CN107586529A - A kind of preparation method of high-power LED encapsulation heat sink material - Google Patents
A kind of preparation method of high-power LED encapsulation heat sink material Download PDFInfo
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- CN107586529A CN107586529A CN201710887874.7A CN201710887874A CN107586529A CN 107586529 A CN107586529 A CN 107586529A CN 201710887874 A CN201710887874 A CN 201710887874A CN 107586529 A CN107586529 A CN 107586529A
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Abstract
The invention discloses a kind of preparation method of high-power LED encapsulation heat sink material, is specially：Polyvinyl butyral resin is prepared first；Then the method peeled off using solvent prepares BN nanometer sheets, disperses again in the case of moist and modified, prepares modified BN nanometer sheets；Finally polyimide resin, modified BN nanometer sheets are added in high mixer, 10min is mixed, obtains compound A；Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, is eventually adding heat stabilizer, 1 3h is stirred, obtains high-power LED encapsulation heat sink material.Heat sink material excellent thermal conductivity produced by the present invention, adhesive property is good, and it is low to prepare cost.
Description
Technical field：
The present invention relates to a kind of great power LED encapsulating material, is specifically related to a kind of high-power LED encapsulation radiating material
The preparation method of material.
Background technology：
LED is with a series of protrusions such as its energy-saving and environmental protection, small volume, long lifespan, impact resistance, reliability height, fast response times
Advantage, it is considered to be substitute the novel green lighting source of traditional lighting.As LED is in the application development of lighting field, Gao Gong
Rate, high brightness, the LED of high-quality have become important development trend.However, LED electro-optical efficiency is relatively low at present, with
The increase of power, heat dissipation problem turns into the maximum technical bottleneck that LED illumination is popularized and developed, how to improve great power LED
The heat dispersion of device is one of key technology urgently to be resolved hurrily in its road for development.High-quality, high-power LED are obtained,
High-power LED encapsulation must be just improved, therefore, it is system to prepare the high-power LED encapsulation of excellent thermal conductivity with heat sink material
Standby high-quality, high-power LED key.
Patent 201610296614.8 discloses a kind of high-power LED encapsulation heat-conducting glue and its preparation technology, it include with
The raw material of lower parts by weight：10~20 parts of polyimide resin, span come 20~40 parts of amide resin, 30~70 parts of hexagonal AlN,
3~8 parts of nanometer hydroxyapatite powder, 20~60 parts of solvent, 2~5 parts of curing agent, 5~10 parts of toughener, 1~2 part of crosslinking agent,
3~5 parts of surfactant, the hexagonal AlN are sheet hexagonal AlN, and sheet size is 1~5 μm.It is of the invention by hexagonal AlN and basic
Resin polyimide resin, span come amide resin and property-modifying additive nanometer hydroxyapatite powder, solvent, curing agent, increasing
The conducting resinl tool that tough dose, crosslinking agent and surfactant are mixed to prepare under certain proportion and certain preparation process condition
There are good thermal conductivity, weatherability and heat resistance.But the present invention with the addition of substantial amounts of heat filling, not only increase heat-conducting glue
Preparation cost, also affect the stability and adhesive property of heat-conducting glue.
The content of the invention：
It is an object of the invention to provide a kind of preparation method of high-power LED encapsulation heat sink material, the heat sink material is led
Hot property is excellent, and adhesion strength is big, heat-resist, and it is low to prepare energy consumption.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 1-3h, obtain high-power LED encapsulation heat sink material.
As the preferred of above-mentioned technical proposal, in step (1), hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are
(0.1-0.5)：1：(7-11).
As the preferred of above-mentioned technical proposal, in step (1), the mass ratio of n-butanal and polyvinyl alcohol is (0.5-2)：1.
As the preferred of above-mentioned technical proposal, in step (2), the amount ratio of the boron nitride powder and isopropanol is 1mg：
7mL。
As the preferred of above-mentioned technical proposal, in step (3), the amount ratio of the polyvinylpyrrolidone and ethanol is
1g：(20-40)mL.
As the preferred of above-mentioned technical proposal, in step (3), polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：(0.1-0.5).
As the preferred of above-mentioned technical proposal, unseasoned solid, vinylidene fluoride monomers, CTFE monomer, initiator,
Emulsifying agent, the dosage of chain-transferring agent are respectively in parts by weight：Unseasoned 7 parts of solid, 5 parts of vinylidene fluoride monomers, trifluoro chloroethene
1 part of alkene monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent.
As the preferred of above-mentioned technical proposal, polyimide resin, modified BN nanometer sheets, polyvinyl butyral resin, ethanol,
Curing agent, heat stabilizer dosage in parts by weight, be respectively：Polyimide resin 40-80 parts, modified BN nanometer sheet 2-6 parts,
Polyvinyl butyral resin 1-4 parts, ethanol 15-30 parts, curing agent 1-2 parts, heat stabilizer 1-2 parts.
As the preferred of above-mentioned technical proposal, the curing agent is trimellitic anhydride.
As the preferred of above-mentioned technical proposal, the heat stabilizer is calcium stearate.
The invention has the advantages that：
The present invention uses the temperature control method synthesizing polyethylene butyral of high-temperature feeding low temperature aging, first in certain temperature
Lower progress hemiacetal reaction, then carries out aldolisation so that obtained polyvinyl butyral resin is stable at lower temperatures
Property is good, and high and low temperature resistance is excellent, and energy consumption is low, effectively reduces cost；
Hexagonal boron nitride has larger thermal conductivity factor, and especially in its (001) crystal plane direction, therefore, the present invention is using different
Propyl alcohol is that solvent is peeled off to hexagonal boron nitride, and it is nano level sheet BN to obtain thickness so that more (001) crystal face is sudden and violent
Expose, so as to which the BN nanometer sheets after peeling off have higher heat conductivility；And in order to avoid the BN nanometer sheet weights after stripping
New aggregation, the present invention are not dried to it, are directly scattered in solvent, and in situ altogether using vinylidene, CTFE
Poly- method is modified to BN nanometer sheets surface, and modified BN nanometer sheets not only have higher thermal conductivity factor, also with dissipating
Hot material matrix has good compatibility so that obtained heat sink material good heat conductivity, excellent in mechanical performance.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
Wherein, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are 0.1：1：7；The mass ratio of n-butanal and polyvinyl alcohol is 0.5：1；
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；Its
In, the amount ratio of polyvinylpyrrolidone and ethanol is 1g：20mL；Polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：0.1；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；Wherein, each component dosage is respectively in parts by weight：Unseasoned solid 7
Part, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 1h, obtain high-power LED encapsulation heat sink material；Wherein, each component dosage in parts by weight,
Respectively：40 parts of polyimide resin, modified 2 parts of BN nanometer sheets, 1 part of polyvinyl butyral resin, 15 parts of ethanol, 1 part of curing agent,
1 part of heat stabilizer.
Embodiment 2
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
Wherein, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are 0.5：1：11；The mass ratio of n-butanal and polyvinyl alcohol is 2：1；
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；Its
In, the amount ratio of polyvinylpyrrolidone and ethanol is 1g：40mL；Polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：0.5；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；Wherein, each component dosage is respectively in parts by weight：Unseasoned solid 7
Part, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 3h, obtain high-power LED encapsulation heat sink material；Wherein, each component dosage in parts by weight,
Respectively：80 parts of polyimide resin, modified 6 parts of BN nanometer sheets, 4 parts of polyvinyl butyral resin, 30 parts of ethanol, 2 parts of curing agent,
2 parts of heat stabilizer.
Embodiment 3
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
Wherein, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are 0.2：1：8；The mass ratio of n-butanal and polyvinyl alcohol is 0.8：1
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；Its
In, the amount ratio of polyvinylpyrrolidone and ethanol is 1g：25mL；Polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：0.2；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；Wherein, each component dosage is respectively in parts by weight：Unseasoned solid 7
Part, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 1.5h, obtain high-power LED encapsulation heat sink material；Wherein, each component dosage is with parts by weight
Meter, it is respectively：50 parts of polyimide resin, modified 3 parts of BN nanometer sheets, 2 parts of polyvinyl butyral resin, 20 parts of ethanol, curing agent
1.3 parts, 1.3 parts of heat stabilizer.
Embodiment 4
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
Wherein, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are 0.3：1：9；The mass ratio of n-butanal and polyvinyl alcohol is 1：1
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；Its
In, the amount ratio of polyvinylpyrrolidone and ethanol is 1g：30mL；Polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：0.3；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；Wherein, each component dosage is respectively in parts by weight：Unseasoned solid 7
Part, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 2h, obtain high-power LED encapsulation heat sink material；Wherein, each component dosage in parts by weight,
Respectively：60 parts of polyimide resin, modified 4 parts of BN nanometer sheets, 3 parts of polyvinyl butyral resin, 20 parts of ethanol, curing agent 1.6
Part, 1.6 parts of heat stabilizer.
Embodiment 5
A kind of preparation method of high-power LED encapsulation heat sink material, comprises the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be stirred
Uniformly, mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, is reacted
After end, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h is reacted at 45 DEG C, instead
Filtered after should terminating, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
Wherein, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are 0.4：1：10；The mass ratio of n-butanal and polyvinyl alcohol is 1.5：1
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain
Undried solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then add above-mentioned undried solid,
Water bath sonicator handles 10min under 500W power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；Its
In, the amount ratio of polyvinylpyrrolidone and ethanol is 1g：35mL；Polyvinylpyrrolidone, undried solid, sodium citrate
The mass ratio of the aqueous solution is 1:3：0.4；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, turned after being well mixed
Move in the three-necked flask with condenser pipe, be to slowly warm up to 60 DEG C, be passed through nitrogen protection, and initiator, emulsifying agent, chain is added dropwise
Transfer agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, obtained solid nothing
Dried after water-ethanol washing, obtain being modified BN nanometer sheets；Wherein, each component dosage is respectively in parts by weight：Unseasoned solid 7
Part, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent, 0.01 part of chain-transferring agent；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will
Polyvinyl butyral resin obtained above is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, most
After add heat stabilizer, stir 2.5h, obtain high-power LED encapsulation heat sink material；Wherein, each component dosage is with parts by weight
Meter, it is respectively：70 parts of polyimide resin, modified 5 parts of BN nanometer sheets, 3 parts of polyvinyl butyral resin, 27 parts of ethanol, curing agent
1.8 parts, 1.8 parts of heat stabilizer.
Encapsulating material obtained above is prepared into the cover film that thickness is 0.1mm and carries out performance test, test result
| Thermal conductivity coefficient, W/mk | Peel strength, N/mm | Dielectric strength, KV/mm | Heat resistance (s, 300 DEG C) | |
| Embodiment 1 | 7.9 | 9.6 | 27 | ＞ 300 |
| Embodiment 2 | 7.6 | 9.9 | 26 | ＞ 300 |
| Embodiment 3 | 7.8 | 10.1 | 28 | ＞ 300 |
| Embodiment 4 | 8.0 | 10.3 | 27 | ＞ 300 |
| Embodiment 5 | 7.9 | 9.9 | 26 | ＞ 300 |
It is as follows：
Encapsulating material good heat conductivity obtained above, excellent in mechanical performance are heat-resist.
Claims (10)
1. a kind of preparation method of high-power LED encapsulation heat sink material, it is characterised in that comprise the following steps：
(1) polyvinyl alcohol is dissolved in deionized water at 95 DEG C, is subsequently cooled to room temperature, added hydrochloric acid, be uniformly mixed,
Mixed liquor 1 is made；Mixed liquor 1 and n-butanal are added in ultrasonic reactor simultaneously, 45s is reacted at 60 DEG C, reaction terminates
Afterwards, the liquid in ultrasonic reactor is transferred in the tank reactor with heat exchange jacket, 3h, reaction knot is reacted at 45 DEG C
Filtered after beam, obtained solid is washed using deionized water, absolute ethyl alcohol successively, is dried, and polyvinyl butyral resin is made；
(2) boron nitride powder and isopropanol are mixed, 30min is ultrasonically treated under 1000W power, centrifuged, obtain not dry
Dry solid；
(3) polyvinylpyrrolidone and ethanol are mixed into solid dissolving, then adds above-mentioned undried solid, 500W
Water bath sonicator handles 10min under power, then adds 5g/L sodium citrate aqueous solution, obtains homogeneous dispersion liquid；
(4) vinylidene fluoride monomers, CTFE monomer are added in dispersion liquid obtained above, are transferred to after well mixed
In three-necked flask with condenser pipe, 60 DEG C are to slowly warm up to, is passed through nitrogen protection, and initiator, emulsifying agent, chain tra nsfer is added dropwise
Agent, reaction 3h being stirred at reflux, reaction is cooled to room temperature after terminating, and by reaction solution centrifugal treating, the anhydrous second of obtained solid
Dried after alcohol washing, obtain being modified BN nanometer sheets；
(5) polyimide resin, modified BN nanometer sheets are added in high mixer, mix 10min, obtain compound A；Will be above-mentioned
Obtained polyvinyl butyral resin is dissolved in ethanol, and adds curing agent, is stirring evenly and then adding into compound A, is finally added
Enter heat stabilizer, stir 1-3h, obtain high-power LED encapsulation heat sink material.
A kind of 2. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Step
(1) in, hydrochloric acid, polyvinyl alcohol, the mass ratio of deionized water are (0.1-0.5)：1：(7-11).
A kind of 3. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Step
(1) in, the mass ratio of n-butanal and polyvinyl alcohol is (0.5-2)：1.
A kind of 4. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Step
(2) in, the amount ratio of the boron nitride powder and isopropanol is 1mg：7mL.
A kind of 5. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Step
(3) in, the amount ratio of the polyvinylpyrrolidone and ethanol is 1g：(20-40)mL.
A kind of 6. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Step
(3) in, polyvinylpyrrolidone, undried solid, the mass ratio of sodium citrate aqueous solution are 1:3：(0.1-0.5).
A kind of 7. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：It is not dry
Dry solid, vinylidene fluoride monomers, CTFE monomer, initiator, emulsifying agent, the dosage of chain-transferring agent are distinguished in parts by weight
For：Unseasoned 7 parts of solid, 5 parts of vinylidene fluoride monomers, 1 part of CTFE monomer, 0.3 part of initiator, 0.12 part of emulsifying agent,
0.01 part of chain-transferring agent.
A kind of 8. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：Polyamides
Imide resin, modified BN nanometer sheets, polyvinyl butyral resin, ethanol, curing agent, heat stabilizer dosage in parts by weight, point
It is not：It is polyimide resin 40-80 parts, modified BN nanometer sheet 2-6 parts, polyvinyl butyral resin 1-4 parts, ethanol 15-30 parts, solid
Agent 1-2 parts, heat stabilizer 1-2 parts.
A kind of 9. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：It is described
Curing agent is trimellitic anhydride.
A kind of 10. preparation method of high-power LED encapsulation heat sink material as claimed in claim 1, it is characterised in that：It is described
Heat stabilizer is calcium stearate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137866A (en) * | 2020-01-10 | 2020-05-12 | 中国南方电网有限责任公司电网技术研究中心 | Method for preparing boron nitride nanosheet by efficiently stripping h-BN |
| CN114539940A (en) * | 2022-01-27 | 2022-05-27 | 广东顶峰精密技术有限公司 | Preparation method of high-temperature-resistant adhesive tape for lithium battery |
-
2017
- 2017-09-27 CN CN201710887874.7A patent/CN107586529A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137866A (en) * | 2020-01-10 | 2020-05-12 | 中国南方电网有限责任公司电网技术研究中心 | Method for preparing boron nitride nanosheet by efficiently stripping h-BN |
| CN114539940A (en) * | 2022-01-27 | 2022-05-27 | 广东顶峰精密技术有限公司 | Preparation method of high-temperature-resistant adhesive tape for lithium battery |
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Application publication date: 20180116 |