CN102153348A - Method for sintering fluorescent powder and transparent ceramic together - Google Patents
Method for sintering fluorescent powder and transparent ceramic together Download PDFInfo
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- CN102153348A CN102153348A CN201010585803XA CN201010585803A CN102153348A CN 102153348 A CN102153348 A CN 102153348A CN 201010585803X A CN201010585803X A CN 201010585803XA CN 201010585803 A CN201010585803 A CN 201010585803A CN 102153348 A CN102153348 A CN 102153348A
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Abstract
The invention discloses a method for sintering fluorescent powder and transparent ceramic together. The fluorescent powder and the transparent ceramic powder are doped and sintered together to form transparent fluorescent ceramic, and the method comprises a pressure-free sintering process and a vacuum hot pressing sintering process; the pressure-free sintering process comprises the following steps of: separating a pressing molding process and a sintering process, namely performing cold pressing molding on the powder, then performing bisque firing to remove certain additives, and performing high-temperature sintering under the condition of vacuum, hydrogen or other inert gas; and the vacuum hot pressing sintering process comprises the following steps of: finishing molding and sintering in the same process, namely putting the powder into a mold to perform cold pressing molding, then putting the molded sample into a vacuum hot pressing furnace to perform hot pressing sintering, and putting the obtained product into a hot isostatic pressing furnace to perform post treatment at a high temperature under high pressure so as to improve the optical performance of the transparent fluorescent ceramic. The transparent fluorescent ceramic prepared by the method is used for blue light emitting diode (LED) encapsulation and used as a fluorescent conversion material and an encapsulation material, has excellent optical, thermal and mechanical properties compared with the traditional encapsulation material, and can remarkably 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 processing method of a kind of fluorescent material and crystalline ceramics co-sintering 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 Resins, epoxy 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 Resins, epoxy self exists, easily aging, poor heat resistance, high temperature and short wavelength light have exposed according to defective such as easy to change down, Resins, epoxy 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 Resins, epoxy exists, organosilicon material has been subjected to 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 Resins, epoxy, the ability of working under severe environment such as high temperature, highly corrosive 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 processing method of a kind of fluorescent material and crystalline ceramics co-sintering is used for the LED encapsulation definitely.
The present invention for the technical scheme that solves its technical problem and adopt is:
The processing method of a kind of fluorescent material and crystalline ceramics co-sintering is burnt the transparent fluorescence ceramics of formation altogether with fluorescent material and transparent ceramic powder doping, is 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 finished 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 by process means and obtains.
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 may obtain crystalline ceramics by 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, thereby can replace 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 the optical efficiency of getting of part heat radiation pressure and raising led light source than Resins, epoxy 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 optics, calorifics of transparent ceramic material excellence 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, will greatly expand the Application Areas of 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
The processing method of a kind of fluorescent material and crystalline ceramics co-sintering is burnt the transparent fluorescence ceramics of formation altogether with fluorescent material and transparent ceramic powder doping, is 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 finished 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 by process means and obtains.Be exactly to adopt such way to obtain transparent alumina-ceramic in early days, work out successively afterwards as multiple oxide compound series such as sintering white fused alumina, magnesium oxide, beryllium oxide, yttrium oxide, yttrium oxide-zirconium dioxide crystalline ceramics.Develop Non-oxide Transparent Ceramics in the recent period again, as gallium arsenide, zinc sulphide, zinc selenide, magnesium fluoride, Calcium Fluoride (Fluorspan) etc.
The transparent fluorescence ceramics that makes can be used as the LED packaged material, makes it produce white light under the blue-light LED chip irradiation, 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, crystalline ceramics transmitance in visible-range is suitable substantially as we know from the figure, 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 (2)
1. the processing method of fluorescent material and crystalline ceramics co-sintering is characterized in that: fluorescent material and transparent ceramic powder are mixed to burn altogether forms transparent fluorescence ceramics, is 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 finished 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 processing method of a kind of fluorescent material according to claim 1 and crystalline ceramics co-sintering is characterized in that: described crystalline ceramics is selected high pure raw material for use, gets rid of pore by process means and obtains.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718492A (en) * | 2012-05-21 | 2012-10-10 | 苏州晶品光电科技有限公司 | Method for producing transparent ceramic fluorescence substrate used for LED |
| CN102723424A (en) * | 2012-05-25 | 2012-10-10 | 苏州晶品光电科技有限公司 | Method for preparing fluorescent wafer for LED (light-emitting diode) |
| CN107200588A (en) * | 2016-03-18 | 2017-09-26 | 深圳市绎立锐光科技开发有限公司 | A kind of preparation method and fluorescence associated ceramics of the fluorescence ceramics of aluminium nitride matrix |
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| CN101629077A (en) * | 2009-08-14 | 2010-01-20 | 上海芯光科技有限公司 | Multi-component oxynitride or nitride base fluorescent powder and preparation method thereof |
| CN101665695A (en) * | 2009-09-25 | 2010-03-10 | 上海大学 | Preparation method of Pr<3+> doped (Yx La (1-x)) 2 O3 luminescent material |
| CN101665696A (en) * | 2009-09-25 | 2010-03-10 | 上海大学 | Preparation method of Eu<3+> doped yttrium lanthanum oxide fluorescent powder and transparent scintillating ceramic |
| CN101697367A (en) * | 2009-09-30 | 2010-04-21 | 烁光特晶科技有限公司 | Method for preparing LED by using transparent ceramics |
| CN101899301A (en) * | 2010-06-25 | 2010-12-01 | 海洋王照明科技股份有限公司 | LED light-emitting material, LED light-emitting device and manufacturing method |
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Patent Citations (5)
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| CN101629077A (en) * | 2009-08-14 | 2010-01-20 | 上海芯光科技有限公司 | Multi-component oxynitride or nitride base fluorescent powder and preparation method thereof |
| CN101665695A (en) * | 2009-09-25 | 2010-03-10 | 上海大学 | Preparation method of Pr<3+> doped (Yx La (1-x)) 2 O3 luminescent material |
| CN101665696A (en) * | 2009-09-25 | 2010-03-10 | 上海大学 | Preparation method of Eu<3+> doped yttrium lanthanum oxide fluorescent powder and transparent scintillating ceramic |
| CN101697367A (en) * | 2009-09-30 | 2010-04-21 | 烁光特晶科技有限公司 | Method for preparing LED by using transparent ceramics |
| CN101899301A (en) * | 2010-06-25 | 2010-12-01 | 海洋王照明科技股份有限公司 | LED light-emitting material, LED light-emitting device and manufacturing method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718492A (en) * | 2012-05-21 | 2012-10-10 | 苏州晶品光电科技有限公司 | Method for producing transparent ceramic fluorescence substrate used for LED |
| CN102723424A (en) * | 2012-05-25 | 2012-10-10 | 苏州晶品光电科技有限公司 | Method for preparing fluorescent wafer for LED (light-emitting diode) |
| CN102723424B (en) * | 2012-05-25 | 2015-01-21 | 苏州晶品光电科技有限公司 | Method for preparing fluorescent wafer for LED (light-emitting diode) |
| CN107200588A (en) * | 2016-03-18 | 2017-09-26 | 深圳市绎立锐光科技开发有限公司 | A kind of preparation method and fluorescence associated ceramics of the fluorescence ceramics of aluminium nitride matrix |
| CN107200588B (en) * | 2016-03-18 | 2020-10-20 | 深圳光峰科技股份有限公司 | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic |
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Assignee: Jiangsu Yangtze Electromechanical Science & Technology Co.,Ltd. Assignor: Huang Jinlu Contract record no.: 2012320000247 Denomination of invention: Method for sintering fluorescent powder and transparent ceramic together License type: Exclusive License Open date: 20110817 Record date: 20120319 |
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Application publication date: 20110817 |