CN105754297A - Heat-conducting electronic packaging composite and preparation method thereof - Google Patents
Heat-conducting electronic packaging composite and preparation method thereof Download PDFInfo
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- CN105754297A CN105754297A CN201610295259.2A CN201610295259A CN105754297A CN 105754297 A CN105754297 A CN 105754297A CN 201610295259 A CN201610295259 A CN 201610295259A CN 105754297 A CN105754297 A CN 105754297A
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- heat conductive
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- conductive electronic
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000004100 electronic packaging Methods 0.000 title abstract 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 63
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 52
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 50
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 41
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 40
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 21
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 21
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 21
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 20
- UENRXLSRMCSUSN-UHFFFAOYSA-N 3,5-diaminobenzoic acid Chemical compound NC1=CC(N)=CC(C(O)=O)=C1 UENRXLSRMCSUSN-UHFFFAOYSA-N 0.000 claims abstract description 19
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 5
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 80
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 38
- 238000005538 encapsulation Methods 0.000 claims description 32
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 32
- 239000005543 nano-size silicon particle Substances 0.000 claims description 27
- 229910052779 Neodymium Inorganic materials 0.000 claims description 20
- 239000003822 epoxy resin Substances 0.000 claims description 20
- 229920000647 polyepoxide Polymers 0.000 claims description 20
- 229940106691 bisphenol a Drugs 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 18
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 14
- 229910000077 silane Inorganic materials 0.000 claims description 14
- -1 γ-aminopropyl Chemical group 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000012467 final product Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 claims 1
- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 abstract description 7
- 230000017525 heat dissipation Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000009849 vacuum degassing Methods 0.000 abstract description 2
- 238000003287 bathing Methods 0.000 abstract 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000011010 flushing procedure Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 12
- 241000209094 Oryza Species 0.000 description 11
- 235000007164 Oryza sativa Nutrition 0.000 description 11
- 235000009566 rice Nutrition 0.000 description 11
- 239000000463 material Substances 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- NWODFYYWMUKPPE-UHFFFAOYSA-N C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(O)(O)O Chemical compound C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(O)(O)O NWODFYYWMUKPPE-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Abstract
The invention provides a heat-conducting electronic packaging composite and a preparation method thereof. The preparation method comprises the following steps: mixing nano-alumina, nano-silica, a silane coupling agent KH-551, a gamma-aminopropyltriethoxysilane and water at first, and stirring; drying after filtering; mixing with N-methyl pyrrolidone, pyridine and triphenyl phosphate for reaction; adding lithium chloride and methyl alcohol for further reaction; filtering, flushing with N-dimethyl formamide and drying; re-adding acetone for ultrasonic dispersion; mixing bisphenol A epoxy resin, Neodymium(III) 2,4-pentanedionate and water, heating, and stirring for dissolution; mixing the two mixtures, and stirring while performing ultrasonic treatment; performing water bathing, adding 3,5-diaminobenzoic acid, N-aminoethylpiperazine and trimethyl hexamethylene diamine, stirring, and then conducting vacuum degassing; finally, pouring the mixture into a die for curing to obtain the heat-conducting electronic packaging composite. The heat-conducting electronic packaging composite has excellent heat stability, and meanwhile, has very good heat conductivity and a good heat dissipation effect.
Description
Technical field
The present invention relates to Material Field, be specifically related to a kind of heat conductive electronic encapsulation composite and preparation method thereof.
Background technology
Along with developing rapidly of science and technology, electronics is integrated the rapidest with the development of package technique, electronic device and circuit
Just towards miniaturization, constantly reduce.Meanwhile, its workload is the most increasing, and frequency is more and more higher, thus
The heat produced also is continuously increased, in order to enable electronic device the most effectively to work, it is necessary to the heat radiation solving it is asked
Topic, stops constantly raising and reducing its operating efficiency and service life of temperature.Traditional electronic package material mainly uses pottery
Porcelain encapsulating material, but it is not high enough to have thermal conductivity factor, and density is big and high in cost of production shortcoming, therefore, research and development one thermal conductance
The electronic package material that rate is high, density is little, electrical insulation properties is good and with low cost has pass for the development of electron trade
The effect of key, also has wide market prospects simultaneously.
Summary of the invention
Solve the technical problem that: it is an object of the invention to provide a kind of heat conductive electronic encapsulation composite, there is brilliance
Thermal stability, there is good heat conductivility, excellent in heat dissipation effect simultaneously.
Technical scheme: a kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol-A ring
Epoxy resins 30-50 part, nano aluminium oxide 10-20 part, nano silicon 5-10 part, acetylacetone,2,4-pentanedione neodymium 1-3 part, 3,5-diaminourea
Benzoic acid 1-2 part, silane coupler KH-551 1-2 part, gamma-aminopropyl-triethoxy-silane 1-3 part, lithium chloride 1-2 part, N-
Methyl pyrrolidone 0.2-0.5 part, pyridine 0.5-1 part, triphenyl phosphite 0.1-0.3 part, N-aminoethyl piperazine 0.5-1 part,
N,N-dimethylformamide 40-60 part, trimethylhexamethylenediamine 1-3 part, acetone 50-70 part, methyl alcohol 80-100 part, water
80-100 part.
It is further preferred that described a kind of heat conductive electronic encapsulation composite, by following component with weight portion preparation
Become: bisphenol A epoxide resin 35-45 part, nano aluminium oxide 12-18 part, nano silicon 6-9 part, acetylacetone,2,4-pentanedione neodymium 1.5-2.5
Part, 3,5-diaminobenzoic acid 1.2-1.8 part, silane coupler KH-551 1.3-1.7 part, gamma-aminopropyl-triethoxy-silane
1.5-2.5 part, lithium chloride 1.2-1.8 part, 1-METHYLPYRROLIDONE 0.3-0.4 part, pyridine 0.6-0.9 part, triphenyl phosphite
0.15-0.25 part, N-aminoethyl piperazine 0.6-0.9 part, N,N-dimethylformamide 45-55 part, trimethylhexamethylenediamine
1.5-2.5 part, acetone 55-65 part, methyl alcohol 85-95 part, water 85-95 part.
The preparation method of above-mentioned heat conductive electronic encapsulation composite comprises the following steps:
Step 1: by nano aluminium oxide, nano silicon, silane coupler KH-551, gamma-aminopropyl-triethoxy-silane and
Water mixes, and stirs 3-5 hour at temperature 70-100 DEG C, rotating speed 60-80r/min with magnetic stirrer；
Step 2: filter, puts in vacuum drying chamber and is dried 2-3 hour at temperature 110-130 DEG C；
Step 3: by modified nano aluminium oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite
Hybrid reaction 3 hours, adds lithium chloride and methyl alcohol reacts 40 minutes；
Step 4: filter, be rinsed with DMF, be then placed in vacuum drying chamber at temperature 80-100 DEG C
Dry；
Step 5: add acetone, carry out ultrasonic disperse 40 minutes；
Step 6: bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, is heated to 80-90 DEG C of stirring and dissolving；
Step 7: by above-mentioned two step mixture mixing, stir the most ultrasonic 20-30 under rotating speed 400-600r/min with mixer
Minute；
Step 8: be placed in the water-bath of 60-80 DEG C, adds 3,5-diaminobenzoic acid, N-aminoethyl piperazine and trimethyl six methylene
Base diamines, stirs 5-10 minute final vacuum with mixer and deaerates 20-30 minute；
Step 9: be cast in mould by compound, at 130-140 DEG C, precuring is warming up to 160-170 DEG C admittedly after 2-3 hour
Change 13-15 hour, cool down and get final product.
One step is preferred, and in step 1, temperature is 80-90 DEG C, and rotating speed is 65-75r/min, and mixing time is that 3.5-4.5 is little
Time.
One step is preferred, and in step 2, temperature is 115-125 DEG C, and drying time is 2.5 hours.
One step is preferred, and in step 4, temperature is 85-95 DEG C.
One step is preferred, is heated to 85 DEG C in step 6.
One step is preferred, and step 7 medium speed is 450-550r/min, and ultrasonic time is 25 minutes.
One step is preferred, and in step 8, bath temperature is 65-75 DEG C, and mixing time is 6-9 minute, and degassing time is 25 points
Clock.
One step is preferred, and in step 9, precuring temperature is 135 DEG C, and pre-cure time is 2.5 hours, and solidification temperature is 165
DEG C, hardening time is 14 hours.
Beneficial effect: the heat conductive electronic encapsulation composite of the present invention has the thermal stability of brilliance, when temperature reaches
When 800 DEG C, its loss late is only 2.39%, and the present invention has good heat conductivility simultaneously, and its thermal conductivity factor reaches as high as
0.391W/ (m K), excellent heat dissipation performance.
Detailed description of the invention
Embodiment 1
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 30 parts, receive
Rice 10 parts of aluminum oxide, nano silicon 5 parts, acetylacetone,2,4-pentanedione neodymium 1 part, 3,5-diaminobenzoic acid 1 part, silane coupler KH-
551 1 parts, gamma-aminopropyl-triethoxy-silane 1 part, lithium chloride 1 part, 1-METHYLPYRROLIDONE 0.2 part, pyridine 0.5 part, phosphorous
Triphenyl phosphate ester 0.1 part, N-aminoethyl piperazine 0.5 part, N,N-dimethylformamide 40 parts, trimethylhexamethylenediamine 1 part, third
Ketone 50-70 part, methyl alcohol 80 parts, 80 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 70 C, rotating speed 60r/min
Lower stirring 3 hours, puts into after filtration in vacuum drying chamber and is dried 2 hours at temperature 110 DEG C, then by modified nano oxygen
Change aluminium, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add lithium chloride and
Methyl alcohol reacts 40 minutes, filters, is rinsed with DMF, is then placed in vacuum drying chamber at temperature 80 DEG C
Dry, add acetone, carry out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, is heated to
80 DEG C of stirring and dissolving；Above two mixture is mixed, stirs under rotating speed 400r/min the most ultrasonic 20 minutes with mixer,
Being placed in the water-bath of 60 DEG C again, add 3,5-diaminobenzoic acid, N-aminoethyl piperazine and trimethylhexamethylenediamine, with stirring
Machine of mixing stirs 5 minutes final vacuums and deaerates 20 minutes, is finally cast in mould by compound, at 130 DEG C after precuring 2 hours
It is warming up to 160 DEG C solidify 13 hours, cools down and get final product.
Embodiment 2
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 35 parts, receive
Rice 12 parts of aluminum oxide, nano silicon 6 parts, acetylacetone,2,4-pentanedione neodymium 1.5 parts, 3,5-diaminobenzoic acid 1.2 parts, silane coupler
KH-551 1.3 parts, gamma-aminopropyl-triethoxy-silane 1.5 parts, lithium chloride 1.2 parts, 1-METHYLPYRROLIDONE 0.3 part, pyridine
0.6 part, triphenyl phosphite 0.15 part, N-aminoethyl piperazine 0.6 part, N,N-dimethylformamide 45 parts, trimethyl six methylene
Base diamines 1.5 parts, 55 parts of acetone, methyl alcohol 85 parts, 85 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 80 DEG C, rotating speed 65r/min
Lower stirring 3.5 hours, puts into after filtration in vacuum drying chamber and is dried 2.5 hours at temperature 115 DEG C, then received by modified
Rice aluminum oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add chlorination
Lithium and methyl alcohol react 40 minutes, filter, are rinsed with DMF, are then placed in vacuum drying chamber in temperature 85
Dry at DEG C, add acetone, carry out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, adds
Heat is to 85 DEG C of stirring and dissolving；Above two mixture is mixed, under rotating speed 450r/min, stirs the most ultrasonic 25 with mixer
Minute, then be placed in the water-bath of 65 DEG C, add 3,5-diaminobenzoic acid, N-aminoethyl piperazine and tri-methyl hexamethylene two
Amine, stirs 6 minutes final vacuums with mixer and deaerates 25 minutes, be finally cast in mould by compound, precuring at 135 DEG C
It is warming up to 165 DEG C after 2.5 hours solidify 14 hours, cools down and get final product.
Embodiment 3
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 40 parts, receive
Rice 15 parts of aluminum oxide, nano silicon 7.5 parts, acetylacetone,2,4-pentanedione neodymium 2 parts, 3,5-diaminobenzoic acid 1.5 parts, silane coupler
KH-551 1.5 parts, gamma-aminopropyl-triethoxy-silane 2 parts, lithium chloride 1.5 parts, 1-METHYLPYRROLIDONE 0.35 part, pyridine
0.75 part, triphenyl phosphite 0.2 part, N-aminoethyl piperazine 0.75 part, N,N-dimethylformamide 50 parts, trimethyl six methylene
Base diamines 2 parts, 60 parts of acetone, methyl alcohol 90 parts, 90 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 85 DEG C, rotating speed 70r/min
Lower stirring 4 hours, puts into after filtration in vacuum drying chamber and is dried 2.5 hours at temperature 120 DEG C, then by modified nanometer
Aluminum oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add lithium chloride
React 40 minutes with methyl alcohol, filter, be rinsed with DMF, be then placed in vacuum drying chamber temperature 90 DEG C
Lower drying, adds acetone, carries out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, heating
To 85 DEG C of stirring and dissolving；Above two mixture is mixed, under rotating speed 500r/min, stirs the most ultrasonic 25 points with mixer
Clock, then be placed in the water-bath of 70 DEG C, addition 3,5-diaminobenzoic acid, N-aminoethyl piperazine and trimethylhexamethylenediamine,
Stir 7.5 minutes final vacuums with mixer to deaerate 25 minutes, finally compound is cast in mould, precuring at 135 DEG C
It is warming up to 165 DEG C after 2.5 hours solidify 14 hours, cools down and get final product.
Embodiment 4
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 45 parts, receive
Rice 18 parts of aluminum oxide, nano silicon 9 parts, acetylacetone,2,4-pentanedione neodymium 2.5 parts, 3,5-diaminobenzoic acid 1.8 parts, silane coupler
KH-551 1.7 parts, gamma-aminopropyl-triethoxy-silane 2.5 parts, lithium chloride 1.8 parts, 1-METHYLPYRROLIDONE 0.4 part, pyridine
0.9 part, triphenyl phosphite 0.25 part, N-aminoethyl piperazine 0.9 part, N,N-dimethylformamide 55 parts, trimethyl six methylene
Base diamines 2.5 parts, 65 parts of acetone, methyl alcohol 95 parts, 95 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 90 DEG C, rotating speed 75r/min
Lower stirring 4.5 hours, puts into after filtration in vacuum drying chamber and is dried 2.5 hours at temperature 125 DEG C, then received by modified
Rice aluminum oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add chlorination
Lithium and methyl alcohol react 40 minutes, filter, are rinsed with DMF, are then placed in vacuum drying chamber in temperature 95
Dry at DEG C, add acetone, carry out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, adds
Heat is to 85 DEG C of stirring and dissolving；Above two mixture is mixed, under rotating speed 550r/min, stirs the most ultrasonic 25 with mixer
Minute, then be placed in the water-bath of 75 DEG C, add 3,5-diaminobenzoic acid, N-aminoethyl piperazine and tri-methyl hexamethylene two
Amine, stirs 9 minutes final vacuums with mixer and deaerates 25 minutes, be finally cast in mould by compound, precuring at 135 DEG C
It is warming up to 165 DEG C after 2.5 hours solidify 14 hours, cools down and get final product.
Embodiment 5
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 50 parts, receive
Rice 20 parts of aluminum oxide, nano silicon 10 parts, acetylacetone,2,4-pentanedione neodymium 3 parts, 3,5-diaminobenzoic acid 2 parts, silane coupler KH-
551 2 parts, gamma-aminopropyl-triethoxy-silane 3 parts, lithium chloride 2 parts, 1-METHYLPYRROLIDONE 0.5 part, pyridine 1 part, phosphorous acid
Triphenylmethyl methacrylate 0.3 part, N-aminoethyl piperazine 1 part, N,N-dimethylformamide 60 parts, trimethylhexamethylenediamine 3 parts, acetone 70
Part, methyl alcohol 100 parts, 100 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 100 DEG C, rotating speed 80r/
Stir 5 hours under min, put into after filtration in vacuum drying chamber and be dried 3 hours at temperature 130 DEG C, then modified is received
Rice aluminum oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add chlorination
Lithium and methyl alcohol react 40 minutes, filter, are rinsed with DMF, are then placed in vacuum drying chamber in temperature
Dry at 100 DEG C, add acetone, carry out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed,
It is heated to 90 DEG C of stirring and dissolving；Above two mixture is mixed, stirs the most ultrasonic under rotating speed 600r/min with mixer
30 minutes, then be placed in the water-bath of 80 DEG C, add 3,5-diaminobenzoic acid, N-aminoethyl piperazine and tri-methyl hexamethylene two
Amine, stirs 10 minutes final vacuums with mixer and deaerates 30 minutes, be finally cast in mould by compound, pre-solid at 140 DEG C
It is warming up to 170 DEG C after changing 3 hours solidify 15 hours, cools down and get final product.
Comparative example 1
The present embodiment is not contain N-aminoethyl piperazine and trimethylhexamethylenediamine with the difference of embodiment 5.Specifically
Say and be:
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 50 parts, receive
Rice 20 parts of aluminum oxide, nano silicon 10 parts, acetylacetone,2,4-pentanedione neodymium 3 parts, 3,5-diaminobenzoic acid 2 parts, silane coupler KH-
551 2 parts, gamma-aminopropyl-triethoxy-silane 3 parts, lithium chloride 2 parts, 1-METHYLPYRROLIDONE 0.5 part, pyridine 1 part, phosphorous acid
Triphenylmethyl methacrylate 0.3 part, N,N-dimethylformamide 60 parts, 70 parts of acetone, methyl alcohol 100 parts, 100 parts of water.
The preparation method of above-mentioned heat conductive electronic encapsulation composite is: first by nano aluminium oxide, nano silicon, silane
Coupling agent KH-551, gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer at temperature 100 DEG C, rotating speed 80r/
Stir 5 hours under min, put into after filtration in vacuum drying chamber and be dried 3 hours at temperature 130 DEG C, then modified is received
Rice aluminum oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite hybrid reaction 3 hours, add chlorination
Lithium and methyl alcohol react 40 minutes, filter, are rinsed with DMF, are then placed in vacuum drying chamber in temperature
Dry at 100 DEG C, add acetone, carry out ultrasonic disperse 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed,
It is heated to 90 DEG C of stirring and dissolving；Above two mixture is mixed, stirs the most ultrasonic under rotating speed 600r/min with mixer
30 minutes, then be placed in the water-bath of 80 DEG C, adding 3,5-diaminobenzoic acid, with mixer stirring final vacuum degassing 30 in 10 minutes
Minute, finally compound is cast in mould, at 140 DEG C, precuring is warming up to 170 DEG C of solidifications 15 hours after 3 hours, cold
But and get final product.
Comparative example 2
The present embodiment is not contain nano silicon with the difference of embodiment 5, replaces with nano aluminium oxide.Specifically
It is:
A kind of heat conductive electronic encapsulation composite, is prepared from weight portion by following component: bisphenol A epoxide resin 50 parts, receive
Rice 30 parts of aluminum oxide, acetylacetone,2,4-pentanedione neodymium 3 parts, 3,5-diaminobenzoic acid 2 parts, silane coupler KH-551 2 parts, γ-aminopropyl
Triethoxysilane 3 parts, lithium chloride 2 parts, 1-METHYLPYRROLIDONE 0.5 part, pyridine 1 part, triphenyl phosphite 0.3 part, N-ammonia
Ethyl piperazidine 1 part, N,N-dimethylformamide 60 parts, trimethylhexamethylenediamine 3 parts, 70 parts of acetone, methyl alcohol 100 parts, water
100 parts.
Above-mentioned heat conductive electronic encapsulation composite preparation method be: first by nano aluminium oxide, silane coupler KH-551,
Gamma-aminopropyl-triethoxy-silane and water mixing, with magnetic stirrer temperature 100 DEG C, stir 5 hours under rotating speed 80r/min,
Put into after filtration in vacuum drying chamber and be dried 3 hours at temperature 130 DEG C, then by modified nano aluminium oxide and N-methyl
Pyrrolidones, pyridine, triphenyl phosphite hybrid reaction 3 hours, add lithium chloride and methyl alcohol reacts 40 minutes, filters, with N,
Dinethylformamide is rinsed, and is then placed in vacuum drying chamber and dries at temperature 100 DEG C, adds acetone, surpass
Sound disperses 40 minutes；Bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, is heated to 90 DEG C of stirring and dissolving；By above two
Mixture mixes, and stirs the most ultrasonic 30 minutes with mixer, then be placed in the water-bath of 80 DEG C under rotating speed 600r/min, adds
3,5-diaminobenzoic acids, N-aminoethyl piperazine and trimethylhexamethylenediamine, stir 10 minutes final vacuums with mixer and take off
Gas 30 minutes, is finally cast into compound in mould, and at 140 DEG C, to be warming up to 170 DEG C of solidifications after 3 hours 15 little in precuring
Time, cool down and get final product.
The property indices of material of the present invention see table, it may be seen that the present invention has the heat endurance of brilliance
Can, when temperature reaches 800 DEG C, its loss late is only 2.39%, and the present invention has good heat conductivility simultaneously, its thermal conductivity factor
Reach as high as 0.391W/ (m K), excellent heat dissipation performance.
The performance indications of table 1 heat conductive electronic encapsulation composite
Claims (10)
1. a heat conductive electronic encapsulation composite, it is characterised in that: it is prepared from weight portion by following component: bisphenol-A ring
Epoxy resins 30-50 part, nano aluminium oxide 10-20 part, nano silicon 5-10 part, acetylacetone,2,4-pentanedione neodymium 1-3 part, 3,5-diaminourea
Benzoic acid 1-2 part, silane coupler KH-551 1-2 part, gamma-aminopropyl-triethoxy-silane 1-3 part, lithium chloride 1-2 part, N-
Methyl pyrrolidone 0.2-0.5 part, pyridine 0.5-1 part, triphenyl phosphite 0.1-0.3 part, N-aminoethyl piperazine 0.5-1 part,
N,N-dimethylformamide 40-60 part, trimethylhexamethylenediamine 1-3 part, acetone 50-70 part, methyl alcohol 80-100 part, water
80-100 part.
A kind of heat conductive electronic encapsulation composite the most according to claim 1, it is characterised in that: by following component with weight
Part is prepared from: bisphenol A epoxide resin 35-45 part, nano aluminium oxide 12-18 part, nano silicon 6-9 part, acetylacetone,2,4-pentanedione
Neodymium 1.5-2.5 part, 3,5-diaminobenzoic acid 1.2-1.8 part, silane coupler KH-551 1.3-1.7 part, γ-aminopropyl three
Ethoxysilane 1.5-2.5 part, lithium chloride 1.2-1.8 part, 1-METHYLPYRROLIDONE 0.3-0.4 part, pyridine 0.6-0.9 part, Asia
Triphenyl phosphate 0.15-0.25 part, N-aminoethyl piperazine 0.6-0.9 part, N,N-dimethylformamide 45-55 part, trimethyl six
Methylene diamine 1.5-2.5 part, acetone 55-65 part, methyl alcohol 85-95 part, water 85-95 part.
3. the preparation method of a kind of heat conductive electronic encapsulation composite described in any one of claim 1 to 2, it is characterised in that:
Comprise the following steps:
Step 1: by nano aluminium oxide, nano silicon, silane coupler KH-551, gamma-aminopropyl-triethoxy-silane and
Water mixes, and stirs 3-5 hour at temperature 70-100 DEG C, rotating speed 60-80r/min with magnetic stirrer；
Step 2: filter, puts in vacuum drying chamber and is dried 2-3 hour at temperature 110-130 DEG C；
Step 3: by modified nano aluminium oxide, nano silicon and 1-METHYLPYRROLIDONE, pyridine, triphenyl phosphite
Hybrid reaction 3 hours, adds lithium chloride and methyl alcohol reacts 40 minutes；
Step 4: filter, be rinsed with DMF, be then placed in vacuum drying chamber at temperature 80-100 DEG C
Dry；
Step 5: add acetone, carry out ultrasonic disperse 40 minutes；
Step 6: bisphenol A epoxide resin, acetylacetone,2,4-pentanedione neodymium and water are mixed, is heated to 80-90 DEG C of stirring and dissolving；
Step 7: by above-mentioned two step mixture mixing, stir the most ultrasonic 20-30 under rotating speed 400-600r/min with mixer
Minute；
Step 8: be placed in the water-bath of 60-80 DEG C, adds 3,5-diaminobenzoic acid, N-aminoethyl piperazine and trimethyl six methylene
Base diamines, stirs 5-10 minute final vacuum with mixer and deaerates 20-30 minute；
Step 9: be cast in mould by compound, at 130-140 DEG C, precuring is warming up to 160-170 DEG C admittedly after 2-3 hour
Change 13-15 hour, cool down and get final product.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
In rapid 1, temperature is 80-90 DEG C, and rotating speed is 65-75r/min, and mixing time is 3.5-4.5 hour.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
In rapid 2, temperature is 115-125 DEG C, and drying time is 2.5 hours.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
In rapid 4, temperature is 85-95 DEG C.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
85 DEG C it are heated in rapid 6.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
Rapid 7 medium speeds are 450-550r/min, and ultrasonic time is 25 minutes.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described step
In rapid 8, bath temperature is 65-75 DEG C, and mixing time is 6-9 minute, and degassing time is 25 minutes.
The preparation method of a kind of heat conductive electronic the most according to claim 3 encapsulation composite, it is characterised in that: described
In step 9, precuring temperature is 135 DEG C, and pre-cure time is 2.5 hours, and solidification temperature is 165 DEG C, and hardening time is 14 little
Time.
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