CN104610849B - Heat-conducting insulating coating for electronic components and preparation method thereof - Google Patents
Heat-conducting insulating coating for electronic components and preparation method thereof Download PDFInfo
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- CN104610849B CN104610849B CN201510050226.7A CN201510050226A CN104610849B CN 104610849 B CN104610849 B CN 104610849B CN 201510050226 A CN201510050226 A CN 201510050226A CN 104610849 B CN104610849 B CN 104610849B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a heat-conducting insulating coating for electronic components. The coating comprises the following raw materials in parts by weight: 40-60 parts of epoxy resin, 35-50 parts of an active diluent, 5-20 parts of nanometer silicon carbide, 1-5 parts of a coupling agent and 0.5-2 parts of a cationic initiator, wherein the particle size of nanometer silicon carbide is 40-100nm and the cationic initiator is diphenyl-(4-phenylthio)phenylsulfonium hexafluoroantimonate and/or diphenyl-(4-phenylsulfanyl)phenylsulfonium hexafluorophosphate. The heat-conducting insulating coating can be cured into a film within 1 minute by virtue of ultraviolet light curing, high-temperature baking is not needed, the heat-conducting insulating coating is high in curing speed and the coating efficiency of the coating is greatly increased. Nanometer silicon carbide is added so that the curing efficiency of the coating can be increased and meanwhile, the film can have good heat-conducting property. Since the coating is free of easily volatile organic solvents, the coating is a completely environment-friendly coating.
Description
Technical field
The invention belongs to coating process field is and in particular to a kind of insulating heat conductive coating for electronic devices and components and its system
Preparation Method.
Background technology
Due to developing rapidly of integrated technology and package technique, electronic component, the volume hundreds of millions of times ground of logic circuit
Reduce, the thermal diffusivity of material is put forward higher requirement.There is the metal of Thermal conductivity and its oxide due to electricity absolutely
Edge, chemical resistance and building-up property poor it is difficult to adapt to actual use requirement.Therefore, in the urgent need to developing
The insulating polymer composite of high thermal conductivity.
The macromolecular material of preparation high heat conduction has two kinds of approach.The first is to prepare the macromolecule with good heat conductive structure
Material, such as has the materials such as the polyacetylene of conjugated structure, polyaniline, polypyrrole.These material conjugated structures are big, can be using electricity
The heat conduction well of sub- pass through mechanism, the heat conductivility of these materials is relatively good, but also has electric conductivity simultaneously；Can also pass through
Improve polymer crystallinity, using phonon thermal conduction mechanism heat conduction, preparation has the macromolecule of high heat conduction structure.Come in this way
Prepare heat-conducting insulation material very high to equipment, technological requirement, industrialized production relatively difficult to achieve.Prepared by heat conductive insulating macromolecular material
Second approach it is simply that in polymer filling heat conduction component to prepare polymer composite, general high heat conduction component
It is the inorganic matters of high heat conduction.When the consumption of inorganic matters is less, though filler is dispersed in resin, fail to each other to be formed
Contact with each other and interact, the heat conductivility of material is improved less.But face accordingly when the loading of inorganic matters reaches
After dividing value, inorganic matters are connected with each other, and form one and are similar to netted or chain heat conduction network.Direction and hot-fluid when heat conduction network
When direction is consistent, the heat conductivility of material significantly improves.This method, simply it is easy to industrialized production, is also that current heat conduction is exhausted
The Main way of edge macromolecular material research.
The Chinese patent literature of Publication No. CN102757712A, with epoxy resin as matrix, directly mixes on this basis
Plus through silane coupler modified BN nanometer grade high heat conduction granule, prepare high heat conductive insulating paint.This insullac has excellent
Heat conductivity and resistance to surface breakdown ability.This paint film needs in high temperature furnace through 60 DEG C of 1h, 120 DEG C of 1.5h, 150 DEG C of 2h gradient liters
The continuous baking of temperature is obtained.
The open one kind of the Chinese patent literature of Publication No. CN102690597A adds absolutely in polyamide-imide resin
The insulating heat-conductive coating of edge heat filling.This insulating heat-conductive filler is aluminium sesquioxide, silicon nitride, carborundum, aluminium nitride, dioxy
Any a kind in SiClx, magnesium oxide, beryllium oxide, oxidisability or carbon dust or at least 2 kinds of combination.This insullac needs in 0.8mm
Copper conductor on coating sintering be obtained enamel-covered wire.
The Chinese patent literature of Publication No. CN102559048A discloses one kind in epoxy modified silicone insulating heat-conductive
The preparation method of high-temperature resistant coating.This coating is made up of epoxy modified silicone resin, filler, coupling agent, solvent.This invention solution
Determine coatings combine insulation, heat conduction, resistant to elevated temperatures performance issue.This paint film needs to be obtained in 160 DEG C of solidification 30min.
The Chinese patent literature of Publication No. CN102139263A discloses a kind of use of polyether-ether-ketone insulating heat conductive coating
Method.The method is by not cooled polyether-ether-ketone insulating heat conductive coating after the completion of preparation, is applied directly on matrix material,
After coating, matrix material is cleaned with water, after removing solvent and inorganic salt, puts into and 3-5 hour is dried in baking oven at 180 DEG C, so
Afterwards material is placed in vacuum sintering furnace, sinters 5～10 minutes at 380～400 DEG C, obtaining surface-coated has the base of polyether-ether-ketone
Body material.This insulating heat conductive coating is during the synthesis of polyether-ether-ketone, adds heat conduction inorganic filler to obtain.This coating
There is good heat conductivity, insulating properties and toughness, can be widely applied to non-stick pan, chemical anticorrosion.
These insulating heat-conductive coating above-mentioned are all to need to solidify at high temperature half an hour more than to can be only achieved preferable performance.
So both consume the energy, reduced the service efficiency of coating again, do not meet very much the fast-developing demand of current economic.
Content of the invention
The invention provides one kind has curing rate soon, high-termal conductivity, do not affect electronic device precision, insulate simultaneously
Excellent insulating heat conductive coating for electronic devices and components of property and preparation method thereof.
A kind of insulating heat conductive coating for electronic devices and components, in terms of parts by weight, raw material consists of：
The particle diameter of described nanometer silicon carbide is 40～100nm；
Described cationic initiator is diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate and/or diphenyl-(4-
Phenyl sulfur) phenyl sulfonium hexafluorophosphate.
Preferably, described epoxy resin be selected from bisphenol A epoxide resin, bisphenol F epoxy resin, cycloaliphatic epoxy resin,
At least one in epoxidised soybean oil, modifying epoxy resin by organosilicon.These resins have preferable electrical insulating property, resistance to height
Temperature, chemical resistance, through cationic curing, volume contraction is little, has preferable adhesive force to metal base, also will not make base material simultaneously
Deformation, does not affect precision.
Further preferably, described epoxy resin be bisphenol A epoxide resin and epoxidised soybean oil, bisphenol A epoxide resin and
The mass ratio of epoxidised soybean oil is 1.5～4:1.Under this special ratios, feature composition epoxy resin after cationic curing,
Paint film can be made to accomplish hard and tough effective coordination.
Preferably, described reactive diluent be selected from phenyl glycidyl ether, o-tolyl glycidyl ether, to tertiary fourth
Base phenyl glycidyl ether, resorcinolformaldehyde resin, polypropylene glycol diglycidyl ether, tetramethylolmethane (+)-2,3-Epoxy-1-propanol
At least one in ether, trihydroxymethylpropanyltri diglycidyl ether.The addition of these reactive diluents can improve described leading
The laundering period of heat insulation coating, and the toughness of the coating that described insulating heat conductive coating is formed can be improved.
Further preferably, described reactive diluent is trihydroxy methyl triglycidyl ether and tert-butyl-phenyl is shunk sweet
Oily ether, trihydroxy methyl triglycidyl ether and the mass ratio to tert-butyl-phenyl glycidyl ether are 3:1.Under this special ratios,
The reactive diluent of feature composition and the better adaptability of other components, can effectively adjust the working viscosity of coating, also not simultaneously
The curing rate of impact system.
Using coupling agent, nanometer silicon carbide is surface-treated, the compatibility with coating can be increased so as to energy is good
It is dispersed in coating and do not settle.Preferably, described coupling agent is selected from γ aminopropyltriethoxy silane, γ-shrink
At least one in glycerol ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane.Described
Coupling agent not only can make heat filling dispersed in coating, also can promote the adhesive force to base material simultaneously, improves paint film
Performance.More preferably γ-glycidyl ether oxygen propyl trimethoxy silicane.
The particle diameter of described nanometer silicon carbide need to control between 40～100nm.Nanometer silicon carbide under this specified particle diameter
Filler has higher heat-conductivity, to diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate, diphenyl-(4- phenyl sulfur) phenyl
Sulfonium hexafluorophosphate both cationic curings have catalytic action, can promote cationic curing, so that particle is more easy in resinite
System is internally formed heat conduction network chain, reduces material internal voidage, improves mechanics and heat conductivility, applies in coating, Ke Yi great
Amplitude improves the heat conductive insulating of coating.
For filled-type thermally conductive coating, thermal conductivity depends on the common work of heat filling and resin matrix and heat filling
With.When the heat filling consumption of different shapes that is scattered in resin is less, though being dispersed in resin, if to each other not
Contact can be formed and interact, material thermal conductivity improves less；When amount of filler brings up to a certain marginal value, shape between filler
Become contact and interact, in system, define similar netted or chain configuration, that is, form heat conduction network chain, thermal conductivity carries
Quickly, nanometer silicon carbide optimum addition is only 8～15% to height.
Preferably, in terms of parts by weight, the raw material of described insulating heat conductive coating consists of：
The particle diameter of described nanometer silicon carbide is 40～100nm；
Described cationic initiator is diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate or diphenyl-(4- phenyl
Sulfur) phenyl sulfonium hexafluorophosphate.
Further preferably,
The raw material of described insulating heat conductive coating consists of：
The mass ratio of described E-51 and epoxidised soybean oil is 1.5～4:1；
Described trihydroxy methyl triglycidyl ether and the mass ratio to tert-butyl-phenyl glycidyl ether are 3:1；
The particle diameter of described nanometer silicon carbide is 40～100nm；
Described cationic initiator is diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate or diphenyl-(4- phenyl
Sulfur) phenyl sulfonium hexafluorophosphate.
The invention also discloses the preparation method of described insulating heat conductive coating, comprise the following steps：
(1) by nanometer silicon carbide, coupling agent, amount of activated diluent mix homogeneously, ultrasonic disperse 1 at 60～70 DEG C～
2h, obtains dispersion liquid；
(2) epoxy resin and residual activity diluent are mixed, after being uniformly dispersed, the dispersion liquid being obtained with step (1) is mixed
Close, after being uniformly dispersed again, obtain material liquid, add cationic initiator, mix homogeneously obtains described insulating heat conductive coating.
Preferably, in step (2), after epoxy resin and the mixing of residual activity diluent, under 800～1200 revs/min
Dispersion 30～40 minutes is to uniform；The dispersion liquid being obtained with step (1) again is mixed, and disperses 40 under 1500～2000 revs/min again
～50 minutes to uniform.
Preferably, first the temperature of material liquid is down to less than 35 DEG C, add cationic initiator, then 800～
Under 1200 revs/min, dispersion obtains described insulating heat conductive coating to uniform in 10～20 minutes.
Compared with prior art, beneficial effects of the present invention are embodied in：
(1) coating of present invention preparation is through ultraviolet light polymerization, can in 1 minute film-forming, without high-temperature baking, have
There is curing rate faster, do not interfere with the precision of electronic devices and components simultaneously, the coating efficiency of coating can be made to obtain very big
Improve.
(2) employ and there is the nanometer silicon carbide of superior insulation heat conductivility as filler, impart excellent exhausted of coating
Edge, the performance of heat conduction, and the cationic curing speed of epoxy resin can be improved, therefore can be widely used in various electronic components,
The protection of logic circuit.
(3) coating of present invention preparation makes and coating process is simple, it is convenient to apply, and can directly adopt the side such as screen painting
Method coats or is sprayed on surface of workpiece so as to obtain preferably insulation, the performance of heat conduction.
Specific embodiment
Embodiment 1～5
(1) press the parts by weight shown in table 1 add in container 1 trihydroxy methyl triglycidyl ether, particle diameter be 40～
The nanometer silicon carbide of 60nm, coupling agent, after being sufficiently stirred for, carry out 1.5h using sound wave washer to this mixed solution at 60 DEG C
Dispersion；
(2) the bisphenol A epoxide resin E-51 of parts by weight shown in table 1, epoxidised soybean oil, three hydroxyls are added in container 2
Methyl triglycidyl ether, to tert-butyl-phenyl glycidyl ether, under 1000 revs/min, dispersion 30 minutes is so as to mix homogeneously.
Add the material that (1st) step obtains, dispersion under 2000 revs/min adds at temperature is less than 35 DEG C for 40 minutes so as to be uniformly dispersed
Plus the cationic initiator of parts by weight shown in table 1, disperse 20 minutes under 800 revs/min, that is, obtain for electronic devices and components
Insulating heat conductive coating, the performance test results are shown in Table 2.
Comparative example 1
Using raw material composition same as Example 1 and preparation method, differ only in, be added without nanometer silicon carbide.?
The performance test results of the insulating heat conductive coating obtaining eventually are shown in Table 3.
Comparative example 2
Using raw material composition same as Example 1 and preparation method, differ only in, add aluminium nitride to replace nano-sized carbon
SiClx, the performance test results of the insulating heat conductive coating finally giving are shown in Table 3.
Comparative example 3
Using raw material composition same as Example 1 and preparation method, differ only in, add diaryl group iodized salt CD-
1012 replacement initiators 6976, the performance test results of the insulating heat conductive coating finally giving are shown in Table 3.
Comparative example 1 and comparative example 1～3 understand, only nanometer silicon carbide is to the diphenyl-(4- adopting in the present invention
Phenyl sulfur) phenyl sulfonium hexafluoro antimonate and diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluorophosphate both cationic initiators
There is catalytic action, change the kind of heat filling or cationic initiator, all do not have this synergism.
Embodiment 6～8
Using raw material composition same as Example 1 and preparation method, differ only in, the grain of the nanometer silicon carbide of addition
Footpath is respectively 60～80nm, 80～100nm and 100～120nm.The performance test results of the insulating heat conductive coating finally giving are shown in
Table 4.
The coating that embodiment 1～8 and comparative example 1～3 are obtained is sprayed on copper coin when 30～40 DEG C, through 600～
1500mJ/cm2Ultraviolet light polymerization, you can obtain heat conductive insulating coating.The performance test results are as shown in table 2～4.
It can be seen that insulating heat conductive coating of the present invention has the advantages that adhesive force is good, heat conductivity and insulating properties are strong in table 2.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Bisphenol-A epoxy E-51 | 40 | 40 | 30 | 35 | 40 |
| Epoxidised soybean oil | 10 | 10 | 20 | 15 | 10 |
| Trihydroxy methyl triglycidyl ether | 30 | 30 | 30 | 30 | 30 |
| To tert-butyl-phenyl glycidyl ether | 10 | 10 | 10 | 10 | 10 |
| Nanometer silicon carbide | 5 | 10 | 15 | 8 | 5 |
| Coupling agent KH-560 | 2 | 2 | 2 | 2 | 2 |
| Initiator UNI-6976 | 2 | 2 | 2 | 2 | 0 |
| Initiator UNI-6992 | 0 | 0 | 0 | 0 | 2 |
Table 2
Table 3
Table 4
Claims (6)
1. a kind of insulating heat conductive coating by electronic devices and components is it is characterised in that in terms of parts by weight, raw material consists of：
The mass ratio of described bisphenol A epoxide resin and epoxidised soybean oil is 1.5～4:1；
Described reactive diluent is for trihydroxy methyl triglycidyl ether with to tert-butyl-phenyl glycidyl ether, trihydroxy methyl three
Glycidyl ether and the mass ratio to tert-butyl-phenyl glycidyl ether are 3:1；
The particle diameter of described nanometer silicon carbide is 40～100nm；
Described cationic initiator is diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate and/or diphenyl-(4- phenyl
Sulfur) phenyl sulfonium hexafluorophosphate.
2. the insulating heat conductive coating for electronic devices and components according to claim 1 is it is characterised in that described coupling agent
Selected from γ aminopropyltriethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxy
At least one in propyl trimethoxy silicane.
3. the insulating heat conductive coating for electronic devices and components according to claim 2 is it is characterised in that described coupling agent
For γ-glycidyl ether oxygen propyl trimethoxy silicane.
4. the insulating heat conductive coating for electronic devices and components according to claims 1 to 3 any claim, its feature exists
In, in terms of parts by weight, raw material consists of：
The particle diameter of described nanometer silicon carbide is 40～100nm；
Described cationic initiator is diphenyl-(4- phenyl sulfur) phenyl sulfonium hexafluoro antimonate or diphenyl-(4- phenyl sulfur)
Phenyl sulfonium hexafluorophosphate.
5. a kind of preparation method of insulating heat conductive coating according to claim 1 is it is characterised in that comprise the following steps：
(1) by nanometer silicon carbide, coupling agent, amount of activated diluent mix homogeneously, at 60～70 DEG C, ultrasonic disperse 1～2h, obtains
To dispersion liquid；
(2) epoxy resin and residual activity diluent are mixed, after being uniformly dispersed, the dispersion liquid being obtained with step (1) is mixed, then
Secondary be uniformly dispersed after obtain material liquid, add cationic initiator, mix homogeneously obtains described insulating heat conductive coating.
6. the preparation method of insulating heat conductive coating according to claim 5 is it is characterised in that in step (2), first by raw material
The temperature of liquid is down to less than 35 DEG C, adds cationic initiator.
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| KR20170132605A (en) * | 2016-05-24 | 2017-12-04 | 주식회사 아모그린텍 | Electrically insulated and heat radiated coating composition and electrically insulated heat radiator coated with the same |
| CN107880721A (en) * | 2017-11-27 | 2018-04-06 | 苏州科茂电子材料科技有限公司 | High heat conduction/heat radiation coating of LED surface and preparation method thereof |
| CN108641550A (en) * | 2018-05-25 | 2018-10-12 | 广州惠利电子材料有限公司 | A kind of curing insulation protection glue and its preparation method and application |
| CN111621830A (en) * | 2020-06-09 | 2020-09-04 | 深圳市富济新材料科技有限公司 | Aluminum alloy surface treatment process |
| CN112877039A (en) * | 2021-03-05 | 2021-06-01 | 江苏晶河电子科技有限公司 | High-performance single-component organic silicon modified epoxy heat conduction material and preparation method thereof |
| CN113999591A (en) * | 2021-11-19 | 2022-02-01 | 国网江苏省电力有限公司电力科学研究院 | Photocuring epoxy graphene micaceous iron intermediate paint and preparation method thereof |
| CN115287028A (en) * | 2022-07-04 | 2022-11-04 | 李小源 | Pressure-sensitive UV (ultraviolet) insulating glue solution and preparation method and application thereof |
| CN115746703B (en) * | 2022-11-21 | 2023-11-10 | 东莞市雄驰电子有限公司 | Photo-curing coating composition prepared based on epoxy fluorobenzene silicone resin, coating method and application |
| CN115785713A (en) * | 2022-12-09 | 2023-03-14 | 中创新航科技股份有限公司 | Insulating paint and battery comprising same |
| CN116144243A (en) * | 2022-12-13 | 2023-05-23 | 国网安徽省电力有限公司超高压分公司 | Photo-curing heat-resistant epoxy resin coating for current transformer and preparation method and application thereof |
| CN117511353A (en) * | 2023-10-18 | 2024-02-06 | 东莞市瑞盟涂料有限公司 | Cell thermal runaway insulation protection material based on ultraviolet light and process |
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