganous carbonate that purity is 99.95%, trioxide and the terbium sesquioxide that purity is 99.99% is raw material, according to component formula: 41ZnO-21SrO-37P 2o 5-1K 2o-0.2Tm 2o 3-0.5Tb 4o 7-xMnO, prepare burden (x=0.5,1,2);
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 12 h and is made admixtion;
(3) after described admixtion is dry, pour in the clean corundum crucible of previously prepd standby;
(4) crucible of placing glass admixtion is placed in to electric furnace, first at 550 ℃ of insulation 0.5h, is then warming up to the glass metal that 1150 ℃ of insulation 0.5h obtain fusing;
(5) subsequently described glass metal is poured into 300 ℃ of preheated copper coin die for molding;
(6) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 450 ℃ and annealed after 8 hours, furnace cooling, to room temperature, obtains white light LEDs luminescent material.
Raw material primary ammonium phosphate (NH wherein 4h 2pO 4), zinc oxide (ZnO), salt of wormwood (K 2cO 3) and Strontium carbonate powder (SrCO 3) be analytical pure raw material, manganous carbonate is high pure raw material (concentration 99.95%), rare earths material trioxide (Tm 2o 3), terbium sesquioxide (Tb 4o 7) purity be 99.99%.
(7) processing of sample
Block glass, through being cut into the thick sheet glass in 1mm left and right, becomes transparence sheet glass through grinding, polishing.
Product is after tested: under 368nm excites, the emission spectrum of glass sample is by indigo plant red green composition, and blue emission center is 413nm, and green peak center is 542nm, and red peak center is 618nm.Wherein blue color spectrum is banded transmitting, and green red spectrum is wire transmitting.
The chromaticity coordinates (x, y) that above-mentioned glass is 368nm ultraviolet excitation lower-glass sample at wavelength is respectively (0.315,0.380), (0.327,0.359), (0.330,0.352) and (0.321,0.325).

Claims (6)

1. a preparation method for luminous glass material for white light LEDs, comprises the steps:
(1), with analytically pure primary ammonium phosphate, zinc oxide, Strontium carbonate powder, salt of wormwood, the trioxide that the manganous carbonate that purity is 99.95% and purity are 99.99% and terbium sesquioxide are raw material, according to component formula: aZnO-bSrO-cP 2o 5-dK 2o-eTm 2o 3-fTb 4o 7-gMnO prepares burden;
(2) the above-mentioned raw material weighing up is put into ball grinder, the amount that adds dehydrated alcohol, just to flood raw material and abrading-ball is advisable, is ground 11 ~ 13 h and is made admixtion;
(3) glass batch is placed in to electric furnace, first at 500 ℃ ~ 700 ℃ insulation 0.5 ~ 1h, is then warming up to the glass metal that 1150-1200 ℃ of insulation 0.5-1.5 h obtains having melted;
(4) subsequently described glass metal is poured into 250 ~ 350 ℃ of preheated copper coin die for molding;
(5) then the glass of described moulding is put into rapidly in the retort furnace that is heated in advance 400 ~ 450 ℃ and annealed after 7 ~ 9 h, furnace cooling, to room temperature, obtains white light LEDs luminous glass material.
2. preparation method according to claim 1, is characterized in that: step (1) is described: aZnO-bSrO-cP 2o 5-dK 2o-eTm 2o 3-fTb 4o 7-gMnO, wherein Tm 2o 3, Tb 4o 7with MnO be extraneous component, a+b+c+d=100, wherein, by molecular fraction: 40≤a≤42,20≤b≤22,35≤c≤39, d=1, e, f, g are respectively additional Tm 2o 3, Tb 4o 7with the content of MnO, its molecular fraction is: 0.1≤e≤0.2,0.125≤f≤0.5,0.5≤g≤3.
3. white light LEDs luminous glass material as claimed in claim 1, is characterized in that: the described glass batch of step (3), first at 600 ℃ of insulation 0.5h, is then warming up to 1150-1200 ℃ of insulation 1 h.
4. white light LEDs luminous glass material as claimed in claim 1, is characterized in that: the described copper coin mold preheating temperature of step (4) is 300 ℃.
5. white light LEDs luminous glass material as claimed in claim 1, is characterized in that: the described preheating temperature of step (5) is 450 ℃.
6. white light LEDs luminous glass material as claimed in claim 1, is characterized in that: the described annealing time of step (5) is 8 h.
CN201410165081.0A 2014-04-23 2014-04-23 Light-emitting glass material for white light LED (Light-Emitting Diode) and preparation method thereof Pending CN103951187A (en)

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Application publication date: 20140730