CN106380208B - High-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for LED and preparation method thereof - Google Patents
High-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for LED and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED, which comprises the following raw materials in parts by weight: 80-120 parts of silicon nitride; 80-120 parts of aluminum nitride; 2-10 parts of an additive; the additive comprises the following substances in parts by weight: 1-3 parts of magnesium fluoride; 1-3 parts of yttrium fluoride; 1-3 parts of lithium carbonate; the best physical and chemical properties of the ceramic substrate are that the thermal conductivity is 330W/(m.k), the bending strength is 950Mpa, and the Vickers hardness is 20 GPa.
Description
Technical Field
The invention belongs to the field of substrates for LEDs, and particularly relates to a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for LEDs and a preparation method thereof.
Background
As a fourth generation illumination light source, Light Emitting Diodes (LEDs) are gaining attention from all countries in the world due to their advantages of low maintenance cost, long life, good shock resistance, low power consumption, environmental friendliness, etc., and are widely used in indicator lights, display screens, backlights, landscape illuminations, traffic, etc., and have great market potential.
A series of ceramic substrates (such as CN201510334118.2 and the like) for LEDs are applied by Changsha new material science and technology limited company in 2015, various raw materials in the LTCC preparation process are optimized, aluminum nitride, boron nitride, aluminum oxide and beryllium oxide are used as main raw materials, and additives such as a glass sintering aid, copper-aluminum alloy nanoparticles, rare earth oxide, a solvent, a plasticizer, a dispersing agent, a binder and the like are added, so that the physical and chemical properties of the ceramic substrates are further optimized, the thermal conductivity of the ceramic substrates is more than 400W/(m.k), the bending strength is more than 300Mpa, and the dielectric constant is less than 2. Meanwhile, the main raw materials and the additives can be prepared into the ceramic substrate with high conductivity by the conventional LTCC preparation method, the preparation process is simple, the industrialization is facilitated, and in the method, along with the increasing urgent demand of LED illumination, the heat dissipation problem of a high-power LED is emphasized (the LED luminous efficiency is attenuated due to the overhigh temperature); if waste heat generated by the use of the LED cannot be effectively dissipated, the life of the LED is fatally affected. The ceramic heat dissipation substrates which are popular at present comprise 4 types, namely a direct copper-clad ceramic (DBC) substrate, a direct copper-clad substrate (DPC), a high-temperature co-fired multilayer ceramic (HTCC) substrate and a low-temperature co-fired multilayer ceramic (LTCC) substrate. However, how to design an LED ceramic substrate with excellent performance, especially good heat dissipation performance, is a difficult problem in the present research.
The research on the multiphase ceramic substrate for the LED is less, and CN201110299348.1 discloses that the ceramic is one of alumina, aluminum nitride, SiC and SiAlON or the multiphase ceramic among the alumina, the aluminum nitride, the SiC and the SiAlON; there is a lot of research blank on the complex phase ceramic substrate. For ceramic substrates, sintering aids are very important, and CN201510738040.0 discloses a ceramic substrate for heat dissipation of high-power LEDs, wherein a composite sintering aid is used, which comprises, by mass: 40-60% of silicon powder, 5-10% of aluminum powder, 20-30% of kaolin powder and 10-30% of calcium fluoride; CN201510321089.6 discloses a method for producing an aluminum nitride ceramic substrate for LED, which comprises a ternary composite sintering aid, wherein the ternary composite sintering aid is a combination of oxides or a combination of oxides and nitrides such as BN; CN201510188853.7 also discloses a sintering aid of a ternary oxide system, and has no more innovation; CN201310531348.9 discloses a particle dispersion toughening aluminum nitride ceramic substrate and a preparation method thereof, and discloses that a sintering aid is any one or the composition of any more of rare earth metal oxide, weak alkali oxide, rare earth fluoride or weak alkali fluoride; the rare earth metal oxide is Y2O3、Sm2O3、Dy2O3、Yb2O3One or the composition of any more of the above; the weak alkali oxide is one or the composition of any one of CaO, Li2O and BaO; the rare earth metal fluoride is YF3、DyF3、YbF3One or the composition of any more of the above; the weak baseThe metal fluoride being CaF2. In the preparation process, generally, solid sintering or tape casting sintering and other processes are adopted, and the traditional preparation process has certain need of verification on whether the complex phase system is suitable for use.
For a complex phase system, how to obtain a product with high thermal conductivity by optimizing raw materials and a preparation process thereof is a problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the problems, and provides a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED and a preparation method thereof, wherein the high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate comprises the following steps:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
80-120 parts of silicon nitride;
80-120 parts of aluminum nitride;
2-10 parts of an additive;
the additive comprises the following substances in parts by weight:
1-3 parts of magnesium fluoride; 1-3 parts of yttrium fluoride; 1-3 parts of lithium carbonate.
Preferably, the additive consists of the following substances in parts by weight: 2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
As a preference, the first and second liquid crystal compositions are,
the feed comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive; .
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) removing glue, and performing glue removing treatment at 800 ℃ for 1-2 h;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
Preferably, the gel-casting molding is specifically as follows:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 10-15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 10-20min, and demolding to obtain a blank.
Preferably, the mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
Preferably, the sintering process conditions are that the sintering temperature is 1600-1650 ℃, and the heat preservation time is 1-2 h.
In addition to the silicon nitride-aluminum nitride system, the inventive concept of the present invention is also applicable to the silicon nitride-silicon carbide system as well as the silicon nitride-aluminum nitride-silicon carbide system. The specific preparation scheme is as follows:
a high-thermal-conductivity silicon nitride-silicon carbide complex phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
80-150 parts of silicon nitride;
80-150 parts of silicon carbide;
2-15 parts of an additive;
the additive comprises the following substances in parts by weight:
1-4 parts of magnesium fluoride; 1-4 parts of yttrium fluoride; 1-4 parts of lithium carbonate.
Preferably, the additive consists of the following substances in parts by weight: 2 parts of magnesium fluoride; 4 parts of yttrium fluoride; and 1 part of lithium carbonate.
As a preference, the first and second liquid crystal compositions are,
the feed comprises the following raw materials in parts by weight:
120 parts of silicon nitride;
120 parts of silicon carbide;
7 parts of an additive; .
A preparation method of the high-thermal-conductivity silicon nitride-silicon carbide complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, silicon carbide and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) removing glue, and performing glue removing treatment at 700 ℃ for 1-2 h;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-silicon carbide composite ceramic substrate for the LED can be obtained.
Preferably, the gel-casting molding is specifically as follows:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 10-15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 10-20min, and demolding to obtain a blank.
Preferably, the mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
Preferably, the sintering process conditions are that the sintering temperature is 1500-1600 ℃, and the heat preservation time is 1-2 h.
A high-thermal-conductivity silicon nitride-aluminum nitride-silicon carbide composite ceramic substrate for an LED comprises the following raw materials in parts by weight:
80-120 parts of silicon nitride;
80-120 parts of aluminum nitride;
80-120 parts of silicon carbide;
2-10 parts of an additive;
the additive comprises the following substances in parts by weight:
1-5 parts of magnesium fluoride; 1-5 parts of yttrium fluoride; 1-3 parts of lithium carbonate.
Preferably, the additive consists of the following substances in parts by weight: 4 parts of magnesium fluoride; 5 parts of yttrium fluoride; and 1 part of lithium carbonate.
As a preference, the first and second liquid crystal compositions are,
the feed comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
100 parts of silicon carbide;
6 parts of an additive; .
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride-silicon carbide complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride, silicon carbide and an additive according to the proportion;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) removing glue, and performing glue removing treatment at 780 ℃ for 1-2 h;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
Preferably, the gel-casting molding is specifically as follows:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 10-15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 10-20min, and demolding to obtain a blank.
Preferably, the mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
Preferably, the sintering process conditions are that the sintering temperature is 1500-1650 ℃, and the heat preservation time is 1-2 h.
Detailed Description
The present invention is described in further detail below with reference to specific examples and with reference to the data. It will be understood that these examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way.
the silicon nitride used in the embodiment of the invention is α -Si3N4, the specific surface area is 9-13m2/g, the oxygen content is less than 1.5 wt%, the α -Si3N4 purity is more than 97%, the average particle size is 2 μm, the aluminum nitride is 8-12m2/g, the oxygen content is less than 1 wt%, the AlN purity is more than 99%, the average particle size is 2 μm, the silicon carbide is green silicon carbide, the specific surface area is 8-15m2/g, the oxygen content is less than 0.8 wt%, the SiC purity is more than 99%, the average particle size is 2 μm, other raw materials are not particularly mentioned and are analytical pure reagents;
example 1:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate has a thermal conductivity of 330W/(m.k), a bending strength of 950MPa, and a Vickers hardness of 20 GPa.
Example 2:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
80 parts of silicon nitride;
120 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 320W/(m.k), a flexural strength of 900MPa, and a Vickers hardness of 19.5 GPa.
Example 3:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
120 parts of silicon nitride;
80 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 322W/(m.k), a flexural strength of 948MPa, and a Vickers hardness of 19.4 GPa.
Example 4:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
1 part of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 300W/(m.k), a flexural strength of 900MPa, and a Vickers hardness of 17 GPa.
Example 5:
a high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
2 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 310W/(m.k), a flexural strength of 920MPa, and a Vickers hardness of 19.7 GPa.
Example 6
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
10 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 315W/(m.k), a flexural strength of 935MPa, and a Vickers hardness of 19.2 GPa.
Example 7
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
1 part of magnesium fluoride; 1 part of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 324W/(m.k), a flexural strength of 944MPa, and a Vickers hardness of 19.7 GPa.
Example 8
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 2 parts of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 321W/(m.k), a flexural strength of 941MPa, and a Vickers hardness of 19.1 GPa.
Example 9
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1650 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 324W/(m.k), a flexural strength of 949MPa, and a Vickers hardness of 20 GPa.
Example 10
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 2 hours;
the ceramic substrate had a thermal conductivity of 326W/(m.k), a flexural strength of 946MPa, and a Vickers hardness of 20 GPa.
Example 11
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
120 parts of silicon nitride;
120 parts of silicon carbide;
7 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 4 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 700 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1550 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 340W/(m.k), a flexural strength of 965MPa, and a Vickers hardness of 22 GPa.
Example 12
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
100 parts of silicon carbide;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
4 parts of magnesium fluoride; 5 parts of yttrium fluoride; lithium carbonate 1 part
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride-silicon carbide complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride, silicon carbide and an additive according to the proportion;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) removing glue, and performing glue removing treatment for 2h at 780 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1620 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 337W/(m.k), a flexural strength of 959MPa, and a Vickers hardness of 21 GPa.
Comparative example 1
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
200 parts of silicon nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 290W/(m.k), a flexural strength of 900MPa, and a Vickers hardness of 19.2 GPa.
Comparative example 2
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
200 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate had a thermal conductivity of 300W/(m.k), a flexural strength of 850MPa, and a Vickers hardness of 18 GPa.
Comparative example 3
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
a preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding rubber material is obtained;
and injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank.
The mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
when the additive is yttrium oxide, the thermal conductivity of the ceramic substrate is 311W/(m.k), the bending strength is 941MPa, and the Vickers hardness is 18.3 GPa.
When the additive is yttrium fluoride, the thermal conductivity of the ceramic substrate is 318W/(m.k), the bending strength is 942Mpa, and the Vickers hardness is 19.3 GPa.
When the additive is magnesium oxide, the thermal conductivity of the ceramic substrate is 302W/(m.k), the bending strength is 923Mpa, and the Vickers hardness is 18.2 GPa.
When the additive is lithium oxide, the thermal conductivity of the ceramic substrate is 303W/(m.k), the bending strength is 919MPa, and the Vickers hardness is 18.1 GPa.
When the additive is 2 parts of magnesium fluoride; when 3 parts of yttrium fluoride is used, the thermal conductivity of the ceramic substrate is 342W/(m.k), the flexural strength is 944MPa, and the Vickers hardness is 19.8 GPa.
When the additive is 3 parts of yttrium fluoride; when 1 part of lithium carbonate is used, the thermal conductivity of the ceramic substrate is 341W/(m.k), the flexural strength is 941MPa, and the Vickers hardness is 19.1 GPa.
When the additive is 2 parts of magnesium fluoride; when 1 part of lithium carbonate is used, the thermal conductivity of the ceramic substrate is 342W/(m.k), the flexural strength is 942MPa, and the Vickers hardness is 19.2 GPa.
Comparative example 4
A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED comprises the following raw materials in parts by weight:
100 parts of silicon nitride;
100 parts of aluminum nitride;
6 parts of an additive;
the additive comprises the following substances in parts by weight:
2 parts of magnesium fluoride; 3 parts of yttrium fluoride; and 1 part of lithium carbonate.
A preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps:
(1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) molding:
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained.
The sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
performing static pressure forming under the pressure of 20 MPa; the ceramic substrate had a thermal conductivity of 321W/(m.k), a flexural strength of 940MPa, and a Vickers hardness of 19.5 GPa.
Dry pressing and forming under the pressure of 20 MPa; the ceramic substrate had a thermal conductivity of 320W/(m.k), a flexural strength of 933MPa, and a Vickers hardness of 19.1 GPa.
The ceramic substrate is subjected to water-based tape casting, the thermal conductivity of the ceramic substrate is 341W/(m.k), the bending strength is 945Mpa, and the Vickers hardness is 19.6 GPa.
As can be seen from the specific examples and comparative examples, according to the technical scheme of the present invention, by using silicon nitride and aluminum nitride in combination, the thermal conductivity, bending strength and vickers hardness are all improved as compared with the single component, wherein the possible reason is that new silicon aluminum nitride, Si (C, N) and other compounds are formed during the combination process; compared with an oxide system or single magnesium fluoride, yttrium fluoride and lithium carbonate, the additive used in a composite way has a very significant influence on the performance of the ceramic substrate, and probably because magnesium ions and yttrium ions of the magnesium fluoride and the yttrium fluoride enter the complex phase ceramic system, the sintering temperature is reduced, and besides, fluoride ions can form volatilizable silicon fluoride with silicon ions in the system, so that crystal media of the system are broken, the fusion of the system is promoted, and then the particle size of alkali metal of lithium carbonate is small, so that the uniform dispersion of the system is easily promoted in a molten state, and the breaking of crystals is generated by combining gas, so that the crystallization performance of the whole system is better and higher in compactness, and the thermal conductivity and the mechanical property of the system are improved; in the forming process, the use of injection-coagulation forming can ensure that the slurry of the system is dispersed more uniformly, promote the raw materials not only to improve the relative density before sintering, and ensure that the relative density can reach more than 70%; but rather to improve the uniform dispersion of the raw materials, including raw materials and additives. Meanwhile, the sintering gas atmosphere of the invention adopts other reductive hydrogen, so that oxygen in the system can be eliminated to the greatest extent, and the improvement of the thermal conductivity of the system is promoted. Therefore, the technical scheme of the selection and preparation process of the sintering aid plays a synergistic role, the diaphragm between crystal media is broken through the improvement of the dispersibility of the base material, the ceramic material with high density is formed, oxygen and other impurities contained in the ceramic material are few, and the thermal conductivity, the bending strength and the Vickers hardness of the ceramic substrate completely meet the requirements of LED packaging.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (2)
1. A high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for an LED is characterized in that: the feed comprises the following raw materials in parts by weight: 100 parts of silicon nitride; 100 parts of aluminum nitride; 6 parts of an additive; the additive comprises the following substances in parts by weight: 2 parts of magnesium fluoride; 3 parts of yttrium fluoride; 1 part of lithium carbonate;
a preparation method of the high-thermal-conductivity silicon nitride-aluminum nitride complex phase ceramic substrate for the LED comprises the following steps: (1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained;
the gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding slurry is obtained;
injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank body;
the mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate;
the sintering process conditions are that the sintering temperature is 1600 ℃, and the heat preservation time is 1.5 h;
the ceramic substrate has a thermal conductivity of 330W/(m.k), a bending strength of 950MPa, and a Vickers hardness of 20 GPa.
2. The method for preparing the high-thermal-conductivity silicon nitride-aluminum nitride complex-phase ceramic substrate for the LED as claimed in claim 1, is characterized in that:
the method comprises the following steps: (1) proportioning, namely weighing silicon nitride, aluminum nitride and an additive according to a ratio;
(2) mixing materials, namely mixing the raw materials, adding alcohol as a dispersion medium, and performing ball milling and mixing for 10 hours; drying at 50 deg.C for 5 hr, and sieving with 300-400 mesh sieve;
(3) the mixture is subjected to injection-solidification molding,
(4) performing rubber discharge, and performing rubber discharge treatment for 2 hours at 800 ℃;
(5) sintering, wherein the sintering atmosphere is flowing nitrogen and hydrogen composite gas, and the high-thermal-conductivity silicon nitride-aluminum nitride composite ceramic substrate for the LED can be obtained;
the gel-casting molding specifically comprises the following steps:
adding the sieved powder and the mixed solution into a vacuum stirrer, stirring and vacuumizing until the vacuum degree reaches-0.2 MPa, and keeping for 15min to obtain initial slurry;
adding a catalyst into the initial slurry, fully and uniformly stirring under the vacuum condition of-0.2 MPa, adding an initiator, and continuously stirring until the uniformly dispersed molding slurry is obtained;
injecting the formed slurry into a ceramic substrate model, curing for 15min, and demolding to obtain a blank body;
the mixed solution is a mixed aqueous solution of acrylamide, ammonium polymethacrylate and gum arabic;
the catalyst is tetramethylethylenediamine TMEDA;
the initiator is ammonium persulfate;
the sintering process conditions are that the sintering temperature is 1600 ℃ and the heat preservation time is 1.5 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423397A (en) * | 2008-11-20 | 2009-05-06 | 中国科学院上海硅酸盐研究所 | Method for controlling ceramic slurry curing proceeding |
| CN103102156A (en) * | 2011-11-10 | 2013-05-15 | 中国科学院福建物质结构研究所 | Re:YAG transparent ceramic prepared through gel casting molding |
| 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 |
| CN105503199A (en) * | 2015-12-30 | 2016-04-20 | 山东大学 | High-heat conductivity silicon nitride-aluminum nitride composite material and preparation method thereof |
-
2016
- 2016-08-26 CN CN201610738715.6A patent/CN106380208B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423397A (en) * | 2008-11-20 | 2009-05-06 | 中国科学院上海硅酸盐研究所 | Method for controlling ceramic slurry curing proceeding |
| CN103102156A (en) * | 2011-11-10 | 2013-05-15 | 中国科学院福建物质结构研究所 | Re:YAG transparent ceramic prepared through gel casting molding |
| 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 |
| CN105503199A (en) * | 2015-12-30 | 2016-04-20 | 山东大学 | High-heat conductivity silicon nitride-aluminum nitride composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高热导率AlN/Si3N4复合陶瓷材料制备技术及性能研究;张琳;《硕士学位论文》;万方数据库;20141028;全文 * |
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