CN105254285A - Preparation process of ceramic base plate for high-power LED (light emitting diode) heat radiation - Google Patents

Preparation process of ceramic base plate for high-power LED (light emitting diode) heat radiation Download PDF

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Publication number
CN105254285A
CN105254285A CN201510737571.8A CN201510737571A CN105254285A CN 105254285 A CN105254285 A CN 105254285A CN 201510737571 A CN201510737571 A CN 201510737571A CN 105254285 A CN105254285 A CN 105254285A
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China
Prior art keywords
ceramic
sintering
power led
base plate
powder
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Pending
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CN201510737571.8A
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Chinese (zh)
Inventor
左士祥
张宇
王永飞
吕列超
于楼云
杨阳
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Suzhou Zhirui Photoelectric Material Technology Co Ltd
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Suzhou Zhirui Photoelectric Material Technology Co Ltd
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Priority to CN201510737571.8A priority Critical patent/CN105254285A/en
Publication of CN105254285A publication Critical patent/CN105254285A/en
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Abstract

The invention belongs to the technical field of a ceramic base plate, and particularly relates to a preparation process of a ceramic base plate for high-power LED (light emitting diode) heat radiation. The preparation process comprises the following steps of 1, preparing composite sintering auxiliary agents; 2, preparing ceramic slurry; 3, forming ceramics. The preparation process has the following beneficial effects that 1, the heat conduction coefficient of the ceramic base plate is great, the heat-resistant performance is excellent; the bending-resistant intensity is high, and phenomena such as bending and tilting are avoided; 2, a proper sintering method is used, and the proper sintering auxiliary agents are selected, so that the compactness of alumina ceramic sintering bodies is realized, and the heat conductivity of the alumina ceramics is greatly improved; 3, low-melting point phases can be formed by the sintering auxiliary agents, the liquid-phase sintering can be realized, the sintering temperature is lowered, and the blank compactness is promoted; 4, melamine in a recipe can produce aluminum nitride and carbonitride at high temperature, and the hardness and the lustrousness of the surface of the ceramic base plate are improved.

Description

A kind of preparation technology of great power LED cooling ceramic substrate
Technical field
The invention belongs to ceramic substrate technical field, be specifically related to a kind of preparation technology of great power LED cooling ceramic substrate.
Background technology
LED mainly comprises LED chip and Lamp cup, usual LED chip is connected on heat-radiating substrate with LED luminescent wafer is formed to beat gold thread, eutectic or to cover brilliant mode, again LED chip is fixed on the circuit card of system, heat-radiating substrate plays heat radiation, conduction, insulation triple role, existing heat-radiating substrate mainly metal substrate, modal is copper substrate and aluminum substrate, the common feature of these two kinds of substrates is that electroconductibility is fine, but the technology of this kind of metal substrate connection LED luminescent wafer also exists the drawback of poor radiation, poor insulativity.The quality of heat dispersion directly affects the work-ing life of LED, because the light produced when LED luminescent wafer works is not containing ultraviolet and infrared rays, therefore its light can not take away heat, also just mean that most electric energy distributes around wafer with heat, and the junction temperature of LED luminescent wafer is generally between 60-75 DEG C, the heat failing to dissipate in time accumulated that works long hours makes the constant temperature in Lamp cup raise, and then it is luminous to affect LED luminescent wafer, affect LED work-ing life.
Aluminium oxide ceramic substrate, because of the insulating property of its good heat-conductive characteristic, higher physical strength and excellence, becomes the sector application such as semi-conductor, electronics inorganic non-metallic baseplate material the most widely.Ceramics heat-radiating substrate replaces traditional metal substrate, has better thermal conductivity and insulativity having relative conventional metals substrate on mechanical basis concurrently, and then improves light efficiency and the work-ing life of LED.Therefore, aluminium oxide ceramic substrate is applied in high-power and high-luminance LED as insulating radiation substrate, there is boundless application prospect.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of new great power LED cooling ceramic metal substrate.
The technical scheme adopted to realize the object of the invention is: a kind of preparation technology of great power LED cooling ceramic substrate, and its processing step is:
1) preparation of complex sintering aids
By mass percentage, silica flour, aluminium powder, kaolin powder, Calcium Fluoride (Fluorspan) are scattered in dehydrated alcohol, soak 20 minutes; Then in stink cupboard, limit stirring, limit hot blast blow, until dehydrated alcohol is dried completely and obtains mixed powder, i.e. and obtained complex sintering aids;
2) preparation of ceramic size
By mass percentage, the complex sintering aids adding aluminum oxide powder, trimeric cyanamide, Walocel MT 20.000PV, deionized water and step (1) successively obtained carries out wet ball grinding, ball milling 2 ~ 4 hours, making can gel ceramic slurry, carries out vacuum stirring de-bubble to this ceramic size;
3) forming process of ceramics
By step 2) obtained ceramic size by mold bottom press-in die, naturally placed gelation process; Take out ceramic green sheet and carry out drying treatment, put into hot pressing die and be placed in hot pressing furnace and carry out sintering and suppress, then cooling down obtains ceramic substrate.
Wherein, step 1) middle silica flour 40% ~ 60%, aluminium powder 5% ~ 10%, kaolin powder 20% ~ 30%, Calcium Fluoride (Fluorspan) 10% ~ 30%, the mass volume ratio of described silica flour and dehydrated alcohol is 1g:5mL.
Wherein, step 2) in aluminum oxide powder 70% ~ 80%, trimeric cyanamide 3% ~ 8%, Walocel MT 20.000PV 3% ~ 6%, deionized water 6 ~ 10% and complex sintering aids 5% ~ 10%.
Wherein, step 3) in ceramic green sheet adopt at least 2 layer by layer poststack carry out high temperature sintering, sintering temperature is 1280 ~ 1540 DEG C, sintering time 2 ~ 5 hours, and drying treatment temperature is 60 ~ 95 DEG C, 2 ~ 12 hours time of drying.
Preferably, aluminum oxide powder of the present invention be mean particle size 1 ~ 4 μm of microcosmic crystal formation in the form of sheets or short cylinder high-temperature calcination alpha-aluminium oxide powder.
Beneficial effect of the present invention is as follows:
(1) the ceramic substrate thermal conductivity obtained by the present invention is large, and resistance toheat is excellent, and bending strength is high, there is not the phenomenons such as bending, warpage.
(2) the present invention is by adopting suitable sintering method and choosing suitable sintering aid, realizes the densification of Alumina Ceramics Sintering body, substantially increases the thermal conductivity of alumina-ceramic.
(3) sintering aid of the present invention can form the thing phase of low melting point, realizes liquid phase sintering, reduces firing temperature, promotes the densification of base substrate.
(4) trimeric cyanamide in the present invention's formula at high temperature can produce aluminium nitride and carbonitride, adds hardness and the glossiness of ceramic base plate surface.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) preparation of complex sintering aids
Silica flour 40 kilograms, aluminium powder 8 kilograms, kaolin powder 22 kilograms, 30 kilograms, Calcium Fluoride (Fluorspan) are scattered in 200 kilograms of dehydrated alcohols, soak 20 minutes; Then in stink cupboard, limit stirring, limit hot blast blow, until dehydrated alcohol is dried completely and obtains mixed powder, i.e. and obtained complex sintering aids;
2) preparation of ceramic size
The complex sintering aids 10 kilograms adding mean particle size 3.5 μm of sheet microcosmic crystal formation high-temperature calcination alpha-aluminium oxide powders 70 kilograms, trimeric cyanamide 4 kilograms, Walocel MT 20.000PV 6 kilograms, deionized water 10 kilograms and step (1) successively obtained carries out wet ball grinding, ball milling 2 hours, making can gel ceramic slurry, carries out vacuum stirring de-bubble to this ceramic size;
3) forming process of ceramics
By ceramic size obtained for step (2) by mold bottom press-in die, naturally place gelation process; Take out ceramic green sheet under temperature 60 C condition dry 12 hours, then place folded for ceramic body monolithic spreading aluminum oxide powder 2 layers on load bearing boards, put into hot pressing die and be placed in hot pressing furnace sinter 5 hours at 1280 DEG C, last cooling down obtains ceramic substrate.
Embodiment 2
1) preparation of complex sintering aids
Silica flour 60 kilograms, aluminium powder 10 kilograms, kaolin powder 20 kilograms, 10 kilograms, Calcium Fluoride (Fluorspan) are scattered in 300 kilograms of dehydrated alcohols, soak 20 minutes; Then in stink cupboard, limit stirring, limit hot blast blow, until dehydrated alcohol is dried completely and obtains mixed powder, i.e. and obtained complex sintering aids;
2) preparation of ceramic size
The complex sintering aids 8 kilograms adding mean particle size 1.0 μm of short cylinder microcosmic crystal formation high-temperature calcination alpha-aluminium oxide powders 75 kilograms, trimeric cyanamide 8 kilograms, Walocel MT 20.000PV 3 kilograms, deionized water 6 kilograms and step (1) successively obtained carries out wet ball grinding, ball milling 3 hours, making can gel ceramic slurry, carries out vacuum stirring de-bubble to this ceramic size;
3) forming process of ceramics
By ceramic size obtained for step (2) by mold bottom press-in die, naturally place gelation process; Take out ceramic green sheet under temperature 80 DEG C of conditions dry 6 hours, then place folded for ceramic body monolithic spreading aluminum oxide powder 3 layers on load bearing boards, put into hot pressing die and be placed in hot pressing furnace sinter 3 hours at 1400 DEG C, last cooling down obtains ceramic substrate.
Embodiment 3
1) preparation of complex sintering aids
Silica flour 50 kilograms, aluminium powder 5 kilograms, kaolin powder 30 kilograms, 15 kilograms, Calcium Fluoride (Fluorspan) are scattered in 250 kilograms of dehydrated alcohols, soak 20 minutes; Then in stink cupboard, limit stirring, limit hot blast blow, until dehydrated alcohol is dried completely and obtains mixed powder, i.e. and obtained complex sintering aids;
2) preparation of ceramic size
The complex sintering aids 5 kilograms adding mean particle size 4.0 μm of sheet microcosmic crystal formation high-temperature calcination alpha-aluminium oxide powders 80 kilograms, trimeric cyanamide 3 kilograms, Walocel MT 20.000PV 4 kilograms, deionized water 8 kilograms and step (1) successively obtained carries out wet ball grinding, ball milling 4 hours, making can gel ceramic slurry, carries out vacuum stirring de-bubble to this ceramic size;
3) forming process of ceramics
By ceramic size obtained for step (2) by mold bottom press-in die, naturally place gelation process; Take out ceramic green sheet under temperature 95 DEG C of conditions dry 2 hours, then place folded for ceramic body monolithic spreading aluminum oxide powder 5 layers on load bearing boards, put into hot pressing die and be placed in hot pressing furnace sinter 2 hours at 1540 DEG C, last cooling down obtains ceramic substrate.
Detect the ceramic substrate obtained by embodiment 1 ~ 3, performance is as shown in table 1.
Table 1
Embodiment Density Flexural strength Surfaceness Amount of warpage
Embodiment 1 3.7g/cm 3 237MPa 0.6μm <0.2%
Embodiment 2 3.6g/cm 3 242MPa 0.5μm <0.2%
Embodiment 3 3.8/cm 3 254MPa 0.8μm <0.2%

Claims (5)

1. a preparation technology for great power LED cooling ceramic substrate, is characterized in that: comprise the steps:
1) preparation of complex sintering aids
By mass percentage, silica flour, aluminium powder, kaolin powder, Calcium Fluoride (Fluorspan) are scattered in dehydrated alcohol, soak 20 minutes; Then in stink cupboard, limit stirring, limit hot blast blow, until dehydrated alcohol is dried completely and obtains mixed powder, i.e. and obtained complex sintering aids;
2) preparation of ceramic size
By mass percentage, adding aluminum oxide powder, trimeric cyanamide, Walocel MT 20.000PV, deionized water and step 1 successively) obtained complex sintering aids carries out wet ball grinding, ball milling 2 ~ 4 hours, making can gel ceramic slurry, carries out vacuum stirring de-bubble to this ceramic size;
3) forming process of ceramics
By step 2) obtained ceramic size by mold bottom press-in die, naturally placed gelation process; Take out ceramic green sheet and carry out drying treatment, put into hot pressing die and be placed in hot pressing furnace and carry out sintering and suppress, then cooling down obtains ceramic substrate.
2. the preparation technology of a kind of great power LED cooling ceramic substrate according to claim 1, is characterized in that:
Step 1) middle silica flour 40% ~ 60%, aluminium powder 5% ~ 10%, kaolin powder 20% ~ 30%, Calcium Fluoride (Fluorspan) 10% ~ 30%, the mass volume ratio of described silica flour and dehydrated alcohol is 1g:5mL.
3. the preparation technology of a kind of great power LED cooling ceramic substrate according to claim 1, is characterized in that:
Step 2) in aluminum oxide powder 70% ~ 80%, trimeric cyanamide 3% ~ 8%, Walocel MT 20.000PV 3% ~ 6%, deionized water 6 ~ 10% and complex sintering aids 5% ~ 10%.
4. the preparation technology of a kind of great power LED cooling ceramic substrate according to claim 1, is characterized in that:
Step 3) in ceramic green sheet adopt at least 2 layer by layer poststack carry out high temperature sintering, sintering temperature is 1280 ~ 1540 DEG C, sintering time 2 ~ 5 hours, and drying treatment temperature is 60 ~ 95 DEG C, 2 ~ 12 hours time of drying.
5. the preparation technology of a kind of great power LED cooling ceramic substrate according to claim 1, is characterized in that: described aluminum oxide powder be mean particle size 1 ~ 4 μm of microcosmic crystal formation in the form of sheets or short cylinder high-temperature calcination alpha-aluminium oxide powder.
CN201510737571.8A 2015-11-04 2015-11-04 Preparation process of ceramic base plate for high-power LED (light emitting diode) heat radiation Pending CN105254285A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105693223A (en) * 2016-03-09 2016-06-22 苏州皓金石新材料科技有限公司 Electronic ceramic substrate for heat dissipation
CN106348761A (en) * 2016-08-11 2017-01-25 安徽波浪岛游乐设备有限公司 Preparation process of high-thermal-conductivity substrate for LEDs
CN110183217A (en) * 2019-05-31 2019-08-30 绍兴上虞威拓机械电子有限公司 Ultra-high brightness LED ceramic substrate processing technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1769168A (en) * 2005-12-02 2006-05-10 中国科学院物理研究所 Method for synthesizing nitride using metal oxide
CN103360039A (en) * 2013-07-16 2013-10-23 山东工业陶瓷研究设计院有限公司 Large-size sheet-type electric-insulation heat-dissipation ceramic substrate and preparation method thereof
CN103539088A (en) * 2013-11-05 2014-01-29 河北工业大学 Synthetic method of aluminium nitride nanoparticles
CN104987081A (en) * 2015-06-05 2015-10-21 黄勤 Method for preparing aluminum nitride ceramic substrate with composite powder grain shape

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1769168A (en) * 2005-12-02 2006-05-10 中国科学院物理研究所 Method for synthesizing nitride using metal oxide
CN103360039A (en) * 2013-07-16 2013-10-23 山东工业陶瓷研究设计院有限公司 Large-size sheet-type electric-insulation heat-dissipation ceramic substrate and preparation method thereof
CN103539088A (en) * 2013-11-05 2014-01-29 河北工业大学 Synthetic method of aluminium nitride nanoparticles
CN104987081A (en) * 2015-06-05 2015-10-21 黄勤 Method for preparing aluminum nitride ceramic substrate with composite powder grain shape

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105693223A (en) * 2016-03-09 2016-06-22 苏州皓金石新材料科技有限公司 Electronic ceramic substrate for heat dissipation
CN106348761A (en) * 2016-08-11 2017-01-25 安徽波浪岛游乐设备有限公司 Preparation process of high-thermal-conductivity substrate for LEDs
CN110183217A (en) * 2019-05-31 2019-08-30 绍兴上虞威拓机械电子有限公司 Ultra-high brightness LED ceramic substrate processing technology

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