CN106380208A - High-thermal-conductivity silicon nitride-aluminum nitride multiphase ceramic substrate of LED and manufacturing method thereof - Google Patents

High-thermal-conductivity silicon nitride-aluminum nitride multiphase ceramic substrate of LED and manufacturing method thereof Download PDF

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CN106380208A
CN106380208A CN201610738715.6A CN201610738715A CN106380208A CN 106380208 A CN106380208 A CN 106380208A CN 201610738715 A CN201610738715 A CN 201610738715A CN 106380208 A CN106380208 A CN 106380208A
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ceramic substrate
silicon nitride
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thermal conductivity
aluminium nitride
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CN106380208B (en
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刘丽梅
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Guangdong Chuanghui Xinluo Science and Technology Co., Ltd.
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刘丽梅
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Abstract

The present invention discloses a high-thermal-conductivity silicon nitride-aluminum nitride multiphase ceramic substrate of an LED. The high-thermal-conductivity silicon nitride-aluminum nitride multiphase ceramic substrate comprises the following raw materials in parts by weight: 80-120 parts of silicon nitride, 80-120 parts of aluminium nitride, and 2-10 parts of additives. The additives comprise the following raw materials in parts by weight: 1-3 parts of magnesium fluoride, 1-3 parts of yttrium fluoride, and 1-3 parts of lithium carbonate. The optimal physical and chemical properties of the ceramic substrate are as follows: 330 w (m*k) as heat conductivity, 950 Mpa as bending strength and 20 Gpa as vickers hardness.

Description

A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate and its preparation Method
Technical field
The invention belongs to LED uses substrate field, particularly to a kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase pottery Porcelain substrate and preparation method thereof.
Background technology
As forth generation lighting source, light emitting diode (LED) with its maintenance cost low, life-span length, shock resistance are good, power consumption The advantages such as little and environmental friendliness and paid attention to by countries in the world, be widely used in display lamp, display screen, backlight, landscape shine Bright, traffic etc., market potential is huge.
Changsha Ding Cheng new material Science and Technology Ltd. applied for the LED of series with ceramic substrate (such as in 2015 CN201510334118.2 etc.), optimize the various raw materials in LTCC preparation technology, with aluminium nitride, boron nitride, aluminium oxide and oxidation Beryllium, as primary raw material, meanwhile, with the addition of glass sintering auxiliary agent, albronze nano-particle, rare earth oxide, solvent, plasticising The additives such as agent, dispersant and binding agent, optimize the physical and chemical performance of ceramic substrate, the ceramic substrate thermal conductivity of the application further Rate is more than 400W/ (m k), and bending strength is more than 300Mpa, and dielectric constant is less than 2.Meanwhile, by conventional LTCC preparation side Method, you can primary raw material and additive are prepared into the ceramic substrate with high conductance, preparation process is simple, beneficial to industrialization, Also talk about wherein, the demand with LED illumination is increasingly urgent, the heat dissipation problem of great power LED is taken seriously (too high increasingly Temperature can lead to LED luminous efficiency to decay)；If LED cannot effectively be shed using produced used heat, can be to the life-span of LED Cause fatefulue impact.Ceramic heat-dissipating substrate more universal at this stage has 4 kinds:Directly cover copper ceramic wafer (DBC), direct copper plating Substrate (DPC), high temperature co-firing multilayer ceramic substrate (HTCC) and low temperature co-fired multilayer ceramic substrate (LTCC).And how to design one The LED ceramic baseplate planting superior performance especially perfect heat-dissipating is a difficult problem for present research.
LED is less with the research of complex phase ceramic substrate, and disclosing pottery in CN201110299348.1 is aluminium oxide, nitridation Aluminum, one of SiC, SiAlON or the complex phase ceramic between them；With regard to complex phase ceramic substrate research also exist more Research blank.For ceramic substrate, sintering aid is very important, and CN201510738040.0 discloses a kind of big Power LED heat transmission ceramic substrate, wherein adopts complex sintering aids, by mass percentage, including：Silica flour 40%～60%, Aluminium powder 5%～10%, Kaolin powder 20%～30%, calcium fluoride 10%～30%；CN201510321089.6 discloses LED and uses The production method of aluminium nitride ceramic substrate, which includes tri compound sintering aid, wherein the combination for oxide or its With combining of the nitride such as BN；CN201510188853.7 also discloses the sintering aid of ternary oxide system, not more Many innovations；CN201310531348.9 discloses a kind of yttria stabilizator aluminum nitride ceramic substrate and preparation method thereof, and Disclose any one that sintering aid is in rare-earth oxide, weak base oxide, rare earth fluoride or weak base fluoride Or arbitrarily several being combined；Described rare-earth oxide is Y2O3、Sm2O3、Dy2O3、Yb2O3One of or arbitrarily several Compound；Described weak base oxide is one of CaO, Li2O, BaO or arbitrarily several being combined；Described rare earth metal Fluoride is YF3、DyF3、YbF3One of or arbitrarily several compound；Described weak base metal fluoride is CaF2.In system In standby technique it is however generally that, using more, the traditional preparation technology of technique such as solid sintering or curtain coating sintering, for complex phase For system, if suitable use also has certain needs checking.
For the system of complex phase, how to pass through optimizing materials and its preparation technology, to obtain the product of high thermal conductivity It is present problem demanding prompt solution.
Content of the invention
The purpose of the present invention is for the problems referred to above, develops a kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase pottery Porcelain substrate and preparation method thereof：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
Silicon nitride 80-120 part；
Aluminium nitride 80-120 part；
Additive 2-10 part；
Described additive is by following weight portion material composition：
Afluon (Asta) 1-3 part；Yttrium fluoride 1-3 part；Lithium carbonate 1-3 part.
Preferably, described additive is by following weight portion material composition：2 parts of Afluon (Asta)；3 parts of yttrium fluoride；Lithium carbonate 1 Part.
Preferably,
Including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 1-2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Preferably, described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 10-15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 10-20min demoulding obtains base substrate.
Preferably, described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Preferably, sintering process conditions are, sintering temperature is 1600-1650 DEG C, and temperature retention time is 1-2h.
In addition to silicon nitride-aluminium nitride system, the invention thinking of the present invention be also used in silicon nitride-silicon carbide system with And silicon nitride-AlN-SiC system.Specific preparation scheme is as follows：
A kind of LED high thermal conductivity silicon nitride-silicon carbide complex phase ceramic substrate, including following raw material：
Silicon nitride 80-150 part；
Carborundum 80-150 part；
Additive 2-15 part；
Described additive is by following weight portion material composition：
Afluon (Asta) 1-4 part；Yttrium fluoride 1-4 part；Lithium carbonate 1-4 part.
Preferably, described additive is by following weight portion material composition：2 parts of Afluon (Asta)；4 parts of yttrium fluoride；Lithium carbonate 1 Part.
Preferably,
Including following raw material：
120 parts of silicon nitride；
120 parts of carborundum；
7 parts of additive；.
A kind of above-mentioned LED preparation method of high thermal conductivity silicon nitride-silicon carbide complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, carborundum and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 700 DEG C and processes 1-2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Carborundum composite-phase ceramic substrate.
Preferably, described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 10-15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 10-20min demoulding obtains base substrate.
Preferably, described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Preferably, sintering process conditions are, sintering temperature is 1500-1600 DEG C, and temperature retention time is 1-2h.
A kind of LED high thermal conductivity silicon nitride-AlN-SiC complex phase ceramic substrate, including following raw material：
Silicon nitride 80-120 part；
Aluminium nitride 80-120 part；
Carborundum 80-120 part；
Additive 2-10 part；
Described additive is by following weight portion material composition：
Afluon (Asta) 1-5 part；Yttrium fluoride 1-5 part；Lithium carbonate 1-3 part.
Preferably, described additive is by following weight portion material composition：4 parts of Afluon (Asta)；5 parts of yttrium fluoride；Lithium carbonate 1 Part.
Preferably,
Including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
100 parts of carborundum；
6 parts of additive；.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-AlN-SiC complex phase ceramic substrate, including Following steps：
(1) dispensing, weighs silicon nitride, aluminium nitride, carborundum and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 780 DEG C and processes 1-2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Preferably, described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 10-15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 10-20min demoulding obtains base substrate.
Preferably, described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Preferably, sintering process conditions are, sintering temperature is 1500-1650 DEG C, and temperature retention time is 1-2h.
Specific embodiment
With reference to specific embodiment, and with reference to data, the present invention is described in further detail.It should be understood that these embodiments The present invention solely for the purpose of illustration, rather than limit the scope of the present invention by any way.
The silicon nitride that the embodiment of the present invention is used is α-Si3N4, and specific surface area is 9-13m2/g；Oxygen content is less than 1.5wt%, α-Si3N4 purity is more than 97%, and mean diameter is 2 μm；Aluminium nitride is 8-12m2/g for specific surface area；Oxygen content is little In 1wt%, AlN purity is more than 99%, and mean diameter is 2 μm；Carborundum is green silicon carbide, and specific surface area is 8-15m2/g； Oxygen content is less than 0.8wt%, and SiC purity is more than 99%, and mean diameter is 2 μm；Other raw materials are not particularly addressed, are analysis pure Reagent；
Embodiment 1：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, until vacuum reaches Arrive -0.2MPa, keep 15min, obtain initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 330W/ (m k), and bending strength is 950Mpa, and Vickers hardness is 20GPa.
Embodiment 2：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
80 parts of silicon nitride；
120 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 320W/ (m k), and bending strength is 900Mpa, and Vickers hardness is 19.5GPa.
Embodiment 3：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
120 parts of silicon nitride；
80 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 322W/ (m k), and bending strength is 948Mpa, and Vickers hardness is 19.4GPa.
Embodiment 4：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
1 part of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 300W/ (m k), and bending strength is 900Mpa, and Vickers hardness is 17GPa.
Embodiment 5：
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
2 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 310W/ (m k), and bending strength is 920Mpa, and Vickers hardness is 19.7GPa.
Embodiment 6
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
10 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 315W/ (m k), and bending strength is 935Mpa, and Vickers hardness is 19.2GPa.
Embodiment 7
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
1 part of Afluon (Asta)；1 part of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 324W/ (m k), and bending strength is 944Mpa, and Vickers hardness is 19.7GPa.
Embodiment 8
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；2 parts of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 321W/ (m k), and bending strength is 941Mpa, and Vickers hardness is 19.1GPa.
Embodiment 9
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1650 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 324W/ (m k), and bending strength is 949Mpa, and Vickers hardness is 20GPa.
Embodiment 10
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 2h；
This ceramic substrate thermal conductivity is 326W/ (m k), and bending strength is 946Mpa, and Vickers hardness is 20GPa.
Embodiment 11
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
120 parts of silicon nitride；
120 parts of carborundum；
7 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；4 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 700 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1550 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 340W/ (m k), and bending strength is 965Mpa, and Vickers hardness is 22GPa.
Embodiment 12
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
100 parts of carborundum；
6 parts of additive；
Described additive is by following weight portion material composition：
4 parts of Afluon (Asta)；5 parts of yttrium fluoride；1 part of lithium carbonate
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-AlN-SiC complex phase ceramic substrate, including Following steps：
(1) dispensing, weighs silicon nitride, aluminium nitride, carborundum and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 780 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1620 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 337W/ (m k), and bending strength is 959Mpa, and Vickers hardness is 21GPa.
Comparative example 1
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
200 parts of silicon nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 290W/ (m k), and bending strength is 900Mpa, and Vickers hardness is 19.2GPa.
Comparative example 2
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
200 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
This ceramic substrate thermal conductivity is 300W/ (m k), and bending strength is 850Mpa, and Vickers hardness is 18GPa.
Comparative example 3
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiation Agent, continues to be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 15min demoulding obtains base substrate.
Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
When additive is for yittrium oxide, this ceramic substrate thermal conductivity is 311W/ (m k), and bending strength is 941Mpa, dimension Family name's hardness is 18.3GPa.
When additive is for yttrium fluoride, this ceramic substrate thermal conductivity is 318W/ (m k), and bending strength is 942Mpa, dimension Family name's hardness is 19.3GPa.
When additive is for magnesium oxide, this ceramic substrate thermal conductivity is 302W/ (m k), and bending strength is 923Mpa, dimension Family name's hardness is 18.2GPa.
When additive is for lithium oxide, this ceramic substrate thermal conductivity is 303W/ (m k), and bending strength is 919Mpa, dimension Family name's hardness is 18.1GPa.
When additive is 2 parts of Afluon (Asta)；During 3 parts of yttrium fluoride, this ceramic substrate thermal conductivity is 342W/ (m k), and bending is strong Spend for 944Mpa, Vickers hardness is 19.8GPa.
When additive is 3 parts of yttrium fluoride；During 1 part of lithium carbonate, this ceramic substrate thermal conductivity is 341W/ (m k), and bending is strong Spend for 941Mpa, Vickers hardness is 19.1GPa.
When additive is 2 parts of Afluon (Asta)；During 1 part of lithium carbonate, this ceramic substrate thermal conductivity is 342W/ (m k), and bending is strong Spend for 942Mpa, Vickers hardness is 19.2GPa.
Comparative example 4
A kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；
Described additive is by following weight portion material composition：
2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
A kind of preparation method of above-mentioned LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, walks including following Suddenly：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently it is dried at 50 DEG C 5h, crosses 300-400 mesh sieve；
(3) molding：
(4) dumping, carries out dumping at 800 DEG C and processes 2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can acquisition LED high thermal conductivity silicon nitride- Aluminium nitride complex phase ceramic substrate.
Sintering process conditions are that sintering temperature is 1600 DEG C, and temperature retention time is 1.5h；
Hydrostatic profile, when pressure is 20MPa；This ceramic substrate thermal conductivity is 321W/ (m k), and bending strength is 940Mpa, Vickers hardness is 19.5GPa.
Dry-pressing formed, when pressure is 20MPa；This ceramic substrate thermal conductivity is 320W/ (m k), and bending strength is 933Mpa, Vickers hardness is 19.1GPa.
Aqueous tape casting forming, this ceramic substrate thermal conductivity is 341W/ (m k), and bending strength is 945Mpa, Vickers hardness For 19.6GPa.
Can be seen that for technical scheme from specific embodiment and comparative example, by by silicon nitride and nitridation Aluminum compound use, compared to one-component, its thermal conductivity, bending strength and Vickers hardness are obtained for raising, wherein may The reason be in recombination process, define new aluminium silicon nitride, the compound such as Si (C, N)；And in the selection of additive, add Plus the content of agent also has significant impact for the performance of ceramic substrate, compared to oxide system, or single Afluon (Asta), fluorine Change yttrium and lithium carbonate, the additive of compound use is also highly significant for the impact of ceramic substrate performance, this be probably by Enter complex phase ceramic system in Afluon (Asta) and yttrium fluoride except magnesium and ruthenium ion, reduce outside sintering temperature, fluorion is likely to Form volatilizable silicon fluoride with the silicon ion in system, then break brilliant Jie of system, the fusion of promotion system, then pass through carbon The alkali-metal particle diameter of sour lithium little it is easy to the homogeneous dispersion of promotion system in the molten state, bound gas produce and are situated between for brilliant Break so that the crystal property of whole system more preferably, consistency is higher, improves thermal conductivity and the mechanical property of system；And On moulding process, the use of note solidification forming, so that the slurry of system disperses evenly, also promotion raw material is not before sintering Only improve relative density, relative density can reach more than 70%；But improve raw material dispersed, include raw material with Additive.Meanwhile, the sintering atmosphere of the present invention, due to additionally using other hydrogen of reproducibility, can use up the degree of maximum Come the oxygen in elimination system, the raising of the thermal conductivity of promotion system.It can be seen that, the selection of the sintering aid in the present invention, preparation work Technical scheme in skill is to play synergistic, by improving the dispersibility of base material, breaks the barrier film between brilliant Jie, is formed and cause The high ceramic material of density, the impurity such as its oxygen containing is few, and the thermal conductivity of ceramic substrate, bending strength and Vickers hardness are complete The demand of full up sufficient LED encapsulation.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit requires rather than described above limits, it is intended that by the institute in the implication and scope of the equivalency of claim that falls Change and include in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment only wraps Containing an independent technical scheme, only for clarity, those skilled in the art should for this narrating mode of description Using description as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined Understandable other embodiment.

Claims (7)

1. a kind of LED high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate it is characterised in that：Former including following weight portion Material：
Silicon nitride 80-120 part；
Aluminium nitride 80-120 part；
Additive 2-10 part；
Described additive is by following weight portion material composition：
Afluon (Asta) 1-3 part；Yttrium fluoride 1-3 part；Lithium carbonate 1-3 part.
2. a kind of LED as claimed in claim 1 high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate it is characterised in that： Described additive is by following weight portion material composition：2 parts of Afluon (Asta)；3 parts of yttrium fluoride；1 part of lithium carbonate.
3. a kind of LED as claimed in claim 1 high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate it is characterised in that：
Including following raw material：
100 parts of silicon nitride；
100 parts of aluminium nitride；
6 parts of additive；.
4. the system of the high thermal conductivity silicon nitride of the LED as described in a kind of any one as claim 1-3-aluminium nitride complex phase ceramic substrate Preparation Method it is characterised in that：Comprise the steps：
(1) dispensing, weighs silicon nitride, aluminium nitride and additive according to proportioning；
(2) batch mixing, raw material is mixed, and adds ethanol as disperse medium, ball milling mixing 10h；Subsequently 5h, mistake are dried at 50 DEG C 300-400 mesh sieve；
(3) note solidification forming,
(4) dumping, carries out dumping at 800 DEG C and processes 1-2h；
(5) sinter, sintering atmosphere is flowing nitrogen, hydrogen composite gas, you can obtain LED high thermal conductivity silicon nitride-nitridation Aluminum complex phase ceramic substrate.
5. the preparation method of a kind of LED as claimed in claim 4 high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, It is characterized in that：Described note solidification forming is specially：
Powder after sieving and mixed liquor are added in de-airing mixer, evacuation while stirring, reach until vacuum- 0.2MPa, keeps 10-15min, obtains initial slurry；
Add catalyst in initial slurry, stir under the vacuum condition of -0.2MPa, add initiator, continue Continue and be stirred until homogeneous scattered molding sizing material；
Molding slurry is injected in ceramic substrate model, the solidification 10-20min demoulding obtains base substrate.
6. the preparation method of a kind of LED as claimed in claim 5 high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate, It is characterized in that：Described mixed liquor is acrylamide, ammonium polymethacrylate and Radix Acaciae senegalis mixed aqueous solution；
Catalyst is tetramethylethylenediamine TMEDA；
Initiator is Ammonium persulfate..
7. the preparation side of a kind of LED as described in claim 5 or 6 high thermal conductivity silicon nitride-aluminium nitride complex phase ceramic substrate Method it is characterised in that：Sintering process conditions are that sintering temperature is 1600-1650 DEG C, and temperature retention time is 1-2h.
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