CN106065164A - A kind of thermosetting encapsulation environment-friendly resin materials - Google Patents
A kind of thermosetting encapsulation environment-friendly resin materials Download PDFInfo
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Abstract
The invention discloses a kind of thermosetting encapsulation environment-friendly resin materials, it is made up of following raw material: 2,2 ' [(1 methyl ethylidene) double (4,1 phenyl ene oxymethylene)] bisoxirane and di-2-ethylhexylphosphine oxide (1,3 benzenediol) four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic anhydride grafting ethylene propylene diene rubber, polysiloxanes, oil base potassium amino acid, sodium metasilicate, paraffin, carbon fiber, poly maleimide, phthalic acid, silica, additive.The thermosetting encapsulation environment-friendly resin materials that the present invention prepares has excellent combination property, can be good at being applied to technical field of electronic components, plays good sealing effectiveness.
Description
Technical field
The invention belongs to technical field of electronic components and encapsulating material preparing technical field, be specifically related to a kind of sealing and use
Thermocurable environment-friendly resin materials.
Background technology
Semiconductor packages generally uses resin as encapsulating material, by diode, transistor, integrated circuit, collects on a large scale
Become the semiconductor devices such as circuit and super large-scale integration and external environment to isolate, with protect semiconductor devices avoid external force or
The damage that environmental factor causes.Due to epoxy resin be provided that compared with other thermosetting resins outstanding plasticity, adhesive force,
Insulation characterisitic, mechanical property and fire resistance characteristic, so epoxy resin obtains widely should as the encapsulating material of semiconductor devices
With.Such as U.S. Patent No. 6342309 discloses a kind of composition epoxy resin, and said composition includes novolac type epoxy
Resin, bromination phenol aldehyde type epoxy resin and phenolic resin.The liquidity scale of said composition and reaction hardening index can be preferably
Meet general semiconductor packages demand.
In microelectronic integrated circuit and high-power rectifying device, intensive countless minute sized element produces a large amount of
Heat, because of between chip with encapsulating material not mating of thermal coefficient of expansion and the thermal stress fatigue and the heat dispersion that cause be not good
And the chip overheating causing has become the main failure forms of microelectronic circuit and device.Being packaged into restrict of electronic component
The bottleneck problem of systematic function.According to estimates, the chip computing capability of 30% is limited by encapsulating material, its impact become and
Chip is of equal importance.So-called encapsulation refers to support and protect semiconductor chip and electronic circuit with substrate, base plate, shell, with
When play heat radiation and/or conduction effect.Electronic package material, as a kind of base electronic component, is used for carrying electronic devices and components
And phase interconnection line, therefore encapsulating material must keep good with components and parts placed on it in terms of electricity, physics, chemical property
Good coupling.Based on plastic electronic packages material is mainly with epoxy resin, organosilicon；Secondly it is organosilicon epoxy, poly-phthalimide
With liquid crystal polymer etc..The large-scale production simple, applicable of epoxy resin low price, moulding process, reliability are also higher, because of
This development recently is quickly.External at present semiconductor packages 80%-90% is replaced by epoxide resin material, especially consumer electricity
The device encapsulation almost all of sub-product uses Plastic Package, and its development prospect is very good.
Electronic package material along with circuit, the generation of electronic devices and components and produce, its development decides electronic industry
Development level.Electronic package material experienced by the evolution from metal material, ceramic material to macromolecular material, current high score
Sub-encapsulating material has become the main body of electronic package material, with thermosetting resin envelopes such as epoxy resin, phenolic resin and organosilicons
Based on package material, consumption accounts for the 90% of whole electronic package material, and towards high-performance thermoplastic macromolecule electronic package material side
To development.The thermosetting resin electronic package materials such as epoxy resin have that low price, moulding process be simple, technical maturity, can
The advantages such as allotment property is good, but the proper property of the thermosetting resins such as epoxy resin makes it there is shaping week in processing and application
Phase length, molding shrinkage compared with easily bursting when using under big, low temperature, fragility is big, various organic additive easily causes pollutions, first
The easy stress damage of device, and can not recycle, cause great pressure to environment.
Content of the invention
The present invention provides a kind of thermosetting encapsulation environment-friendly resin materials, seals dress material to solve existing semiconductor chip
Material dielectric constant, tensile strength are little, the problems such as dielectric loss reaches, weight-loss ratio is big.The thermosetting encapsulation ring that the present invention prepares
Protect resin material and there is excellent combination property, can be good at being applied to technical field of electronic components, play good close
Envelope effect.
For solving above technical problem, the present invention by the following technical solutions:
A kind of thermosetting encapsulation environment-friendly resin materials, in units of weight, is made up of following raw material: 2,2 '-[(1-methyl
Ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(Resorcinol)-four glycidol ether 168-
275 parts, tributoxyethyl phosphate 54-78 part, o-cresol formaldehyde epoxy resin A44-58 part, dioctyl phthalate 25-30
Part, maleic anhydride grafting ethylene propylene diene rubber 35-50 part, polysiloxanes 22-32 part, oil base potassium amino acid 20-26 part, sodium metasilicate
16-22 part, paraffin 26-34 part, carbon fiber 14-25 part, poly maleimide 15-20 part, phthalic acid 14-25 part, dioxy
SiClx 14-26 part, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3-5 part, modified polyacrylic acid
Ester compatilizer 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part, anhydrous gypsum stabilization agent
0.6-1.2 part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid conditioning agent 0.5-1 part, 701 powder hardening agent 0.4-0.6 parts, poly-
Close aluminium chloride flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8 part, phthalic acid two
(2-ethyl hexyl) ester plasticiser 0.5-0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol sebacates are steady
Determine agent 0.3-0.4 part, antioxidant DLPP0.3-0.4 part, styrene terminator 0.2-0.3 part, azo two isobutyric acid (acrylic acid
Ethylene glycol) ester initiator 0.3-0.5 part, di-t-butyl hexane peroxide crosslinking agent 0.3-0.4 part, polyester fiber softening agent 0.5-
0.9 part, fire retardant 0.1-0.2 part, antismoke agent 0.1-0.2 part, catalyst 0.05-0.1 part, curing agent 0.6-1.2 part, solidification promote
Enter agent 0.2-0.4 part, releasing agent 0.3-0.5 part, colouring agent 0.4-0.8 part, tackifier 0.3-0.5 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 0.6-1 part, HBCD
0.3-0.7 part, monohydroxy acrylate 0.3-0.7 part, molybdenum oxide 0.6-1.2 part, methyl acrylate 0.3-0.5 part, butanol
0.3-0.5 part, kaolin 0.6-0.9 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 0.8-1.5 part, hydroxide
Zirconium 0.8-1.5 part, talcum powder 0.4-0.8 part, aluminum oxide 0.4-0.6 part；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 240-255 DEG C in temperature, and rotating speed is stirring 6-under 300-400r/min
8min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 250-350W at microwave power, temperature is 155-175 DEG C, and rotating speed is under 250-350r/min
Stirring 3-5h, prepares mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 200-300W, and temperature is 130-150 DEG C, and rotating speed is stirring 4-6h under 300-400r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 125-145 DEG C in temperature, and rotating speed is stirring 0.8-1.2h under 200-300r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 85-95 DEG C, and molding pressure is 2-4MPa, temperature
For 100-110 DEG C, the dwell time is 25-35min, with mould Slow cooling, proceeds to drying box when temperature drops to 45-55 DEG C,
116-124 DEG C of annealing 1.5-2.5h continues solidification, destressing, naturally cools to room temperature.
Further, described catalyst is Raney nickel.
Further, described curing agent is phenol linear phenolic resin B.
Further, described curing accelerator is diazabicylo C1.
Further, described releasing agent is Brazil wax W.
Further, described colouring agent is carbon black T.
Further, described tackifier are aromatic petroleum resin.
The method have the advantages that
(1) the thermosetting encapsulation environment-friendly resin materials that the present invention prepares, has good performance, and its medium dielectric constant microwave medium reaches
More than 8.2268F/m, dielectric loss has reached less than 0.0272, weight-loss ratio has reached less than 12.48%, and tensile strength reaches
More than 61.17, there is excellent combination property, can be good at being applied to technical field of electronic components, play good
Sealing effectiveness.
(2) the thermosetting encapsulation environment-friendly resin materials that the present invention prepares is environmentally friendly, green energy conservation, has extensively
Application prospect, be the green encapsulant of a kind of innovation.
Detailed description of the invention
For ease of being more fully understood that the present invention, being illustrated by following example, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In an embodiment, described thermosetting encapsulation environment-friendly resin materials, in units of weight, by following raw material system
Become: 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(Resorcinols)-
Four glycidol ether 168-275 parts, tributoxyethyl phosphate 54-78 part, o-cresol formaldehyde epoxy resin A44-58 part, adjacent benzene two
Formic acid dioctyl ester 25-30 part, maleic anhydride grafting ethylene propylene diene rubber 35-50 part, polysiloxanes 22-32 part, oil base amino acid
Potassium 20-26 part, sodium metasilicate 16-22 part, paraffin 26-34 part, carbon fiber 14-25 part, poly maleimide 15-20 part, adjacent benzene two
Acetic acid 14-25 part, silica 1 4-26 part, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3-
5 parts, modified polyacrylate compatilizer 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part,
Anhydrous gypsum stabilization agent 0.6-1.2 part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid conditioning agent 0.5-1 part, 701 powder strengthenings
Agent 0.4-0.6 part, aluminium polychloride flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8
Part, phthalic acid two (2-ethyl hexyl) ester plasticiser 0.5-0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidines-
4-alcohol sebacate stabilizer 0.3-0.4 part, antioxidant DLPP0.3-0.4 part, styrene terminator 0.2-0.3 part, azo two
Isobutyric acid (acrylic acid ethylene glycol) ester initiator 0.3-0.5 part, di-t-butyl hexane peroxide crosslinking agent 0.3-0.4 part, polyester
Softening agent for fibres 0.5-0.9 part, fire retardant 0.1-0.2 part, antismoke agent 0.1-0.2 part, Raney nickel 0.05-0.1 part, phenol line
Property phenolic resin curative B0.6-1.2 part, diazabicylo C1 curing accelerator 0.2-0.4 part, Brazil wax W releasing agent
0.3-0.5 part, carbon black T colouring agent 0.4-0.8 part, aromatic petroleum resin tackifier 0.3-0.5 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 0.6-1 part, HBCD
0.3-0.7 part, monohydroxy acrylate 0.3-0.7 part, molybdenum oxide 0.6-1.2 part, methyl acrylate 0.3-0.5 part, butanol
0.3-0.5 part, kaolin 0.6-0.9 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 0.8-1.5 part, hydroxide
Zirconium 0.8-1.5 part, talcum powder 0.4-0.8 part, aluminum oxide 0.4-0.6 part；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 240-255 DEG C in temperature, and rotating speed is stirring 6-under 300-400r/min
8min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 250-350W at microwave power, temperature is 155-175 DEG C, and rotating speed is under 250-350r/min
Stirring 3-5h, prepares mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 200-300W, and temperature is 130-150 DEG C, and rotating speed is stirring 4-6h under 300-400r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 125-145 DEG C in temperature, and rotating speed is stirring 0.8-1.2h under 200-300r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 85-95 DEG C, and molding pressure is 2-4MPa, temperature
For 100-110 DEG C, the dwell time is 25-35min, with mould Slow cooling, proceeds to drying box when temperature drops to 45-55 DEG C,
116-124 DEG C of annealing 1.5-2.5h continues solidification, destressing, naturally cools to room temperature.
Embodiment 1
A kind of thermosetting encapsulation environment-friendly resin materials, in units of weight, is made up of following raw material: 2,2 '-[(1-methyl
Ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(Resorcinol)-four glycidol ether 220
Part, tributoxyethyl phosphate 65 parts, o-cresol formaldehyde epoxy resin A50 part, dioctyl phthalate 25 parts, maleic anhydride connect
Branch ethylene propylene diene rubber 42 parts, polysiloxanes 27 parts, oil base potassium amino acid 23 parts, sodium metasilicate 19 parts, 30 parts of paraffin, carbon fiber 20
Part, poly maleimide 17 parts, phthalic acid 20 parts, silica 20 parts, N-2-(amino-ethyl)-3-amino propyl methyl
Dimethoxysilane coupling agent 4 parts, modified polyacrylate compatilizer 4 parts, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl group
Phenol) 1.2 parts, anhydrous gypsum stabilization agent 0.9 part, DCP bridging agent 0.9 part, esters of acrylic acid conditioning agent 0.8 part, 701 powder strengthenings
Agent 0.5 part, aluminium polychloride flocculation agent 0.5 part, styrene butadiene thermoplasticelastomer toughener 0.7 part, phthalic acid
Two (2-ethyl hexyl) ester plasticiser 0.7 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol sebacates are stable
Agent 0.3 part, antioxidant DLPP0.3 part, styrene terminator 0.2 part, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator
0.4 part, di-t-butyl hexane peroxide crosslinking agent 0.3 part, polyester fiber softening agent 0.7 part, fire retardant 0.1 part, antismoke agent 0.1
Part, Raney nickel 0.08 part, phenol linear phenolic resin curing agent B0.9 part, diazabicylo C1 curing accelerator 0.3 part, bar
Western palm wax W releasing agent 0.4 part, carbon black T colouring agent 0.6 part, aromatic petroleum resin tackifier 0.4 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 0.8 part, HBCD 0.5
Part, monohydroxy acrylate 0.5 part, molybdenum oxide 0.9 part, methyl acrylate 0.4 part, 0.4 part of butanol, kaolin 0.8 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 1.2 parts, zirconium hydroxide 1.2
Part, talcum powder 0.6 part, 0.5 part of aluminum oxide；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 250 DEG C in temperature, and rotating speed is stirring 7min under 350r/min, prepares mixed
Compound A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 300W at microwave power, temperature is 165 DEG C, and rotating speed is stirring 4h under 3000r/min, prepares
Mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 250W, and temperature is 140 DEG C, and rotating speed is stirring 5h under 350r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 135 DEG C in temperature, and rotating speed is stirring 1h under 250r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 90 DEG C, and molding pressure is 3MPa, and temperature is 105
DEG C, the dwell time is 30min, with mould Slow cooling, proceeds to drying box when temperature drops to 50 DEG C, and 120 DEG C of annealing 2h continue
Solidification, destressing, naturally cool to room temperature.
Embodiment 2
A kind of thermosetting encapsulation environment-friendly resin materials, in units of weight, 2,2 '-[(1-methyl ethylidene) is double, and (4,1-is sub-
Phenyl formaldehyde)] bisoxirane and methylene-bis-(Resorcinol)-four glycidol ether 168 parts, tricresyl phosphate butoxy second
Ester 54 parts, o-cresol formaldehyde epoxy resin A44 part, dioctyl phthalate 25 parts, maleic anhydride grafting ethylene propylene diene rubber 35
Part, polysiloxanes 22 parts, oil base potassium amino acid 20 parts, sodium metasilicate 16 parts, 26 parts of paraffin, 14 parts of carbon fiber, poly maleimide
15 parts, phthalic acid 14 parts, silica 14 parts, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane is even
Connection agent 3 parts, modified polyacrylate compatilizer 3 parts, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8 part, nothing
Water gypsum stabilization agent 0.6 part, DCP bridging agent 0.6 part, esters of acrylic acid conditioning agent 0.5 part, 701 powder hardening agent 0.4 part, polymerization
Aluminium chloride flocculation agent 0.4 part, styrene butadiene thermoplasticelastomer toughener 0.5 part, phthalic acid two (2-ethyl hexyl)
Ester plasticiser 0.5 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol sebacate stabilizers 0.3 part, antioxygen
Agent DLPP0.3 part, styrene terminator 0.2 part, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator 0.3 part, two tertiary fourths
Base butylperoxyhexane crosslinking agent 0.3 part, polyester fiber softening agent 0.5 part, fire retardant 0.1 part, antismoke agent 0.1 part, Raney nickel
0.05 part, phenol linear phenolic resin curing agent B0.6 part, diazabicylo C1 curing accelerator 0.2 part, Brazil wax W take off
Mould agent 0.3 part, carbon black T colouring agent 0.4 part, aromatic petroleum resin tackifier 0.3 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 0.6 part, HBCD 0.3
Part, monohydroxy acrylate 0.3 part, molybdenum oxide 0.6 part, methyl acrylate 0.3 part, 0.3 part of butanol, kaolin 0.6 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 0.8 part, zirconium hydroxide 0.8
Part, talcum powder 0.4 part, 0.4 part of aluminum oxide；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 240 DEG C in temperature, and rotating speed is stirring 8min under 300r/min, prepares mixed
Compound A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 250W at microwave power, temperature is 155 DEG C, and rotating speed is stirring 5h under 250r/min, prepares
Mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 200W, and temperature is 130 DEG C, and rotating speed is stirring 6h under 300r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 125 DEG C in temperature, and rotating speed is stirring 1.2h under 200r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 85 DEG C, and molding pressure is 2MPa, and temperature is 100
DEG C, the dwell time is 35min, with mould Slow cooling, proceeds to drying box when temperature drops to 45 DEG C, and 116 DEG C of annealing 2.5h continue
Continuous solidification, destressing, naturally cool to room temperature.
Embodiment 3
A kind of thermosetting encapsulation environment-friendly resin materials, in units of weight, is made up of following raw material: 2,2 '-[(1-methyl
Ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(Resorcinol)-four glycidol ether 275
Part, tributoxyethyl phosphate 78 parts, o-cresol formaldehyde epoxy resin A58 part, dioctyl phthalate 30 parts, maleic anhydride connect
Branch ethylene propylene diene rubber 50 parts, polysiloxanes 32 parts, oil base potassium amino acid 26 parts, sodium metasilicate 22 parts, 34 parts of paraffin, carbon fiber 25
Part, poly maleimide 20 parts, phthalic acid 25 parts, silica 26 parts, N-2-(amino-ethyl)-3-amino propyl methyl
Dimethoxysilane coupling agent 5 parts, modified polyacrylate compatilizer 5 parts, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl group
Phenol) 1.4 parts, anhydrous gypsum stabilization agent 1.2 parts, DCP bridging agent 1.2 parts, esters of acrylic acid conditioning agent 1 part, 701 powder hardening agents
0.6 part, aluminium polychloride flocculation agent 0.6 part, styrene butadiene thermoplasticelastomer toughener 0.8 part, phthalic acid two
(2-ethyl hexyl) ester plasticiser 0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol sebacate stabilizers
0.4 part, antioxidant DLPP0.4 part, styrene terminator 0.3 part, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator
0.5 part, di-t-butyl hexane peroxide crosslinking agent 0.4 part, polyester fiber softening agent 0.9 part, fire retardant 0.2 part, antismoke agent 0.2
Part, Raney nickel 0.1 part, phenol linear phenolic resin curing agent B1.2 part, diazabicylo C1 curing accelerator 0.4 part, bar
Western palm wax W releasing agent 0.5 part, carbon black T colouring agent 0.8 part, aromatic petroleum resin tackifier 0.5 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 1 part, HBCD 0.7 part,
Monohydroxy acrylate 0.7 part, molybdenum oxide 1.2 parts, methyl acrylate 0.5 part, 0.5 part of butanol, kaolin 0.9 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 1.5 parts, zirconium hydroxide 1.5
Part, talcum powder 0.8 part, 0.6 part of aluminum oxide；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 255 DEG C in temperature, and rotating speed is stirring 6min under 400r/min, prepares mixed
Compound A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 350W at microwave power, temperature is 175 DEG C, and rotating speed is stirring 3h under 350r/min, prepares
Mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 300W, and temperature is 150 DEG C, and rotating speed is stirring 4h under 400r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 145 DEG C in temperature, and rotating speed is stirring 0.8h under 300r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 95 DEG C, and molding pressure is 4MPa, and temperature is 110
DEG C, the dwell time is 25min, with mould Slow cooling, proceeds to drying box when temperature drops to 55 DEG C, and 124 DEG C of annealing 1.5h continue
Continuous solidification, destressing, naturally cool to room temperature.
Prepare thermosetting encapsulation environment-friendly resin materials to embodiment 1-3 and carry out performance test, test event and method
As follows:
Dielectric properties are tested: use accurate dielectric constant and dielectric loss to prepared composite for the LCR digital electric bridge to carry out
Test；
Composite thermal weight loss is tested: adopts TA SDTQ600 type thermogravimetric synchronization discrepancy thermal analyzer and carries out TG analysis to composite；
Mechanics Performance Testing: use the tensile force to prepared composite for the SANS5105 type microcomputer controlled electronic universal tester
Learning performance to test, the standard of test is according to GB-1446-83 " the generals of test methods for properties of fiberreinforced plastics " and GB-
1040-79 " plastic tensile method for testing performance ".Clamping gauge length is 100mm, and loading velocity is 5mm/min, each sample testing 3
Secondary, take average.
Test result see table.
| Embodiment | Dielectric constant (F/m) | Dielectric loss | Weight-loss ratio (%) | Tensile strength (MPa) |
| 1 | 8.8356 | 0.0255 | 11.07 | 66.53 |
| 2 | 8.2268 | 0.0272 | 12.48 | 61.17 |
| 3 | 9.1953 | 0.0158 | 9.2 | 71.89 |
From upper table result it can be seen that the thermosetting encapsulation environment-friendly resin materials for preparing of the present invention, have good
Performance, its medium dielectric constant microwave medium has reached more than 8.2268F/m, and dielectric loss has reached less than 0.0272, and weight-loss ratio reaches
Less than 12.48%, tensile strength has reached more than 61.17, has excellent combination property, can be good at being applied to electronics unit
Device arts, plays good sealing effectiveness.
Above content it cannot be assumed that the present invention be embodied as be confined to these explanation, technology belonging to the present invention is led
For the those of ordinary skill in territory, without departing from the inventive concept of the premise, some simple deduction or replace can also be made,
All should be considered as belonging to the scope of patent protection that the present invention is determined by the claims submitted to.
Claims (7)
1. a thermosetting encapsulation environment-friendly resin materials, it is characterised in that in units of weight, is made up of following raw material:
2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(Resorcinol)-four contracting
Water glycerin ether 168-275 part, tributoxyethyl phosphate 54-78 part, o-cresol formaldehyde epoxy resin A44-58 part, phthalic acid
Dioctyl ester 25-30 part, maleic anhydride grafting ethylene propylene diene rubber 35-50 part, polysiloxanes 22-32 part, oil base potassium amino acid 20-
26 parts, sodium metasilicate 16-22 part, paraffin 26-34 part, carbon fiber 14-25 part, poly maleimide 15-20 part, phthalic acid
14-25 part, silica 1 4-26 part, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3-5 part,
Modified polyacrylate compatilizer 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part, anhydrous
Gypsum stabilization agent 0.6-1.2 part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid conditioning agent 0.5-1 part, 701 powder hardening agents
0.4-0.6 part, aluminium polychloride flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8 part,
Phthalic acid two (2-ethyl hexyl) ester plasticiser 0.5-0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-
Alcohol sebacate stabilizer 0.3-0.4 part, antioxidant DLPP0.3-0.4 part, styrene terminator 0.2-0.3 part, azo two are different
Butyric acid (acrylic acid ethylene glycol) ester initiator 0.3-0.5 part, di-t-butyl hexane peroxide crosslinking agent 0.3-0.4 part, polyester are fine
Dimension softening agent 0.5-0.9 part, fire retardant 0.1-0.2 part, antismoke agent 0.1-0.2 part, catalyst 0.05-0.1 part, curing agent 0.6-
1.2 parts, curing accelerator 0.2-0.4 part, releasing agent 0.3-0.5 part, colouring agent 0.4-0.8 part, tackifier 0.3-0.5 part；
Described fire retardant, in units of weight portion, is made up of following raw material: antimony oxide 0.6-1 part, HBCD
0.3-0.7 part, monohydroxy acrylate 0.3-0.7 part, molybdenum oxide 0.6-1.2 part, methyl acrylate 0.3-0.5 part, butanol
0.3-0.5 part, kaolin 0.6-0.9 part；
Described antismoke agent, in units of weight portion, is made up of following raw material: dibutyl tin laurate 0.8-1.5 part, hydroxide
Zirconium 0.8-1.5 part, talcum powder 0.4-0.8 part, aluminum oxide 0.4-0.6 part；
The preparation method of described thermosetting encapsulation environment-friendly resin materials, comprises the following steps:
S1: by 2,2 '-[(1-methyl ethylidene) double (4,1-phenyl ene oxymethylene)] bisoxirane and methylene-bis-(1,3-benzene
Diphenol)-four glycidol ethers, tributoxyethyl phosphate, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, maleic acid
Acid anhydride grafting ethylene propylene diene rubber, polysiloxanes mixing, be 240-255 DEG C in temperature, and rotating speed is stirring 6-under 300-400r/min
8min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, paraffin, carbon fine in the mixture A that step 1 prepares
Dimension, poly maleimide, phthalic acid, silica, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane
Coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous gypsum stabilize
Agent, DCP bridging agent, esters of acrylic acid conditioning agent, azo two isobutyric acid (acrylic acid ethylene glycol) ester initiator, di-t-butyl peroxide
Changing hexane crosslinking agent, catalyst, being 250-350W at microwave power, temperature is 155-175 DEG C, and rotating speed is under 250-350r/min
Stirring 3-5h, prepares mixture B；
S3: add 701 powder hardening agents, aluminium polychloride flocculation agent, styrene-butadiene in the mixture B that step 2 prepares
Thermoplastic elastomer toughening agent, phthalic acid two (2-ethyl hexyl) ester plasticiser, polyester fiber softening agent, tackifier, surpassing
Acoustic power is 200-300W, and temperature is 130-150 DEG C, and rotating speed is stirring 4-6h under 300-400r/min, prepares mixture C；
S4: add double-1-decane epoxide-2 in the mixture C that step 3 prepares, 2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer, antioxidant DLPP, styrene terminator, fire retardant, antismoke agent, curing agent, curing accelerator, releasing agent,
Toner, is 125-145 DEG C in temperature, and rotating speed is stirring 0.8-1.2h under 200-300r/min, prepares mixture D；
S5: the mixture D that step 4 prepares is joined compression molding on vulcanizing press, prepares semiconductor chip sealing heat
Curability environment-friendly resin material, wherein preparation technology parameter is: precuring temperature is 85-95 DEG C, and molding pressure is 2-4MPa, temperature
For 100-110 DEG C, the dwell time is 25-35min, with mould Slow cooling, proceeds to drying box when temperature drops to 45-55 DEG C,
116-124 DEG C of annealing 1.5-2.5h continues solidification, destressing, naturally cools to room temperature.
2. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described catalyst is nickel
Catalyst.
3. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described curing agent is benzene
Phenol linear phenolic resin B.
4. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described curing accelerator
For diazabicylo C1.
5. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described releasing agent is bar
Western palm wax W.
6. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described colouring agent is charcoal
Black T.
7. thermosetting encapsulation environment-friendly resin materials according to claim 1, it is characterised in that described tackifier are virtue
Fragrant race Petropols.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762288A (en) * | 2019-02-12 | 2019-05-17 | 青岛科技大学 | A kind of flame-proof highly anti-flush polyphenylacetylene material and preparation method thereof with good photo and thermal stability |
| CN114032036A (en) * | 2021-11-12 | 2022-02-11 | 上海本诺电子材料有限公司 | High-temperature-resistant UV (ultraviolet) curing sealant and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104987666A (en) * | 2015-06-30 | 2015-10-21 | 苏州洋杰电子有限公司 | Epoxy resin-polymaleimide composite semiconductor packaging material and preparation method thereof |
-
2016
- 2016-07-26 CN CN201610594512.4A patent/CN106065164A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104987666A (en) * | 2015-06-30 | 2015-10-21 | 苏州洋杰电子有限公司 | Epoxy resin-polymaleimide composite semiconductor packaging material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762288A (en) * | 2019-02-12 | 2019-05-17 | 青岛科技大学 | A kind of flame-proof highly anti-flush polyphenylacetylene material and preparation method thereof with good photo and thermal stability |
| CN114032036A (en) * | 2021-11-12 | 2022-02-11 | 上海本诺电子材料有限公司 | High-temperature-resistant UV (ultraviolet) curing sealant and preparation method thereof |
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