CN102925975A - Making method for YAG single crystal for white light LED - Google Patents
Making method for YAG single crystal for white light LED Download PDFInfo
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- CN102925975A CN102925975A CN2011102266383A CN201110226638A CN102925975A CN 102925975 A CN102925975 A CN 102925975A CN 2011102266383 A CN2011102266383 A CN 2011102266383A CN 201110226638 A CN201110226638 A CN 201110226638A CN 102925975 A CN102925975 A CN 102925975A
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Abstract
The present invention relates to a making method for a YAG single crystal for a white light LED. The YAG single crystal has a chemical general formula of (A3-x)(Al5-2mBmCm)FnO12-n:xCe, wherein A is one or a plurality of materials selected from Y, Gd, La and Tb, B is one or a plurality of materials selected from Ti, Zr and V, C is one or two materials selected from Mn, Zn, Mg and Li, x is more than or equal to 0.03 and is less than or equal to 0.1, m is more than or equal to 0.01 and is less than or equal to 2, and n is more than or equal to 0 and is less than or equal to 3x. According to the making method, matched raw materials are pretreated, and then heated to a temperature of 1970 DEG C in an iridium crucible to obtain a melt; a pure YAG crystal is adopted as a seed crystal, and crystal growth is performed in a single crystal furnace to obtain complete single crystals with characteristics of various concentrations and no obvious flaw; a carbon sheet cutting machine is adopted to adhere the crystals to organic glass to cut into crystal sheets having the desired thickness of approximate 0.2-5 mm; soaking is performed for 12 hours by using acetone; burnishing is performed through coarse sand and fine sand; a polishing machine is adopted to carry out polishing on both surfaces of the crystal for more than 6 hours; no blister and defect exists through microscopic detection; and the processed crystal sheets having different concentrations and thicknesses are encapsulated on a LED light emitting diode by using a high temperature resistance colloidal, wherein the crystal has good thermal conductivity and physical and chemical stability so as to effectively improve luminous efficiency of the LED and prolong a service life of the LED.
Description
Technical field
The present invention relates to a kind of white light LEDs making method---RE of YAG single crystal, Ce:YAG (RE=La, Tb, Gd) single crystal is used for the method for design of LED, and the present invention is designed into growth, the processing of single crystal and the encapsulation process that is used for LED.
Background technology
White light LEDs possesses solidification, volume is little, thermal value is low, current consumption is little, the life-span is long, speed of response is fast and the advantage such as environmental protection, is widely used in the fields such as general illumination and backlight.Present commercial white light LEDs is mainly formed by blue chip and gold-tinted phosphor combination, and the blue light of blue chip emission and fluorescent material are by blue-light excited and yellow light mix generation emission is luminous.According to the complementary color principle, namely obtain the visible white light behind blue light and the gold-tinted additive color mixture.Although business-like fluorescent material has been obtained huge success, still exist efficient low, lack of homogeneity, the shortcoming such as light decay is large, and the life-span is short, and physical and chemical performance is poor has a strong impact on the performance of white light LEDs.
Existing document has certain research about fluorescent material in the change of defective aspect its stability, the aging, the La such as the Wang Jing of information science and engineering institute of Chinese Marine University
2O
3Coating fluorescent powder carries out the encapsulation of LED so that the fluorescent material of LED has had certain development.The Guan Rongfeng of Institutes Of Technology Of He'nan etc. utilizes glass also to make some progress with the encapsulation that the fluorescent glass that mixes manufacturing of fluorescent material carries out LED.The method of employing single crystal can be gathered the advantage of film and glass, and the performance crystal has advantages of.
This patent is at Ce
3+On the basis of mixing, one or several of Y, Gd, La, Tb in the co-doped lanthanon, perhaps a kind of among the Ti in the metallic element, Zn, Mg, the Li or two kinds.The performance that contrasts the fluorescent crystal that every kind of method of design makes adapts to the needs of white-light LED encapsulation.
Summary of the invention
Technical problem to be solved by this invention provides the RE that a kind of white light LEDs is used, Ce:YAG (RE=La, Tb, Gd) monocrystalline and the encapsulation that is used for white light LEDs.The mol ratio of making monocrystalline is (A
3-x) (Al
5-2mB
mC
m) F
nO
12-n: xCe, wherein A is one or several of Y, Gd, La, Tb, and B is one or several among Ti, Zr, the V, and C is a kind of among Mn, Zn, Mg, the Li or two kinds.0.03≤x≤0.1,0.01≤m≤2,0≤n≤3x wherein.Introduce the element substitution Al such as a small amount of Ti, Zr, Mg, Zn, introduce simultaneously part F and substitute O.Can adjust by the ratio of adjusting Ti, Zr, Mg, Zn, Al and F position and the optical parametric thereof of fluorescent crystal emission peak, the high brightness YAG monocrystalline that different application requires is satisfied in preparation.
Related preparation process:
(1) raw material that adopts of preparation method of the present invention is Y
2O
3, Gd
2O
3, La
2O
3, Tb
2O
3, Al
2O
3, ZnO, MnO, MgO, TiO
2, V
2O
5, CeF
3In several, and material purity is 99.999%.
(2) oven dry: first will with initial feed in air under 600 ℃ of temperature calcination 10 hours to remove planar water and other impurity.
(3) weigh, mixed grinding: by the good raw material of proportioning weighing, mixed more than 12 hours continuously in mixing tank.
(4) binder, pre-burning: will mix again uniform raw material depresses to Φ 15 * 10mm at hydropress material cake, the material cake that presses is put into corundum crucible, in air atmosphere, calcination is approximately 10 hours under 1200 ℃ of temperature condition, and it is for subsequent use that the raw material that sinters should be put into loft drier.
(5) Czochralski grown YAG crystal step: the selection → shove charge of the seed crystal → burner hearth inflation → temperature increasing for melting materials → roasting crystalline substance → necking down → shouldering of sowing → isometrical → carry and take off → lower the temperature grows the YAG monocrystalline.
(6) with the carbon plate cutting machine crystal is adhered to and cut into the wafer that desired size thickness is about 0.2-5mm on the synthetic glass, after soaking 12 hours with acetone, after crossing coarse sand and fine sand and polishing, utilize polishing machine that the crystal two sides was polished more than 6 hours, microscopic inspection is without sand holes and defective, the wafer of the different concns thickness that machines is encapsulated on the LED photodiode with high temperature resistant colloid, detects luminescent properties.
Existing fluorescent material stability and heat-resisting ability are poor, particularly the junction temperature of its PN junction raises so that traditional Resins, epoxy parcel fluorescent material is difficult to satisfy its requirement during the white light LEDs the increase of output power, prolongation along with the time, Resins, epoxy is easily aging, so that variation has also occured the stable homogeneity of fluorescent material, thereby also cause its luminous efficiency to descend.The present invention adopts single crystal as embedded photoluminescent material, the single crystal of growth can adopt the method for processing to produce the single-chip of various different sizes and thickness in batches, its natural cleavage surface of single-chip with regular shape also can with the better combination of LED, the heat conductance of its crystal excellence is so that it can effectively bear the high junction temperature of PN junction, also timely high-quality heat radiation, thereby improve the power of LED, have good physical and chemical stability as crystalline material, improved luminous efficiency.
Description of drawings
Fig. 1 is the spectrum relative energy distribution curve of 50W LED matrix among the embodiment 1;
Fig. 2 is the spectrum relative energy distribution curve of 150W LED matrix among the embodiment 2;
Embodiment
Embodiment 1
The YAG monocrystalline consist of Y
2.94Al
5(O, F)
12: 0.06Ce, making method is as follows: accurately take by weighing raw material Y
2O
366.39g, Al
2O
350.98g, CeF
32.37g, BaF
23.51g, above-mentioned raw materials is carried out early stage to be processed, the raw material that sinters is put into the iridium crucible of 60mm diameter, in the D400 single crystal growing furnace, be heated to 1970 ℃ of thawings, adopt pure YAG single crystal rod to carry out the growth of crystal as seed crystal, rotating speed is 12r/min, and isometrical pulling rate is 2.0mm/h, grows the crystal of certain size.The crystal that grows is fixed on according to desired size on glassly cuts with the carbon plate cutting machine, soaking lower wafer with acetone grinds and polishes, microscopic examination is without sand holes and defective, carry out again the polishing more than 6 hours, the wafer size that processes is thickness 0.2mm, the length of side is the single-chip of 29mm, single-chip used without the shadow tackiness agent be encapsulated on the integrated led chip of 50 1W, its rated output is to encapsulate the device of finishing LED on the 50W (light-emitting area of integrated 50 chips is 27mm*27mm), the adjusting electric current is 1.5A, higher more than 33% than fluorescent material electrical current, the white light colour temperature is about 6000K, exothermic temperature is low by about 30% than fluorescent material, and chip is without damage, and optical throughput is more than the 5000lm.
The YAG monocrystalline consist of Y
2.92Al
4.8Mg
0.1Ti
0.1(O, F)
12: 0.08Ce, making method is as follows: accurately take by weighing raw material Y
2O
365.94g, Al
2O
348.94g, CeF
33.15g, MgO 0.81g, TiO
21.60g, BaF
23.51g, above-mentioned raw materials is carried out early stage to be processed, the raw material that sinters is put into the iridium crucible of 60mm diameter, in the D400 single crystal growing furnace, be heated to 1970 ℃ of thawings, pure YAG single crystal rod is carried out the growth of crystal as seed crystal, rotating speed is 12r/min, and isometrical pulling rate is 2.0mm/h, grows the crystal of certain size.Wafer is ground and polishes, microscopic examination is without sand holes and defective, carry out again the polishing more than 6 hours, single crystal is polished post-treatment become 0.5mm thickness, the length of side is the single-chip of 53mm, single-chip used without the shadow tackiness agent be encapsulated on the integrated led chip of 50 3W, its rated output is to encapsulate the device of finishing LED on the 150W (light-emitting area of integrated 50 chips is 50mm*50mm), the adjusting electric current is 3A, luminescent properties is good, white color gentle and, exothermic temperature is low more than 30% than fluorescent material, luminous illumination slightly descends than fluorescent material, and optical throughput reaches more than the 11000lm under the peak power.
Embodiment 3
The YAG monocrystalline consist of Y
2.82Gd
0.1Al
4.8Mg
0.1Ti
0.1(O, F)
12: 0.08Ce, making method is as follows: accurately take by weighing raw material Y
2O
363.68g, Gd
2O
33.63g, Al
2O
348.94g, CeF
33.15g, MgO 0.81g, TiO
21.60g, BaF
23.51g, above-mentioned raw materials is carried out early stage to be processed, the raw material that sinters is put into the iridium crucible of 60mm diameter, in the D400 single crystal growing furnace, be heated to 1970 ℃ of thawings, pure YAG single crystal rod is carried out the growth of crystal as seed crystal, rotating speed is 11r/min, and isometrical pulling rate is 2.2mm/h, grows the crystal of certain size.Single crystal is polished post-treatment become 0.8mm thickness, the length of side is the single-chip of 55mm, single-chip used without the shadow tackiness agent be encapsulated on the integrated led chip of 50 3W, its rated output is to encapsulate the device of finishing LED on the 150W (light-emitting area of integrated 50 chips is 50mm*50mm), the adjusting electric current is 3A, luminescent properties is good, the white light colour temperature is about 6000K, exothermic temperature is low more than 40% than fluorescent material, optical throughput slightly descends than fluorescent material, and optical throughput reaches more than the 9000lm under the peak power.
Embodiment 4
The YAG monocrystalline consist of Y
2.62La
0.3Al
4.8Mg
0.1Ti
0.1(O, F)
12: 0.08Ce, making method is as follows: accurately take by weighing raw material Y
2O
363.68g, La
2O
39.77g, Al
2O
348.94g, CeF
33.15g, MgO 0.81g, TiO
21.60g, BaF
23.51g, above-mentioned raw materials is carried out early stage to be processed, the raw material that sinters is put into the iridium crucible of 60mm diameter, in the D400 single crystal growing furnace, be heated to 1970 ℃ of thawings, pure YAG single crystal rod is carried out the growth of crystal as seed crystal, rotating speed is 11r/min, and isometrical pulling rate is 1.8mm/h, grows the crystal of certain size.Monocrystalline is processed as thickness 1.2mm, the length of side is the single-chip of 108mm, single-chip used without the shadow tackiness agent be encapsulated on the integrated led chip of 50 5W, its rated output is to encapsulate the device of finishing LED on the 250W (light-emitting area of integrated 50 chips is 100mm*100mm), rated output is 250W, electrical current is 4.5A, and heat dissipation capacity is good, and the test light flux reaches 15000lm.
Claims (4)
1. the making method of a white light LEDs usefulness YAG single crystal is characterized in that: with (A
3-x) (Al
5-2mB
mC
m) F
nO
12-n: the xCe single crystal is as the luminescent material of white light LEDs.Wherein A is one or several of Y, Gd, La, Tb, and B is one or several among Ti, Zr, the V, and C is a kind of among Mn, Zn, Mg, the Li or two kinds.0.03≤x≤0.1,0.01≤m≤2,0≤n≤3x wherein.Raw material with proportioning carries out RE, and the growth of Ce:YAG (RE=La, Tb, Gd) monocrystalline is encapsulated in the single-chip of processing on the LED luminescence chip.
2. as claimed in claim 1 with the making method of single crystal for white light LEDs, it is characterized in that: RE, Ce:YAG (RE=La, Tb, Gd) single-chip become the bright thin slice of rule of 0.2-5mm thickness for cutting and polishing post-treatment.
3. as claimed in claim 1 with the making method of single crystal for white light LEDs, it is characterized in that: RE, all mirror polish of Ce:YAG (RE=La, Tb, Gd) single-chip, the transparent light of crystal, the large 2%-15% of surface area ratio lumination of light emitting diode area.
4. the making method that single crystal is used for white light LEDs as claimed in claim 1 is characterized in that RE, and Ce:YAG (RE=La, Tb, Gd) single-chip is used without on the parallel LED of the being encapsulated in luminescence chip of shadow tackiness agent, contacts with the LED luminescence chip.
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|---|---|---|---|
| CN2011102266383A CN102925975A (en) | 2011-08-09 | 2011-08-09 | Making method for YAG single crystal for white light LED |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910654A (en) * | 2015-06-12 | 2015-09-16 | 佛山市启正电气有限公司 | Heat dissipation material for solar photovoltaic cell and preparation method of heat dissipation material |
| CN106129222A (en) * | 2016-08-23 | 2016-11-16 | 中国科学院上海光学精密机械研究所 | The high power white LED device of monolithic package |
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| CN106129222A (en) * | 2016-08-23 | 2016-11-16 | 中国科学院上海光学精密机械研究所 | The high power white LED device of monolithic package |
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Application publication date: 20130213 |