CN102509752B - Preparation method of a multi-chip set large-power LED substrate - Google Patents
Preparation method of a multi-chip set large-power LED substrate Download PDFInfo
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Abstract
The invention relates to a preparation method of a multi-chip set large-power LED substrate, belongs to the preparation method of the LED substrate. The preparation method solves the problems of the existing LED device that: the thermal expansion coefficient in the LED metal encapsulation does not match the semiconductor material, and the thermal conductivity of a polymer insulation layer is relatively low, so as to result into LED failure. Polycarbosilane, aluminum nitride powder and yttrium oxide are used as the raw material and ball-milled and mixed with dimethylbenzene or tetrahydrofuran in an agate ball-milling jar, so as to obtain a mixed pulp and then the mixed pulp is suspendedly coated on a clean tungsten-copper alloy surface and then dried. The tungsten-copper alloy surface coated with the mixed pulp is arranged on the surface of a copper sheet and heated in a vacuum tube type furnace and then cooled to the room temperature, thus the multi-chip set large-power LED substrate is obtained. The multi-chip set large-power LED substrate has features of high insulation performance, high thermal conductivity, match between the thermal expansion coefficient and the semiconductor material and simplified LED encapsulation structure. The preparation method is suitable for the multi-chip set large-power LED substrate.
Description
Technical field
The present invention relates to LED base plate preparation method.
Background technology
The advantages such as that LED lighting source has is efficient, energy-conservation, long service life, in energy-intensive today, research LED illumination has far-reaching strategic importance.At present, due to LED power limited, adopt single-chip package can not produce enough luminous fluxes and meet the requirement of people to display and lighting.By a plurality of chips (more than 6) connection in series-parallel, be one group, and be encapsulated as device, become a kind of trend of LED device development.Single led chip nearly 20% electric energy conversion is luminous energy, and nearly 80% electric energy conversion is heat, and namely, multi-chip package device quantity of heat production can increase.Heat concentrates in small-sized chip and cannot scatter and disappear, and can reduce device performance, and faster devices is aging.For the effective of heat scattered and disappeared, in high-power (more than 1w) LED device, mainly take metal substrate, but because thermal expansion metal coefficient is larger, make LED device in use produce larger thermal stress, very large on device performance impact; Metal substrate insulating barrier is generally macromolecular material simultaneously, and thermal conductivity is lower, has restricted the heat dispersion of metal substrate.The ceramic-metal substrate package that the ceramic coating of take is insulating barrier, because it can simplify high-power LED encapsulation structure, can also reduce costs simultaneously, becomes a general orientation of following big power LED packaging ceramic base plate development.
Summary of the invention
The present invention is that in order to solve, existing LED substrate thermal coefficient of expansion in LED metallic packaging does not mate, the thermal conductivity of polymeric dielectric layer is lower, thereby cause the poor problem of LED substrate heat dispersion, thereby a kind of multi-chip group high power LED substrate preparation method is provided.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride A1N, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues, after 2h～6h, to obtain mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then, with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
Step 5, the tungsten-copper alloy substrate being carried by copper sheet that step 4 is obtained take out naturally cool to room temperature in vacuum tube furnace after, and remove copper sheet, obtain multi-chip group high power LED substrate.
In step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, remove copper sheet, obtain multi-chip group high power LED substrate.
In step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the secondary heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
In step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
In step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
Multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
Beneficial effect: the multi-chip group high power LED substrate that adopts method of the present invention to prepare, the insulation property of its insulating barrier are high, thermal conductivity is high, and thermal coefficient of expansion mates with semi-conducting material, LED substrate perfect heat-dissipating, and effectively simplified LED encapsulating structure.
Embodiment
Embodiment one, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues, after 2h～6h, to obtain mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then, with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
Step 5, the tungsten-copper alloy substrate being carried by copper sheet that step 4 is obtained take out naturally cool to room temperature in vacuum tube furnace after, and remove copper sheet, obtain multi-chip group high power LED substrate.
The difference of multi-chip group high power LED substrate preparation method described in embodiment two, this embodiment and embodiment one is, in step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Embodiment three, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, remove copper sheet, obtain multi-chip group high power LED substrate.
The difference of multi-chip group high power LED substrate preparation method described in embodiment four, this embodiment and embodiment three is, in step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Embodiment five, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
The difference of multi-chip group high power LED substrate preparation method described in embodiment six, this embodiment and embodiment five is, in step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Embodiment seven, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
The difference of multi-chip group high power LED substrate preparation method described in embodiment eight, this embodiment and embodiment seven is, in step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
Embodiment nine, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
Embodiment ten, multi-chip group high power LED substrate preparation method, it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
The coating that the present invention prepares multi-chip group high power LED substrate is the AlN/Al2O3 complex phase ceramic coating through atmosphere heat treatment, it has mainly passed through the prefabricated coating of following Main Stage: PCS/AlN and has heat-treated in process containing a small amount of oxygen atmosphere condition, may occur suc as formula the chemical reaction shown in (1)～formula (4).Polycarbosilane is owing to being unsettled amorphous substance through Low Temperature Thermal cleavage stages product, and carbon wherein also plays pendulum, and oxidized containing meeting under the atmospheric condition of aerobic, element silicon also can exist with the form of silica simultaneously; The oxidized generation gas of carbon makes material system not have free carbon crystallization through high temperature sintering, does not exist free carbon namely to guarantee the electrical insulation capability of ceramic coating; Meanwhile, the silica of generation can be used as the preparation of follow-up complex phase ceramic sintering and supplies raw materials.Oxidized aluminum nitride is a very complicated process, in room temperature, just can carry out, and the reaction of generating polynomial 4, generates aluminium oxide; Aluminium oxide reacts with silica the preparation that realizes complex phase ceramic coating under certain condition.
2C(s)+O
2(g)→CO(g) (1)
C(s)+O
2(g)→CO
2(g) (2)
Si(s)+O
2(g)→SO
2(s) (3)
Claims (10)
1. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues, after 2h～6h, to obtain mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then, with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
Step 5, the tungsten-copper alloy substrate being carried by copper sheet that step 4 is obtained take out naturally cool to room temperature in vacuum tube furnace after, and remove copper sheet, obtain multi-chip group high power LED substrate.
2. multi-chip group high power LED substrate preparation method according to claim 1, it is characterized in that, in step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
3. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, remove copper sheet, obtain multi-chip group high power LED substrate.
4. multi-chip group high power LED substrate preparation method according to claim 3, it is characterized in that in step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
5. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h, again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
6. multi-chip group high power LED substrate preparation method according to claim 5, it is characterized in that in step 1, measuring mass percent and be 35%～55% Polycarbosilane PCS and mass fraction ratio is 45%～65% aluminium nitride AlN, and puts into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
7. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with on tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
8. multi-chip group high power LED substrate preparation method according to claim 7, it is characterized in that in step 1, measure mass percent and be 35%～55% Polycarbosilane PCS, mass fraction than be 42%～61% aluminium nitride AlN and mass fraction than the yittrium oxide that is 3%～4%, and put into agate jar; The Ball-milling Time that ball milling in step 2 mixes is 3h～5h; Be 6h～9h the drying time in step 3; Purity to the nitrogen being filled with in vacuum tube furnace in step 4 is 99.5%.
9. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be that 30%～60% Polycarbosilane PCS and mass fraction ratio are 40%～70% aluminium nitride AlN, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After the copper sheet of the tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
10. multi-chip group high power LED substrate preparation method, is characterized in that: it is realized by following steps:
Step 1, to measure mass percent be 30%～60% Polycarbosilane PCS, mass fraction than being that 35%～65% aluminium nitride AlN and mass fraction are than the yittrium oxide Y that is 2%～5%
2o
3, and put into agate jar;
Step 2, in agate jar, splash into dimethylbenzene or oxolane, and carry out ball milling mixing under the condition that adopts planetary ball mill to be 20r/s～30r/s at rotating speed, described ball milling mixes and continues 2h～6h, obtains mixed slurry;
Step 3, the mixed slurry that step 2 is obtained are coated with at tungsten-copper alloy substrate surface, and are at room temperature dried 5h～10h, obtain the tungsten-copper alloy substrate with preset coating;
Step 4, the tungsten-copper alloy substrate with preset coating that step 3 is obtained are placed on the copper sheet surface that thickness is 0.4mm～0.6mm, and send in vacuum tube furnace and heat-treat; Described heat treated process is: to being filled with purity in vacuum tube furnace, be 98.5%～99.9% nitrogen, then with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 400 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 800 of vacuum tube furnace ℃, and be incubated 1h～2h; Again with the heating rate of 1 ℃/min～5 ℃/min by the temperature increase to 1100 of vacuum tube furnace ℃～1400 ℃, and be incubated 1h～2h, and then drop to 500 ℃ with the rate of temperature fall of 2～3 ℃/min, obtain the tungsten-copper alloy substrate after the heat treatment of being carried by copper sheet;
After tungsten-copper alloy substrate after step 5, the heat treatment of being carried by copper sheet that step 4 is obtained naturally cools to room temperature in vacuum tube furnace, take out, and remove copper sheet, obtain multi-chip group high power LED substrate.
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| CN104372192A (en) * | 2014-10-30 | 2015-02-25 | 苏州莱特复合材料有限公司 | Nano tungsten-copper composite material and preparation method thereof |
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