CN118222068A - High-heat-conductivity high-dispersibility epoxy resin composition and application thereof - Google Patents
High-heat-conductivity high-dispersibility epoxy resin composition and application thereof Download PDFInfo
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 64
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 64
- 239000000203 mixture Substances 0.000 title claims abstract description 38
- 239000002270 dispersing agent Substances 0.000 claims abstract description 64
- 239000005011 phenolic resin Substances 0.000 claims abstract description 21
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 21
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000011256 inorganic filler Substances 0.000 claims abstract description 7
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 7
- 239000003086 colorant Substances 0.000 claims abstract description 6
- 239000003607 modifier Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 12
- 239000006229 carbon black Substances 0.000 claims description 9
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 9
- 238000004806 packaging method and process Methods 0.000 claims description 9
- -1 polyethylene Polymers 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004203 carnauba wax Substances 0.000 claims description 7
- 239000004209 oxidized polyethylene wax Substances 0.000 claims description 7
- 235000013873 oxidized polyethylene wax Nutrition 0.000 claims description 7
- 239000001993 wax Substances 0.000 claims description 7
- 239000004305 biphenyl Substances 0.000 claims description 6
- 235000010290 biphenyl Nutrition 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- LRMHFDNWKCSEQU-UHFFFAOYSA-N ethoxyethane;phenol Chemical compound CCOCC.OC1=CC=CC=C1 LRMHFDNWKCSEQU-UHFFFAOYSA-N 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 229920013822 aminosilicone Polymers 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920003987 resole Polymers 0.000 claims description 2
- 150000003568 thioethers Chemical class 0.000 claims description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 claims 1
- 125000003118 aryl group Chemical group 0.000 claims 1
- 239000006082 mold release agent Substances 0.000 claims 1
- 229920003986 novolac Polymers 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 17
- 229920005989 resin Polymers 0.000 abstract description 12
- 239000011347 resin Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000005022 packaging material Substances 0.000 abstract description 5
- 238000004100 electronic packaging Methods 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 48
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 26
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 229920001971 elastomer Polymers 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 8
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 6
- 238000004821 distillation Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 230000003301 hydrolyzing effect Effects 0.000 description 6
- 230000003472 neutralizing effect Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000010025 steaming Methods 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 229910002026 crystalline silica Inorganic materials 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- VOOLKNUJNPZAHE-UHFFFAOYSA-N formaldehyde;2-methylphenol Chemical compound O=C.CC1=CC=CC=C1O VOOLKNUJNPZAHE-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 229960004063 propylene glycol Drugs 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 150000001343 alkyl silanes Chemical class 0.000 description 2
- 229910021488 crystalline silicon dioxide Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000012858 packaging process Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229920006336 epoxy molding compound Polymers 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of electronic packaging materials, in particular to a high-heat-conductivity high-dispersibility epoxy resin composition and application thereof, wherein the epoxy resin composition is prepared from the following raw materials: epoxy resin, phenolic resin, inorganic filler, colorant, release agent, coupling agent, curing accelerator, reactive stress modifier, dispersing agent and external dispersing agent; according to the invention, through the synergistic effect of the dispersing agent and the external dispersing agent, the dispersing agent can be attached to the surfaces of the inorganic filler particles, so that the filler particles can be uniformly dispersed in the resin, and the external dispersing agent can assist the dispersing agent to rapidly diffuse in the system, so that the purpose of rapid flow of the dispersing agent is achieved, and finally, the epoxy resin composition with high heat conductivity and high dispersibility is prepared, the high heat conductivity application requirement is met, the whole process is simple and convenient to operate, and the application prospect is wide.
Description
Technical Field
The invention relates to the technical field of electronic packaging materials, in particular to a high-heat-conductivity high-dispersibility epoxy resin composition and application thereof.
Background
The epoxy plastic packaging material (EMC) is generally composed of a plurality of auxiliary agents such as filler, epoxy resin, phenolic resin, curing agent, flame retardant and the like, and is widely applied in the packaging field as the EMC has excellent moisture resistance, high thermal conductivity, high reliability and excellent electrical insulation and mechanical properties, so that the EMC becomes a main stream material for packaging semiconductor components and integrated circuits. However, with miniaturization and integration of semiconductor components, chip energy consumption is larger and chip use environment temperature is higher and higher, and if heat generated by a power semiconductor is not timely dissipated, performance of the power semiconductor is affected, and the components are permanently damaged. Therefore, the packaging material is required to have higher heat conductivity so as to meet the heat dissipation requirement of the components.
The method for improving the heat conductivity mainly relies on a filler with high heat conductivity to form a heat conduction chain and a heat conduction network in an epoxy resin matrix. The EMC constructed by filler silicon dioxide (SiO 2) can not meet the requirement of high thermal conductivity at present, and the EMC constructed by filler aluminum oxide (Al 2O3) is an indispensable packaging material in the electronic packaging industry, but the surface inertia of Al 2O3 is large, the reactive functional groups are few, so that interface bonding is weak, dispersibility is poor, and the uniform distribution of the resin matrix is difficult, thereby reducing the mechanical strength, adhesive force and other properties of the epoxy resin, as in the patent technical document CN115286797B, a surface treating agent for the heat-conducting filler, a preparation method and application thereof are provided.
In order to solve the problems, the surface modification of Al 2O3 can be performed through a coupling agent, so that the mechanical property of the material can be improved to a certain extent, but the surface modified Al 2O3 has different surface tension with resin, has poor compatibility with resin, so that the resin is difficult to wet and disperse on the surfaces of Al 2O3 particles, gaps exist at the interfaces of the resin, the interfacial thermal resistance of the composite material is increased, and the agglomeration of Al 2O3 in the resin is easy to be caused, as in the patent technical document CN115819845A, a filler modification method, modified filler and filled heat-conducting epoxy resin are provided.
Therefore, in view of the above related art, there is a need to develop a high thermal conductivity and high dispersibility epoxy resin composition and application thereof.
Disclosure of Invention
In view of the above, the present invention provides a high thermal conductivity and high dispersibility epoxy resin composition and application thereof, so as to solve the problems of poor thermal conductivity of epoxy resin and poor dispersibility of inorganic filler in epoxy molding compound in the prior art.
Based on the above purpose, the invention provides a high-heat-conductivity high-dispersibility epoxy resin composition and application thereof.
The epoxy resin composition with high heat conductivity and high dispersibility is prepared from the following raw materials in parts by mass: 4-10 parts of epoxy resin, 2-10 parts of phenolic resin, 70-95 parts of inorganic filler, 0.1-0.3 part of colorant, 0.2-0.6 part of release agent, 0.3-1 part of coupling agent, 0.05-0.5 part of curing accelerator, 0.2-1.5 part of reactive stress modifier, 0.2-1.5 part of dispersing agent and 0.2-1.5 part of external dispersing agent;
The structural formula of the dispersing agent is as follows:
Wherein the value range of n is 30-50;
The structural formula of the external dispersing agent is as follows:
Wherein x: y=3:7, and the value range of x is 10-30;
preferably, the epoxy resin is any one of ortho-resol type epoxy resin, dicyclopentadiene type epoxy resin, polyaromatic epoxy resin, polyfunctional epoxy resin, biphenyl type epoxy resin, naphthol phenolic epoxy resin and thioether type epoxy resin.
Preferably, the phenolic resin is any one of phenol ether phenolic resin, o-methyl phenolic resin, biphenyl phenolic resin, polyaromatic phenolic resin and phenol aralkyl phenolic resin.
Preferably, the inorganic filler is obtained by mixing alumina and crystal angle silica in a mass ratio of 77-82:8, wherein the maximum size of the alumina is 70 mu m, the maximum size of the crystal angle silica is 10 mu m, and the colorant is carbon black.
Preferably, the release agent is a wax-based compound, and more preferably, the release agent is any one of a palm wax, a montan ester wax, a polyethylene wax, an oxidized polyethylene wax, and a polyamide wax.
Preferably, the coupling agent is any one of a mercapto-type siloxane coupling agent, an amino-type siloxane coupling agent and an epoxy-type siloxane coupling agent.
Preferably, the curing accelerator is any one of an imidazole compound, a tertiary amine compound, and an organic phosphine compound.
Preferably, the reactive stress modifier is any one of carboxyl silicone oil, amino silicone oil and epoxy silicone oil.
Preferably, the preparation method of the dispersing agent comprises the following steps:
Adding P 2O5 and toluene into a flask, adding methoxy polyethylene glycol and acetone, raising the temperature to 58-62 ℃ under stirring, keeping for 1.8-2.2h, evaporating the acetone by a distillation device, adding distilled water, raising the temperature to 88-92 ℃ and hydrolyzing for 0.8-1.2h, and finally removing the toluene to obtain the dispersing agent;
The mass ratio of the P 2O5 to the toluene to the methoxy polyethylene glycol to the acetone to the distilled water is 0.1-0.2:0.4-0.6-20:35-45:35-45:0.8-1.
Preferably, the preparation method of the external dispersing agent comprises the following steps:
Adding an initiator and potassium hydroxide into a reaction kettle under the atmosphere of nitrogen, adding ethylene oxide and propylene oxide which are uniformly mixed, reacting for 8-10 hours at 100-110 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
The mass ratio of the initiator to the potassium hydroxide to the ethylene oxide is 0.24-0.28:0.2-0.3:2-4, wherein the initiator is any one of 1, 2-propylene glycol, n-butanol and n-octanol.
The application of the epoxy resin composition with high heat conductivity and high dispersibility is used in the fields of chip packaging, semiconductor packaging, electronic devices and electromechanical product packaging protection.
The invention has the beneficial effects that:
When the dispersing agent and the external dispersing agent are added in a blending way, the two additives have synergistic effect, the external dispersing agent has low viscosity, good fluidity and high lipophilicity, can be rapidly dispersed and flowed in a system, reduces the viscosity of the whole system, enables resin in unit volume to be filled with more fillers, reduces the cost, improves the processing performance in the back-stage molding process, and can be adhered to the surfaces of the fillers under the action of the external dispersing agent, thereby enhancing the compatibility between filler particles and a resin matrix, enabling the fillers to be uniformly distributed in the resin, and greatly improving the comprehensive performance of products.
The dispersing agent provided by the invention can convert the surface from a solid-gas interface to a solid-liquid interface when coated on the surface of filler particles, so that the dispersing agent has a certain defoaming effect, the problem of air holes caused by improper packing in the processing process of a final product can be effectively solved, the layering and the flash are effectively reduced in the actual packaging process due to stronger interface affinity, the expansion coefficient can be properly reduced, and the cracking resistance effect can be improved in the cold and hot circulation process, thereby improving the product stability.
The dispersing agent provided by the invention has a good dispersing effect on the colorant carbon black, can effectively solve the problem that the carbon black is easy to agglomerate and causes surface defects caused by mold flow marks in the packaging process, and ensures that the product has no color difference, no dirt and added gloss and improves leveling property.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
The sources or properties of the raw materials used in the examples and comparative examples of the present invention are as follows:
methoxy polyethylene glycol is purchased from sea-safe petrochemical plant in Jiangsu province and has the model number of MPEG-350.
Example 1: a preparation method of a high-heat-conductivity high-dispersibility epoxy resin composition comprises the following steps:
S1, adding 0.1g P 2O5 g of toluene and 0.4g of toluene into a flask, adding 35g of methoxypolyethylene glycol and 35g of acetone, raising the temperature to 58 ℃ under stirring, keeping for 1.8h, steaming off the acetone by using a distillation device, adding 0.8g of distilled water, raising the temperature to 88 ℃ and hydrolyzing for 0.8h, and finally removing the toluene to obtain the dispersing agent;
S2, adding 0.24g of 1, 2-propylene glycol and 0.2g of potassium hydroxide into a reaction kettle under the nitrogen atmosphere, adding 2g of ethylene oxide and 6.15g of propylene oxide which are uniformly mixed, reacting for 8 hours at 100 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
S3, sequentially adding 5g of o-cresol formaldehyde epoxy resin NPCN-702, 3g of phenol ether phenolic resin, 77g of aluminum oxide with the largest dimension of 70 mu m, 8g of crystalline silicon dioxide with the largest dimension of 10 mu m, 0.2g of palm wax, 0.2g of oxidized polyethylene wax, 0.3g of alkylsilane, 0.05g of 2, 4-diamino-6- [2- (2-methyl-1-imidazole) ethyl ] -1,3, 5-triazine, 0.2g of carboxyl silicone oil, 0.1g of carbon black, 0.2g of dispersing agent and 0.2g of external dispersing agent into a high-speed stirrer, uniformly mixing, melting and mixing on an open rubber mixer with the largest dimension of 10 mu m, taking down the uniformly mixed materials from the open rubber mixer, cooling and crushing to obtain powdery materials, and finally preforming into cakes to obtain the epoxy resin composition.
Example 2: a preparation method of a high-heat-conductivity high-dispersibility epoxy resin composition comprises the following steps:
s1, adding 0.13g P 2O5 g and 0.47g of toluene into a flask, adding 38g of methoxypolyethylene glycol and 38g of acetone, raising the temperature to 59 ℃ under stirring, keeping for 1.9h, steaming off the acetone by using a distillation device, adding 0.87g of distilled water, raising the temperature to 89 ℃ and hydrolyzing for 1.0h, and finally removing the toluene to obtain the dispersing agent;
S2, adding 0.26g of n-butanol and 0.23g of potassium hydroxide into a reaction kettle under a nitrogen atmosphere, adding 2.7g of ethylene oxide and 8.3g of propylene oxide which are uniformly mixed, reacting for 8.7 hours at 103 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
S3, sequentially adding 6g of biphenyl epoxy resin BNPE-3501LL, 5g of o-methyl phenolic resin, 79g of alumina with the largest dimension of 70 mu m, 8g of crystalline silica with the largest dimension of 10 mu m, 0.3g of palm wax, 0.3g of oxidized polyethylene wax, 0.5g of aminosilane, 0.2g of 2, 4-diamino-6- [2- (2-methyl-1-imidazole) ethyl ] -1,3, 5-triazine, 0.6g of amino silicone oil, 0.2g of carbon black, 0.3g of dispersing agent and 0.3g of external dispersing agent into a high-speed mixer, uniformly mixing, melting and mixing on an open rubber mixer with the largest dimension of 10 mu m, taking down the uniformly mixed materials from the open rubber mixer, cooling and crushing to obtain powdery materials, and finally preforming into cakes to obtain the epoxy resin composition.
Example 3: a preparation method of a high-heat-conductivity high-dispersibility epoxy resin composition comprises the following steps:
S1, adding 0.16g P 2O5 g and 0.54g of toluene into a flask, adding 42g of methoxypolyethylene glycol and 42g of acetone, raising the temperature to 61 ℃ under stirring, keeping for 2.1h, steaming off the acetone by using a distillation device, adding 0.94g of distilled water, raising the temperature to 91 ℃ and hydrolyzing for 1.1h, and finally removing the toluene to obtain the dispersing agent;
S2, adding 0.27g of n-octanol and 0.26g of potassium hydroxide into a reaction kettle under the atmosphere of nitrogen, adding 3.4g of ethylene oxide and 10.46g of propylene oxide which are uniformly mixed, reacting for 9.4 hours at 106 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
S3, sequentially adding 8g of bisphenol A epoxy resin E-12, 8g of biphenyl phenolic resin, 81g of alumina with the largest dimension of 70 mu m, 8g of crystalline silica with the largest dimension of 10 mu m, 0.4g of palm wax, 0.1g of oxidized polyethylene wax, 0.1g of phenylsilane, 0.35g of 2, 4-diamino-6- [2- (2-methyl-1-imidazole) ethyl ] -1,3, 5-triazine, 1.0g of epoxy silicone oil, 0.25g of carbon black, 0.5g of dispersing agent and 0.5g of external dispersing agent into a high-speed mixer, uniformly mixing, melting and mixing on an open rubber mixer with the largest dimension of 10 mu m, taking down the uniformly mixed materials from the open rubber mixer, cooling and crushing to obtain powdery materials, and finally preforming into cakes to obtain the epoxy resin composition.
Example 4: a preparation method of a high-heat-conductivity high-dispersibility epoxy resin composition comprises the following steps:
S1, adding 0.2g P 2O5 g of toluene and 0.6g of toluene into a flask, adding 45g of methoxypolyethylene glycol and 45g of acetone, raising the temperature to 62 ℃ under stirring, keeping for 2.2h, steaming off the acetone by using a distillation device, adding 1g of distilled water, raising the temperature to 92 ℃ and hydrolyzing for 1.2h, and finally removing the toluene to obtain the dispersing agent;
S2, adding 0.28g of n-octanol and 0.3g of potassium hydroxide into a reaction kettle under the atmosphere of nitrogen, adding 4g of ethylene oxide and 12.3g of propylene oxide which are uniformly mixed, reacting for 10 hours at 110 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
S3, sequentially adding 10g of o-cresol formaldehyde epoxy resin NPCN-702, 10g of phenol ether phenolic resin, 82g of alumina with the largest dimension of 70 mu m, 8g of crystalline silica with the largest dimension of 10 mu m, 0.5g of palm wax, 0.1g of oxidized polyethylene wax, 1.0g of mercaptosilane, 0.5g of 2, 4-diamino-6- [2- (2-methyl-1-imidazole) ethyl ] -1,3, 5-triazine, 1.5g of epoxy silicone oil, 0.3g of carbon black, 0.75g of dispersing agent and 0.75g of external dispersing agent into a high-speed mixer, uniformly mixing, melting and mixing on an open rubber mixer with the largest dimension of 10 mu m, taking down the uniformly mixed materials from the open rubber mixer, cooling and crushing to obtain powdery cakes, and finally preforming to obtain the epoxy resin composition.
Comparative example 1:
In this comparative example, as compared with example 1, the dispersing agent and the external dispersing agent were not added in the preparation process of the epoxy resin composition, and the other steps and parameters were the same, and the detailed description of this comparative example was not repeated, so that the epoxy resin composition was finally prepared.
Comparative example 2:
in this comparative example, no dispersant was added in the preparation process of the epoxy resin composition as compared with example 1, and the other steps and parameters were the same, and the detailed description of this comparative example was not repeated, to finally prepare the epoxy resin composition.
Comparative example 3:
the comparative example was not added with an external dispersant in the preparation process of the epoxy resin composition as compared with example 1, and the other steps and parameters were the same, and the comparative example was not repeated, thus finally preparing the epoxy resin composition.
Comparative example 4: a method of preparing an epoxy composition comprising the steps of:
S1, adding 0.1g P 2O5 g of toluene and 0.4g of toluene into a flask, adding 35g of methoxypolyethylene glycol and 35g of acetone, raising the temperature to 58 ℃ under stirring, keeping for 1.8h, steaming off the acetone by using a distillation device, adding 0.8g of distilled water, raising the temperature to 88 ℃ and hydrolyzing for 0.8h, and finally removing the toluene to obtain the dispersing agent;
S2, adding 0.24g of 1, 2-propanediol and 0.2g of potassium hydroxide into a reaction kettle under the atmosphere of nitrogen, adding 6.15g of ethylene oxide and 2g of propylene oxide which are uniformly mixed, reacting for 8 hours at 100 ℃, and neutralizing, dehydrating, drying and filtering after the reaction is finished to obtain an external dispersing agent;
S3, adding 4g of o-cresol formaldehyde epoxy resin NPCN-702, 2g of phenol ether phenolic resin, 77g of aluminum oxide with the largest dimension of 70 mu m, 8g of crystalline silicon dioxide with the largest dimension of 10 mu m, 0.2g of palm wax, 0.2g of oxidized polyethylene wax, 0.3g of alkylsilane, 0.05g of 2, 4-diamino-6- [2- (2-methyl-1-imidazole) ethyl ] -1,3, 5-triazine, 0.2g of carboxyl silicone oil, 0.1g of carbon black, 0.2g of dispersing agent and 0.2g of external dispersing agent into a high-speed stirrer in sequence, uniformly mixing, melting and mixing on an open rubber mixer with the largest dimension of 10 mu m, taking down the uniformly mixed materials from the open rubber mixer, cooling and crushing to obtain powdery materials, and finally preforming into cakes to obtain the epoxy resin composition.
Performance test:
The spiral flow length, gelation time, flash, viscosity, flexural strength, hot hardness, appearance test and thermal conductivity of the epoxy resin compositions prepared in examples 2 to 6 and comparative examples 1 to 2 were measured with reference to GB/T40564-2021 Standard of method for measuring epoxy Plastic Package for electronic packaging;
TCT test: the epoxy resin compositions prepared in examples 2 to 6 and comparative examples 1 to 2 were pressed by a molding press into a product having a height of 50mm, an inner diameter of 25mm and an outer diameter of 30mm, and molded under the conditions of a metal mold temperature of 175.+ -. 2 ℃ and an injection pressure of 80.+ -. 2kg/cm 2 and a curing time of 150s, and the molded product was post-cured at a temperature of 175.+ -. 2 ℃ for 6 hours and then cooled at room temperature, and then put into a cold and hot cycle impact test box to be cycled from-35 ℃ to 130 ℃ for 2 hours for 300 cycles, and the cracking condition of the product was examined, and the results are shown in the following table 1:
Table 1 summary of experimental results
Data analysis:
As can be seen from table 1, when the dispersing agent and the external dispersing agent are added alone, the additive does not wet the surface of the filler well, which is manifested by short flow length, excessive flash, low normal temperature strength, large brittleness of the product, excessive flash in the later stage of packaging, difficult removal, influence on electroplating effect, and risk of breakage during die opening and application, and the comprehensive performance is poor compared with that of the conventional product formulation.
It can be seen from examples 1, comparative examples 1 and 4 that the relationship between the amounts of the dispersing agent and the external dispersing agent and the amounts thereof has a key effect on the overall properties of the final product, which is manifested in that the final product has poor overall properties when the amounts of the dispersing agent and the external dispersing agent and the amounts of ethylene oxide and propylene oxide added are not added to the system.
However, as is clear from examples 2 to 4, when the dispersant and the external dispersant are added in a blending manner, the two additives have a synergistic effect, the external dispersant has poor compatibility with the matrix, the dispersant rapidly disperses and flows in the system, the viscosity of the whole system is reduced, and the processability is improved in the subsequent molding process. Under the action of the external dispersing agent, the dispersing agent can be attached to the surface of the filler, so that the compatibility between filler particles and a resin matrix is enhanced, the filler can be uniformly distributed in the resin, the comprehensive performance of the product is greatly improved, the flow length is increased, the curing time is prolonged, the flash is reduced, the strength is increased, the modulus is reduced while the strength is increased, the hardness is increased when the product is heated, the heat conductivity is improved, in addition, the expansion coefficient can be properly reduced in the application of the product due to the strong interface affinity of the wetting dispersing agent, the cracking resistance effect can be improved in the cold and hot circulation process, no crack is observed on the surface by using a microscope, and the product stability can be improved, so that the TCT test can be passed.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (8)
1. The high-heat-conductivity high-dispersibility epoxy resin composition is characterized by being prepared from the following raw materials in parts by mass: 4-10 parts of epoxy resin, 2-10 parts of phenolic resin, 70-95 parts of inorganic filler, 0.1-0.3 part of colorant, 0.2-0.6 part of release agent, 0.3-1 part of coupling agent, 0.05-0.5 part of curing accelerator, 0.2-1.5 part of reactive stress modifier, 0.2-1.5 part of dispersing agent and 0.2-1.5 part of external dispersing agent;
The structural formula of the dispersing agent is as follows:
Wherein the value range of n is 30-50;
The structural formula of the external dispersing agent is as follows:
wherein x: y=3:7, and x has a value in the range of 10 to 30.
2. The epoxy resin composition of claim 1, wherein the epoxy resin is any one of an ortho-resol type epoxy resin, a dicyclopentadiene type epoxy resin, a poly-aromatic epoxy resin, a multi-functional epoxy resin, a biphenyl type epoxy resin, a naphthol novolac type epoxy resin, and a thioether type epoxy resin.
3. The epoxy resin composition with high thermal conductivity and high dispersibility according to claim 1, wherein the phenolic resin is any one of phenol ether phenolic resin, o-methyl phenolic resin, biphenyl phenolic resin, polyaromatic phenolic resin and phenol aralkyl phenolic resin.
4. The high thermal conductivity and high dispersibility epoxy resin composition according to claim 1, wherein the inorganic filler is obtained by mixing alumina and crystal angular silica in a mass ratio of 77-82:8, the maximum size of the alumina is 70 μm, the maximum size of the crystal angular silica is 10 μm, and the colorant is carbon black.
5. The high thermal conductivity and high dispersibility epoxy resin composition according to claim 1, wherein the mold release agent is any one of palm wax, montan ester wax, polyethylene wax, oxidized polyethylene wax and polyamide wax.
6. The high thermal conductivity and high dispersibility epoxy resin composition according to claim 1, wherein the coupling agent is any one of a mercapto-type siloxane coupling agent, an amino-type siloxane coupling agent and an epoxy-type siloxane coupling agent.
7. The high-heat-conductivity high-dispersibility epoxy resin composition according to claim 1, wherein the curing accelerator is any one of an imidazole compound, a tertiary amine compound and an organic phosphine compound, and the reactive stress modifier is one or more of carboxyl silicone oil, amino silicone oil and epoxy silicone oil.
8. Use of the high thermal conductivity and high dispersibility epoxy resin composition according to any one of claims 1 to 7, for chip packaging, semiconductor packaging, electronic devices and in the field of packaging protection of electromechanical products.
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