CN102320840A - Fluorescent powder and transparent ceramic doping and co-sintering process method - Google Patents
Fluorescent powder and transparent ceramic doping and co-sintering process method Download PDFInfo
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- CN102320840A CN102320840A CN201110157058A CN201110157058A CN102320840A CN 102320840 A CN102320840 A CN 102320840A CN 201110157058 A CN201110157058 A CN 201110157058A CN 201110157058 A CN201110157058 A CN 201110157058A CN 102320840 A CN102320840 A CN 102320840A
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Abstract
The invention relates to a fluorescent powder and transparent ceramic doping and co-sintering process method, in which fluorescent powder and transparent ceramic powder are doped and co-sintered to form a transparent fluorescent ceramic. The process method is divided into a pressureless sintering process and a vacuum hot pressing sintering process. In the pressureless sintering process, compression molding and sintering are carried out separately, powder is cold molded firstly, then is biscuit fired to remove a certain number of additives and is sintered at a high temperature under the conditions of vacuum, hydrogen or other inert gases; and in the vacuum hot pressing sintering process, molding and sintering are completed in the same step, the powder is firstly put into a mold to be cold pressed to be molded, then a molded sample is put into a vacuum hot pressing furnace for hot pressed sintering, the obtained product is then put into a hot isostatic pressing furnace to be post-treated under high temperature and high pressure, and further the optical property of the fluorescent transparent ceramic is improved. The fluorescent transparent ceramic prepared in the method is used for packaging a blue light LED (light emitting diode) and is also used as fluorescence conversion material and packaging material. Compared with the conventional packaging material, the fluorescent transparent ceramic has excellent optical, thermal and mechanical properties, and can significantly improve the performance of the LED and prolong the service life of the LED.
Description
Technical field
The present invention relates to a kind of making method of transparent fluorescence ceramics, say it is the process method that a kind of fluorescent material and crystalline ceramics mix and burn altogether definitely.
Background technology
The method of current existing at home and abroad generation white light LEDs has multiple; Wherein " blue chip+fluorescent material " produces in the LED packaging process of white light, because epoxy resin has good cohesiveness, electrical insulating property, stopping property and dielectric properties and advantages such as cost is lower, easy-formation become the main flow material that LED encapsulates.But along with improving constantly of white light LEDs brightness and power; Packaged material to LED proposes higher requirement; And the water absorbability that epoxy resin self exists, aging, the poor heat resistance of being prone to, high temperature and short wavelength light have exposed according to defective such as easy to change down; Epoxy resin also is difficult for the even doping of realization and fluorescent material, thereby influences and shorten the performance and the work-ing life of LED device greatly.In order to solve the problems referred to above that epoxy resin exists, organosilicon material has received domestic and international investigator's extensive concern owing to have the good transparency, resistant of high or low temperature, weathering resistance, insulativity etc., is considered to the ideal material of displaced loop epoxy resins.But also there are some shortcomings in organosilicon as packaged material, and organosilicon does not solve the even adulterated problem of fluorescent material, and organosilyl specific refractory power differs bigger with the specific refractory power of led chip about 1.5, be unfavorable for the output of light; In addition, though organosilicon is increasing aspect thermotolerance, the mechanical property than epoxy resin, the ability of under severe environment such as high temperature, highly corrosive, working is relatively poor.And because organosilyl production technique is complicated, cost is higher, currently marketed organosilicon price is very expensive, is unfavorable for the popularization and the application of white light LEDs.
Summary of the invention
In order to overcome above-mentioned defective, the present invention mentions a kind of making method of transparent fluorescence ceramics, says it is that the process method that a kind of fluorescent material and crystalline ceramics doping are burnt altogether is used for the LED encapsulation definitely.
The present invention for the technical scheme that solves its technical problem and adopt is:
A kind of fluorescent material and crystalline ceramics mix and are total to the process method of burning, and fluorescent material and transparent ceramic powder doping are burnt the transparent fluorescence ceramics of formation altogether, are divided into non-pressure sintering technology and vacuum heating-press sintering;
Non-pressure sintering technology: compression moulding and sintering process are separately carried out; Earlier with powder coldmoulding; Molding mode is selected a kind of with in cold isostatic compaction and the wet moulding of punching block coldmoulding or shop; Carry out biscuiting afterwards to remove some additives, under vacuum, hydrogen or other inert gas conditions, carry out high temperature sintering again;
Vacuum heating-press sintering: moulding and sintering are accomplished in same operation; It is molded earlier powder to be put into mold cold; Then the moulding sample is put into vacuum hotpressing stove and carry out hot pressed sintering, resulting product is put into and is carried out aftertreatment under hot isostatic pressing furnace high-temperature, the high pressure, interior temperature 1600-1800 ℃ of stove; Argon gas condition overdraft 150-200Mpa, and then the optical property of raising fluorescence crystalline ceramics.
Described crystalline ceramics is selected high pure raw material for use, gets rid of pore through process means and obtains.
Described fluorescent material is allowed a choice according to led chip type and optical property difference; Blue-light excited yellow fluorescent powder mixes the generation white light; Apply on the blue led chip and greenly can obtain high-color rendering white-light with red fluorescence powder, the fluorescent material of coating three primary colours or multiple color is same on purple light or ultraviolet leds chip obtains white light.
Know-why of the present invention: general ceramic opaque reason is that its inside has impurity and pore, and the former can absorb light, and the latter makes light produce scattering, so just opaque.If so select high pure raw material for use, and just possibly obtain crystalline ceramics through process means eliminating pore.The doping fluorescent powder sintering can obtain transparent fluorescence ceramics in the transparent ceramic powder, and wherein fluorescent material can excite blue light to produce white light when transparent fluorescence ceramics was used for the blue-ray LED packaging process, thus the instead conventional encapsulant.
Beneficial effect of the present invention: the transparent fluorescence ceramics that makes can be used as the LED packaged material, because transparent fluorescence ceramics, can be shared part heat radiation pressure and the optical efficiency of getting that improves led light source than epoxy resin and higher thermal conductivity and the specific refractory power of organosilicon; Because stupalith has the intensity higher than organic materials, hardness, more corrosion-resistant; Can increase substantially the life-span of LED goods, and for realize that the use that white light LEDs works long hours provides possibility under abominable Working environment such as high temperature, HI high impact, corrodibility.
But transparent fluorescence ceramics double as fluorescence transition material and packaged material have saved coating technique and have avoided gluing homogeneity control problem, and the existing fluorescent powder coating technique flow process of comparing is few, and production technique is simple, cost is lower, help large-scale popularization and use.When the excellent optics of transparent ceramic material, calorifics and mechanical property have been given full play in the application of transparent fluorescence ceramics, significantly improve performance and the work-ing life of LED, with the Application Areas of greatly expanding LED.
Description of drawings:
Fig. 1 is the see through graphic representation of crystalline ceramics at visible light wave range;
Fig. 2 be behind the doping fluorescent powder transparent fluorescence ceramics at the graphic representation that sees through of visible light wave range.
Embodiment
A kind of fluorescent material and crystalline ceramics doping are total to the process method of burning fluorescent material and transparent ceramic powder doping are total to the transparent fluorescence ceramics of burning formation, are divided into non-pressure sintering technology and vacuum heating-press sintering;
Non-pressure sintering technology: compression moulding and sintering process are separately carried out; Earlier with powder coldmoulding; Molding mode is selected a kind of with in cold isostatic compaction and the wet moulding of punching block coldmoulding or shop; Carry out biscuiting afterwards to remove some additives, under vacuum, hydrogen or other inert gas conditions, carry out high temperature sintering again;
Vacuum heating-press sintering: moulding and sintering are accomplished in same operation; It is molded earlier powder to be put into mold cold; Then the moulding sample is put into vacuum hotpressing stove and carry out hot pressed sintering, resulting product is put into and is carried out aftertreatment under hot isostatic pressing furnace high-temperature, the high pressure, interior temperature 1600-1800 ℃ of stove; Argon gas condition overdraft 150-200Mpa, and then the optical property of raising fluorescence crystalline ceramics.
Crystalline ceramics is selected high pure raw material for use, gets rid of pore through process means and obtains.Be exactly to adopt such way to obtain transparent alumina-ceramic in early days, work out successively afterwards like multiple oxide compound series such as sintering white fused alumina, Natural manganese dioxide, beryllium oxide, yttrium oxide, yttrium oxide-ZIRCONIUM DIOXIDE 99.5 crystalline ceramics.Develop Non-oxide Transparent Ceramics in the recent period again, like gallium arsenide, zinc sulphide, zinc selenide, Sellaite, Calcium Fluoride (Fluorspan) etc.
Fluorescent material is allowed a choice according to led chip type and optical property difference; Blue-light excited yellow fluorescent powder mixes the generation white light; Apply on the blue led chip and greenly can obtain high-color rendering white-light with red fluorescence powder, the fluorescent material of coating three primary colours or multiple color is same on purple light or ultraviolet leds chip obtains white light.
The transparent fluorescence ceramics that makes can be used as the LED packaged material, makes it under the blue-light LED chip irradiation, produce white light, thereby has realized luminous and shell integrated outward.
Be illustrated in figure 1 as the see through graphic representation of crystalline ceramics at visible light wave range; From figure, can know that crystalline ceramics transmitance in visible-range is suitable basically; Fig. 2 be behind the doping fluorescent powder transparent fluorescence ceramics at the graphic representation that sees through of visible light wave range, among the figure in the visible crystalline ceramics adulterated fluorescent material after exciting mixing behind the incident light that absorbs blue wave band, can realize the white light function.
Claims (3)
1. fluorescent material and the crystalline ceramics process method of mixing and burning altogether is characterized in that: fluorescent material and transparent ceramic powder are mixed burn the transparent fluorescence ceramics of formation altogether, be divided into non-pressure sintering technology and vacuum heating-press sintering;
Non-pressure sintering technology: compression moulding and sintering process are separately carried out; Earlier with powder coldmoulding; Molding mode is selected a kind of with in cold isostatic compaction and the wet moulding of punching block coldmoulding or shop; Carry out biscuiting afterwards to remove some additives, under vacuum, hydrogen or other inert gas conditions, carry out high temperature sintering again;
Vacuum heating-press sintering: moulding and sintering are accomplished in same operation; It is molded earlier powder to be put into mold cold; Then the moulding sample is put into vacuum hotpressing stove and carry out hot pressed sintering, resulting product is put into and is carried out aftertreatment under hot isostatic pressing furnace high-temperature, the high pressure, interior temperature 1600-1800 ℃ of stove; Argon gas condition overdraft 150-200Mpa, and then the optical property of raising fluorescence crystalline ceramics.
2. the process method that a kind of fluorescent material according to claim 1 and crystalline ceramics mix and burn altogether, it is characterized in that: described crystalline ceramics is selected high pure raw material for use, gets rid of pore through process means and obtains.
3. the process method that a kind of fluorescent material according to claim 1 and crystalline ceramics mix and burn altogether; It is characterized in that: described fluorescent material is allowed a choice according to led chip type and optical property difference; Blue-light excited yellow fluorescent powder mixes the generation white light; Apply on the blue led chip and greenly can obtain high-color rendering white-light with red fluorescence powder, the fluorescent material of coating three primary colours or multiple color is same on purple light or ultraviolet leds chip obtains white light.
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| CN201110157058A CN102320840A (en) | 2011-06-08 | 2011-06-08 | Fluorescent powder and transparent ceramic doping and co-sintering process method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439561A (en) * | 2014-08-14 | 2016-03-30 | 清华大学 | Gadolinium oxysulfide scintillation ceramic preparation method |
| CN106565260A (en) * | 2016-11-01 | 2017-04-19 | 安徽江威精密制造有限公司 | High-hardness fluorescent ceramic base for high-power LED and preparation method thereof |
| CN107162574A (en) * | 2017-07-12 | 2017-09-15 | 福建华清电子材料科技有限公司 | Alumina ceramic material and preparation method thereof |
-
2011
- 2011-06-08 CN CN201110157058A patent/CN102320840A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439561A (en) * | 2014-08-14 | 2016-03-30 | 清华大学 | Gadolinium oxysulfide scintillation ceramic preparation method |
| US9771515B2 (en) | 2014-08-14 | 2017-09-26 | Tsinghua University | Process for the preparation of gadolinium oxysulfide scintillation ceramics |
| CN106565260A (en) * | 2016-11-01 | 2017-04-19 | 安徽江威精密制造有限公司 | High-hardness fluorescent ceramic base for high-power LED and preparation method thereof |
| CN107162574A (en) * | 2017-07-12 | 2017-09-15 | 福建华清电子材料科技有限公司 | Alumina ceramic material and preparation method thereof |
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Application publication date: 20120118 |