CN106566409A - AlN radiator surface radiating composite coating material for LED and preparing method of AlN radiator surface radiating composite coating material - Google Patents

AlN radiator surface radiating composite coating material for LED and preparing method of AlN radiator surface radiating composite coating material Download PDF

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CN106566409A
CN106566409A CN201610976764.3A CN201610976764A CN106566409A CN 106566409 A CN106566409 A CN 106566409A CN 201610976764 A CN201610976764 A CN 201610976764A CN 106566409 A CN106566409 A CN 106566409A
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aln
led
composite coating
radiator surface
surface radiating
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张先兵
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Tongling Zhongrui Electronic Technology Co Ltd
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Tongling Zhongrui Electronic Technology Co Ltd
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Abstract

The invention discloses an AlN radiator surface radiating composite coating material for an LED and a preparing process of the AlN radiator surface radiating composite coating material for the LED. The AlN radiator surface radiating composite coating material and the preparing process are characterized in that SiC, aluminium powder, SiO2, Y2O3, a silane coupling agent A1100, montmorillonoid, a curing agent, an antifoaming agent, epoxy resin 828, AIN, polyvinyl butyral, stearic acid, Ag particles, simethicone, graphene, polymethyl triethoxy silane (PTS), dibutyltin dilaurate, a multiwalled carbon nanotube, 2,4-imidazole, nano graphite, polyvinylpyrrolidone and the like serve as raw materials. According to the AlN radiator surface radiating composite coating material and the preparing process, the Y2O3 is added into the AlN powder to prepare AlN ceramic with higher heat conductivity; heat conduction silicone grease prepared with the dimethicone as base oil and the Ag particles as a reinforcing filler has higher thermal conductivity, treatment with the stearic acid can improve the heat-conducting property of silicone grease, and the prepared heat conduction silicone grease can be used for LED radiating; and the AlN radiator surface radiating composite coating material for the LED is obtained.

Description

A kind of LED AlN radiator surface radiating composite coating materials and preparation method thereof
Technical field
The present invention relates to field of compound material, and in particular to a kind of LED AlN radiator surface radiating composite coating materials Material, and its preparation technology.
Background technology
LED has the advantages that small volume, life-span length, low-carbon environment-friendly, energy-conservation are stable as a kind of excellent photoelectric device, It is expected that preferably general illumination light source of new generation will be become in following several years.As LED develops to high light intensity, high power, Its heat dissipation problem is outstanding day by day, has had a strong impact on light output characteristic and the life-span of device of LED, it has also become high-power LED encapsulation must The key issue that need to be solved.
Li Qiaomei is in its master thesis《Conductive particles sinter the shadow with composite orientation to great power LED cooling Ring》In, based on epoxy resin, respectively with SiO2, SiC be conductive particles, be prepared at high proportion conductive particles potsherd and Orientating type Polymer Composites with High Thermal Conductivity, is surface-treated with silane coupler to heat conduction particle, with aluminium powder, Y2O3、 MgO is used as agglutinant, Jing high-pressure moldings, 660 DEG C of sintering in high temperature furnace.The SiO of selection2With aluminium powder conductive particles, heat conduction system Number is not high, and the present invention have chosen the very high conductive particles of AlN heat conductivitys, can preferably improve the radiating of LED.
The present invention adds Y in AlN powder body2O3Prepare the AlN ceramic with higher heat-conductivity；With dimethicone as base Plinth oil, has higher heat-conductivity using Ag microgranules as heat-conducting silicone grease prepared by reinforcer, and with Hard Fat acid treatment silicone grease can be improved Heat conductivility, the heat-conducting silicone grease of preparation can be used for LED radiatings；Pass through chemical modification with poly- MTES (PTS) Method, be successfully prepared modifying epoxy resin by organosilicon；It is prepared for AlN- carbon nano tube/epoxy resin composite materials；This It is bright to be prepared for for the surface heat conduction of LED radiators and high heat loss through radiation composite coating material；Obtain a kind of LED AlN radiators Surface radiating composite coating material.
The content of the invention
The invention mainly solves the technical problem of providing a kind of LED AlN radiator surface radiating composite coating materials And its preparation technology, the thermal conductivity of composite materials made according to the technique is high, corrosion resistance is good, high-temperature stability is good, hard Degree is high, can preferably improve the radiating of LED.
The technical problem to be solved is realized using following technical scheme：
SiC 10-12, aluminium powder 5-8, SiO25-13, Y2O35-8, the 0.5-1.5 of silane coupling A 1100, montmorillonite 3-6, solidification Agent 1-4, emulsified silicone oil 1-2, the 2-5 of epoxy resin 828, AlN 3-4, polyvinyl butyral resin 1-2, stearic acid 1-2, Ag microgranules 1-3, dimethicone 1-2, Graphene 1-4, poly- MTES (PTS) 1-2, dibutyl tin laurate 1-3 are more Wall carbon nano tube 2-5,2,4- imidazoles 1-2, Nano graphite powder 2-5, polyvinylpyrrolidone 0.1-0.3, HF solution, acetone, second Alcohol, distilled water, appropriate NaOH solution.
A kind of LED preparation methoies of AlN radiator surface radiating composite coating materials, it is characterised in that by following step Suddenly carry out：
A. silane coupling A 1100, second alcohol and water are pressed 20:70:The volume ratio mixing of 8-10, after stirring hydrolysis 10-30min, Add SiC, aluminium powder and SiO2, 30-50min is stirred at 60-80 DEG C, ultrasonic disperse 1-2h, alcohol is washed 3-5 time, in 105-125 DEG C Lower vacuum drying 3-5h, it is stand-by；
B. in the AlN of 2-3 parts 1:2-4 adds Y2O3And ethanol, mixing and ball milling 2-4h, add the nothing of polyvinyl butyral resin Hydrous ethanol solution, is subsequently placed in Muffle furnace and is warmed up to 450-550 DEG C, is incubated 1-2h, and 1700- is warming up in nitrogen atmosphere 1900 DEG C of heat preservation sintering 2-3h；
C. by stearic acid 1:3-5 mixes with ethanol, is heated to 60-80 DEG C and stirs, and adds resulting material in Ag microgranules and b, After constant temperature stirring 10-30min, 75-95 DEG C of oven for drying 1-2h is put into, is then mixed with dimethicone, Graphene, be put into glue Body agitator stirs 1-2h, the roasting 2-4h at 140-160 DEG C, further takes out stirring 1-2h, stand-by；
D. epoxy resin 828, PTS and remaining AlN are mixed, is warming up to 75-95 DEG C and stirs, 1:The Laurel of 2-5 Deca two Sour dibutyl tin and distilled water, at 80-95 DEG C 3-5h is reacted, and is then mixed with multi-walled carbon nano-tubes, in 60-80 DEG C of ultrasound 1- 2h, adds 2,4- imidazoles, continues sonic oscillation stirring 1-2h；
E. resulting material in a, c, d is mixed with montmorillonite, 1-2h is stirred at 60-80 DEG C, add firming agent and emulsifying silicon Oil, stirs 20-40min, is put in vacuum drying oven the vacuum defoamation 1-2h at 65-85 DEG C, is subsequently poured into mould, is placed on drying Solidify 3-5h in 60-85 DEG C in case, aging 3-6h, the demoulding at 75-95 DEG C obtain LED AlN high heat conduction type composites；
F. Nano graphite powder is mixed with polyvinylpyrrolidone, add water wiring solution-forming, in being added to NaOH electrolyte solutions, Ultrasonic agitation mix homogeneously, obtains mixed solution；Corrosion resistant plate with electrolysis bath as negative electrode, with e resulting material as anode, with Mixed solution is electrolyte, in the voltage of the additional 500V-1000V in electrolysis bath two ends, at 30-50 DEG C and under conditions of stirring, and oxygen Change reaction 1-2h, obtain a kind of LED AlN radiator surface radiating composite coating materials.
The reaction mechanism of the present invention is as follows：
（1）Add Y in AlN powder body2O3AlN ceramic is prepared, the synergism of the two is effectively facilitated the fine and close burning of AlN ceramic Knot, the high-ratio surface of AlN powder body can also promote the densification process of AlN ceramic, can be had at a relatively low sintering temperature The AlN ceramic of higher heat-conductivity.
（2）Oil, has higher thermal using Ag microgranules as heat-conducting silicone grease prepared by reinforcer based on dimethicone Conductance, with Hard Fat acid treatment the heat conductivility of silicone grease can be improved, and the heat-conducting silicone grease of preparation can be used for LED radiatings.
（3）The method for passing through chemical modification with poly- MTES (PTS), is successfully prepared organic silicon modified epoxy Oxygen tree fat, the hydrolysate of PTS mainly reacts with the hydroxyl in epoxy resin, and organosilicon is successfully introduced into into epoxy resin, Chemical modification epoxy resin product has excellent tensile strength and elongation at break, heat stability.
（4）AlN- carbon nano tube/epoxy resin composite materials are prepared for, using epoxy resin as matrix phase, with two Laurels Sour dibutyl tin is catalyst, and using filler AlN and multi-walled carbon nano-tubes as function phase, AlN can improve multi-walled carbon nano-tubes and exist Dispersibility in resin, both have cooperative effect, impart the good heat conduction of resin and processing characteristics, and excellent dielectric and Fire resistance.
（5）The present invention is prepared for for the surface heat conduction of LED radiators and high heat loss through radiation composite coating material, with combination The advantages of intensity is high, corrosion resistance is good, high-temperature stability is good, hardness is high, while process is simple is adapted to batch production, can implement Property it is strong, low cost can be used for LED radiators surface.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of LED AlN radiator surface radiating composite coating materials, are obtained by the raw material of following weight parts (g)：
SiC 10, aluminium powder 5, SiO25, Y2O38, silane coupling A 1,100 0.5, montmorillonite 3, firming agent 1, emulsified silicone oil 2, ring Oxygen tree fat 828 2, AlN 4, polyvinyl butyral resin 1, stearic acid 2, Ag microgranules 3, dimethicone 1, Graphene 4, poly- methyl Triethoxysilane (PTS) 1, dibutyl tin laurate 1, multi-walled carbon nano-tubes 5,2,4- imidazoles 1, Nano graphite powder 5, poly- second Alkene pyrrolidone 0.1, HF solution, acetone, ethanol, distilled water, appropriate NaOH solution.
A kind of LED preparation methoies of AlN radiator surface radiating composite coating materials, it is characterised in that by following step Suddenly carry out：
A. silane coupling A 1100, second alcohol and water are pressed 20:70:8 volume ratio mixing, after stirring hydrolysis 30min, adds SiC, aluminium powder and SiO2, 40min, ultrasonic disperse 1h are stirred at 60-70 DEG C, alcohol is washed 3 times, is vacuum dried at 115-125 DEG C 3h, it is stand-by；
B. in 2 parts of AlN 1:2 add Y2O3And ethanol, mixing and ball milling 2h, add the dehydrated alcohol of polyvinyl butyral resin Solution, is subsequently placed in Muffle furnace and is warmed up to 500-530 DEG C, is incubated 1h, and 1800-1900 DEG C of insulation is warming up in nitrogen atmosphere Sintering 2h；
C. by stearic acid 1:3 mix with ethanol, are heated to 70-80 DEG C and stir, and add resulting material in Ag microgranules and b, permanent After temperature stirring 30min, 85-95 DEG C of oven for drying 1h is put into, is then mixed with dimethicone, Graphene, be put into colloid stirring Device stirs 1h, the roasting 2h at 140-150 DEG C, further takes out stirring 1h, stand-by；
D. epoxy resin 828, PTS and remaining AlN are mixed, is warming up to 75-85 DEG C and stirs, 1:3 Deca tin dilaurates Dibutyl tin and distilled water, at 85-90 DEG C 3h is reacted, and is then mixed with multi-walled carbon nano-tubes, in 60-70 DEG C of ultrasound 1h, is added 2,4- imidazoles, continue sonic oscillation stirring 1h；
E. resulting material in a, c, d is mixed with montmorillonite, 2h is stirred at 70-80 DEG C, add firming agent and emulsified silicone oil, Stirring 40min, be put in vacuum drying oven the vacuum defoamation 1h at 75-85 DEG C, be subsequently poured into mould, be placed in drying baker in 70-85 DEG C of solidification 3h, aging 3h, the demoulding at 85-95 DEG C obtain LED AlN high heat conduction type composites；
F. Nano graphite powder is mixed with polyvinylpyrrolidone, add water wiring solution-forming, in being added to NaOH electrolyte solutions, Ultrasonic agitation mix homogeneously, obtains mixed solution；Corrosion resistant plate with electrolysis bath as negative electrode, with e resulting material as anode, with Mixed solution is electrolyte, in the voltage of the additional 500V-600V in electrolysis bath two ends, at 40-50 DEG C and under conditions of stirring, and oxidation Reaction 2h, obtains a kind of LED AlN radiator surface radiating composite coating materials.
A kind of LED prepared by above-described embodiment is as follows with the performance test results of AlN radiator surface radiating composite coating materials It is shown：
Heat conductivity is 362.89W/m K, and thermal coefficient of expansion is 13.38 × 10-6·K-1(50-150 DEG C), tensile strength is 60.79MPa, elongation at break is up to 12.92%.

Claims (2)

1. a kind of LED AlN radiator surface radiating composite coating materials, it is characterised in that by the raw material system of following weight parts ：
SiC 10-12, aluminium powder 5-8, SiO25-13, Y2O35-8, the 0.5-1.5 of silane coupling A 1100, montmorillonite 3-6, solidification Agent 1-4, emulsified silicone oil 1-2, the 2-5 of epoxy resin 828, AlN 3-4, polyvinyl butyral resin 1-2, stearic acid 1-2, Ag microgranules 1-3, dimethicone 1-2, Graphene 1-4, poly- MTES (PTS) 1-2, dibutyl tin laurate 1-3 are more Wall carbon nano tube 2-5,2,4- imidazoles 1-2, Nano graphite powder 2-5, polyvinylpyrrolidone 0.1-0.3, HF solution, acetone, second Alcohol, distilled water, appropriate NaOH solution.
2. a kind of LED according to claim 1 preparation methoies of AlN radiator surface radiating composite coating materials, its It is characterised by, carries out according to the following steps：
Silane coupling A 1100, second alcohol and water are pressed 20:70:The volume ratio mixing of 8-10, after stirring hydrolysis 10-30min, plus Enter SiC, aluminium powder and SiO2, 30-50min is stirred at 60-80 DEG C, ultrasonic disperse 1-2h, alcohol is washed 3-5 time, at 105-125 DEG C Vacuum drying 3-5h, it is stand-by；
B. in the AlN of 2-3 parts 1:2-4 adds Y2O3And ethanol, mixing and ball milling 2-4h, add the anhydrous of polyvinyl butyral resin Ethanol solution, is subsequently placed in Muffle furnace and is warmed up to 450-550 DEG C, is incubated 1-2h, and 1700-1900 is warming up in nitrogen atmosphere DEG C heat preservation sintering 2-3h；
C. by stearic acid 1:3-5 mixes with ethanol, is heated to 60-80 DEG C and stirs, and adds resulting material in Ag microgranules and b, After constant temperature stirring 10-30min, 75-95 DEG C of oven for drying 1-2h is put into, is then mixed with dimethicone, Graphene, be put into glue Body agitator stirs 1-2h, the roasting 2-4h at 140-160 DEG C, further takes out stirring 1-2h, stand-by；
D. epoxy resin 828, PTS and remaining AlN are mixed, is warming up to 75-95 DEG C and stirs, 1:The Laurel of 2-5 Deca two Sour dibutyl tin and distilled water, at 80-95 DEG C 3-5h is reacted, and is then mixed with multi-walled carbon nano-tubes, in 60-80 DEG C of ultrasound 1- 2h, adds 2,4- imidazoles, continues sonic oscillation stirring 1-2h；
E. resulting material in a, c, d is mixed with montmorillonite, 1-2h is stirred at 60-80 DEG C, add firming agent and emulsifying silicon Oil, stirs 20-40min, is put in vacuum drying oven the vacuum defoamation 1-2h at 65-85 DEG C, is subsequently poured into mould, is placed on drying Solidify 3-5h in 60-85 DEG C in case, aging 3-6h, the demoulding at 75-95 DEG C obtain LED AlN high heat conduction type composites；
F. Nano graphite powder is mixed with polyvinylpyrrolidone, add water wiring solution-forming, in being added to NaOH electrolyte solutions, Ultrasonic agitation mix homogeneously, obtains mixed solution；Corrosion resistant plate with electrolysis bath as negative electrode, with e resulting material as anode, with Mixed solution is electrolyte, in the voltage of the additional 500V-1000V in electrolysis bath two ends, at 30-50 DEG C and under conditions of stirring, and oxygen Change reaction 1-2h, obtain a kind of LED AlN radiator surface radiating composite coating materials.
CN201610976764.3A 2016-11-08 2016-11-08 AlN radiator surface radiating composite coating material for LED and preparing method of AlN radiator surface radiating composite coating material Pending CN106566409A (en)

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