CN106189090A - A kind of novel seal heat-curing resin material - Google Patents
A kind of novel seal heat-curing resin material Download PDFInfo
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- CN106189090A CN106189090A CN201610593806.5A CN201610593806A CN106189090A CN 106189090 A CN106189090 A CN 106189090A CN 201610593806 A CN201610593806 A CN 201610593806A CN 106189090 A CN106189090 A CN 106189090A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses a kind of novel seal heat-curing resin material, 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 Benzodiazepines) four glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate, phosphate ester, polysiloxanes, oil base potassium amino acid, sodium metasilicate, chlorinated paraffin, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, additive.The novel seal heat-curing resin material that the present invention prepares has the combination property of excellence, it is possible to is well 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 novel close
Envelope uses heat-curing resin material.
Background technology
Semiconductor packages generally uses resin as encapsulating material, by diode, transistor, integrated circuit, collects on a large scale
Become the semiconductor device such as circuit and super large-scale integration and external environment to isolate, with protect semiconductor device avoid external force or
The damage that environmental factors 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 device
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 are the best
And the chip overheating caused 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
Time 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.Plastic electronic packages material is mainly based on epoxy resin, organosilicon；Secondly it is organosilicon epoxy, poly-phthalimide
With liquid crystal polymer etc..Epoxy resin low price, moulding process are simple, be suitable for large-scale production, reliability is the highest, because of
This development recently is quickly.The most external semiconductor packages 80%-90% is replaced by epoxide resin material, consumer electricity
The device encapsulation almost all of sub-product uses Plastic Package, and its development prospect is the most good.
Electronic package material produces along with circuit, the generation of electronic devices and components, and its development decides electronic industry
Level of development.Electronic package material experienced by from metal material, the evolution of 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
Package material is main, and 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 molding 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.
Summary of the invention
The present invention provides a kind of novel seal heat-curing resin material, to solve existing semiconductor chip sealing dress material
Material dielectric constant, hot strength are little, the problems such as dielectric loss reaches, weight-loss ratio is big.The novel seal heat cure that the present invention prepares
Property resin material there is the combination property of excellence, it is possible to be well applied to technical field of electronic components, play good close
Envelope effect.
For solve above technical problem, the present invention by the following technical solutions:
A kind of novel seal heat-curing resin material, 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 glycidyl ether 170-
270 parts, styrene and Oleum Verniciae fordii based alkyd 55-75 part, o-cresol formaldehyde epoxy resin A45-56 part, dioctyl phthalate
25-28 part, phosphate ester 35-50 part, polysiloxanes 22-32 part, oil base potassium amino acid 20-26 part, sodium metasilicate 16-22 part, chlorine
Fossil waxes 26-34 part, carbon fiber 14-25 part, poly maleimide 15-20 part, phthalic acid 14-25 part, silica 1 4-
26 parts, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3-5 part, modified polyacrylate be compatible
Agent 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part, anhydrous gypsum tranquilizer 0.6-1.2
Part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid regulator 0.5-1 part, 701 powder hardening agent 0.4-0.6 parts, aluminium polychlorid
Flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8 part, phthalic acid two (2-ethyl
Oneself) 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 isopropylformic acid. (acrylic acid ethylene glycol) ester
Initiator 0.3-0.5 part, di-t-butyl hexane peroxide cross-linking agent 0.3-0.4 part, polyester fiber softening agent 0.5-0.9 part, resistance
Combustion agent 0.1-0.2 part, antismoke agent 0.1-0.2 part, catalyst 0.05-0.1 part, firming agent 0.6-1.2 part, curing accelerator 0.2-
0.4 part, releasing agent 0.3-0.5 part, coloring agent 0.4-0.8 part, viscosifier 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, acrylic acid methyl ester. 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, Pulvis Talci 0.4-0.8 part, aluminium oxide 0.4-0.6 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 240-255 DEG C in temperature, and rotating speed is stirring 6-8min under 300-400r/min, prepares mixing
Thing A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 250-350W at microwave power, and temperature is 155-175 DEG C, and rotating speed is 250-
Stir 3-5h under 350r/min, prepare mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker 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 firming agent is phenol linear phenolic resin B.
Further, described curing accelerator is diazabicylo C1.
Further, described releasing agent is Brazil wax W.
Further, described coloring agent is white carbon black T.
Further, described viscosifier are aromatic petroleum resin.
The method have the advantages that
(1) the novel seal heat-curing resin material that the present invention prepares, has good performance, and its medium dielectric constant microwave medium reaches
More than 8.2112F/m, dielectric loss has reached less than 0.0254, weight-loss ratio has reached less than 12.34%, and hot strength reaches
More than 61.06, there is the combination property of excellence, it is possible to be well applied to technical field of electronic components, play good
Sealing effectiveness.
(2) the novel seal heat-curing resin material 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 it is not intended to protection scope of the present invention.
In an embodiment, described novel seal heat-curing resin material, 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 glycidyl ether 170-270 parts, styrene and Oleum Verniciae fordii based alkyd 55-75 part, o-cresol formaldehyde epoxy resin A45-56 part,
Dioctyl phthalate 25-30 part, phosphate ester 35-50 part, polysiloxanes 22-32 part, oil base potassium amino acid 20-26 part, partially
Sodium silicate 16-22 part, chlorinated paraffin 26-34 part, carbon fiber 14-25 part, poly maleimide 15-20 part, phthalic acid 14-
25 parts, silica 1 4-26 part, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3-5 part, change
Property polyacrylate compatilizer 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part, without water stone
Cream tranquilizer 0.6-1.2 part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid regulator 0.5-1 part, 701 powder hardening agent 0.4-
0.6 part, aluminium polychlorid flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8 part, adjacent benzene
Dioctyl phthalate two (2-ethyl hexyl) ester plasticiser 0.5-0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems
Diacid ester stabilizer 0.3-0.4 part, antioxidant DLPP0.3-0.4 part, styrene terminator 0.2-0.3 part, azo two isopropylformic acid.
(acrylic acid ethylene glycol) ester initiator 0.3-0.5 part, di-t-butyl hexane peroxide cross-linking agent 0.3-0.4 part, polyester fiber are soft
Soft dose of 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 novolac
Resin curing agent B0.6-1.2 part, diazabicylo C1 curing accelerator 0.2-0.4 part, Brazil wax W releasing agent 0.3-0.5
Part, white carbon black T coloring agent 0.4-0.8 part, aromatic petroleum resin viscosifier 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, acrylic acid methyl ester. 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, Pulvis Talci 0.4-0.8 part, aluminium oxide 0.4-0.6 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 240-255 DEG C in temperature, and rotating speed is stirring 6-8min under 300-400r/min, prepares mixing
Thing A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 250-350W at microwave power, and temperature is 155-175 DEG C, and rotating speed is 250-
Stir 3-5h under 350r/min, prepare mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker 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 novel seal heat-curing resin material, 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 glycidyl ether 220
Part, styrene and Oleum Verniciae fordii based alkyd 65 parts, o-cresol formaldehyde epoxy resin A50 part, dioctyl phthalate 25 parts, phosphoric acid
Ester 42 parts, polysiloxanes 27 parts, oil base potassium amino acid 23 parts, sodium metasilicate 19 parts, chlorinated paraffin 30 parts, 20 parts of carbon fiber, poly-
Maleimide 17 parts, phthalic acid 20 parts, silicon dioxide 20 parts, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent 4 parts, modified polyacrylate compatilizer 4 parts, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl benzene
Phenol) 1.2 parts, anhydrous gypsum tranquilizer 0.9 part, DCP bridging agent 0.9 part, esters of acrylic acid regulator 0.8 part, 701 powder hardening agents
0.5 part, aluminium polychlorid 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 sebacate stabilizers
0.3 part, antioxidant DLPP0.3 part, styrene terminator 0.2 part, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator
0.4 part, di-t-butyl hexane peroxide cross-linking 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 firming agent B0.9 part, diazabicylo C1 curing accelerator 0.3 part, bar
Western palm wax W releasing agent 0.4 part, white carbon black T coloring agent 0.6 part, aromatic petroleum resin viscosifier 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, acrylic acid methyl ester. 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, Pulvis Talci 0.6 part, aluminium oxide 0.5 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 250 DEG C in temperature, and rotating speed is stirring 7min under 350r/min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 300W at microwave power, and temperature is 165 DEG C, and rotating speed is to stir under 3000r/min
Mix 4h, prepare mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker 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 novel seal heat-curing resin material, in units of weight, 2,2 '-[(1-methyl ethylidene) is double, and (4,1-is sub-
Phenyl formaldehyde)] bisoxirane and methylene-bis-(Resorcinol)-four glycidyl ether 170 parts, styrene and Oleum Verniciae fordii base
Alkyd resin 55 parts, o-cresol formaldehyde epoxy resin A45 part, phosphate ester 35 parts, polysiloxanes 22 parts, oil base potassium amino acid 20 parts,
Sodium metasilicate 16 parts, chlorinated paraffin 26 parts, 14 parts of carbon fiber, poly maleimide 15 parts, phthalic acid 14 parts, silicon dioxide
14 parts, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane coupling agent 3 parts, modified polyacrylate compatilizer 3
Part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8 part, anhydrous gypsum tranquilizer 0.6 part, DCP bridging agent 0.6
Part, esters of acrylic acid regulator 0.5 part, 701 powder hardening agent 0.4 part, aluminium polychlorid flocculation agent 0.4 part, styrene-butadiene
Thermoplastic elastomer toughening agent 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, antioxidant DLPP0.3 part, styrene terminator 0.2 part,
Azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator 0.3 part, di-t-butyl hexane peroxide cross-linking agent 0.3 part, polyester are fine
Dimension softening agent 0.5 part, fire retardant 0.1 part, antismoke agent 0.1 part, Raney nickel 0.05 part, phenol linear phenolic resin firming agent
B0.6 part, diazabicylo C1 curing accelerator 0.2 part, Brazil wax W releasing agent 0.3 part, white carbon black T coloring agent 0.4 part, virtue
Fragrant race petroleum resin tackifiers 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, acrylic acid methyl ester. 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, Pulvis Talci 0.4 part, aluminium oxide 0.4 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 240 DEG C in temperature, and rotating speed is stirring 8min under 300r/min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 250W at microwave power, and temperature is 155 DEG C, and rotating speed is to stir under 250r/min
5h, prepares mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker 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 novel seal heat-curing resin material, 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 glycidyl ether 270
Part, styrene and Oleum Verniciae fordii based alkyd 75 parts, o-cresol formaldehyde epoxy resin A56 part, dioctyl phthalate 28 parts, phosphoric acid
Ester 50 parts, polysiloxanes 32 parts, oil base potassium amino acid 26 parts, sodium metasilicate 22 parts, chlorinated paraffin 34 parts, 25 parts of carbon fiber, poly-
Maleimide 20 parts, phthalic acid 25 parts, silicon dioxide 26 parts, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent 5 parts, modified polyacrylate compatilizer 5 parts, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl benzene
Phenol) 1.4 parts, anhydrous gypsum tranquilizer 1.2 parts, DCP bridging agent 1.2 parts, esters of acrylic acid regulator 1 part, 701 powder hardening agents
0.6 part, aluminium polychlorid 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 isopropylformic acid. (acrylic acid ethylene glycol) ester initiator
0.5 part, di-t-butyl hexane peroxide cross-linking 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 firming agent B1.2 part, diazabicylo C1 curing accelerator 0.4 part, bar
Western palm wax W releasing agent 0.5 part, white carbon black T coloring agent 0.8 part, aromatic petroleum resin viscosifier 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, acrylic acid methyl ester. 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, Pulvis Talci 0.8 part, aluminium oxide 0.6 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 255 DEG C in temperature, and rotating speed is stirring 6min under 400r/min, prepares mixture A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 350W at microwave power, and temperature is 175 DEG C, and rotating speed is to stir under 350r/min
3h, prepares mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker when temperature drops to 55 DEG C, and 124 DEG C of annealing 1.5h continue
Continuous solidification, destressing, naturally cool to room temperature.
Embodiment 1-3 is prepared novel seal heat-curing resin material and carries out performance test, test event and method
As follows:
Dielectric properties are tested: use accurate LCR digital electric bridge to carry out dielectric constant and the dielectric loss of prepared composite
Test；
Composite thermal weight loss is tested: adopt TA SDTQ600 type thermogravimetric synchronization discrepancy thermal analyzer and composite is carried out TG analysis；
Mechanics Performance Testing: use the SANS5105 type microcomputer controlled electronic universal tester tensile force to prepared composite
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 (%) | Hot strength (MPa) |
| 1 | 8.8126 | 0.0236 | 10.79 | 66.26 |
| 2 | 8.2112 | 0.0254 | 12.34 | 61.06 |
| 3 | 9.1783 | 0.0177 | 9.259 | 71.65 |
From upper table result it can be seen that the novel seal heat-curing resin material for preparing of the present invention, have good
Performance, its medium dielectric constant microwave medium has reached more than 8.2112F/m, and dielectric loss has reached less than 0.0254, and weight-loss ratio reaches
Less than 12.34%, hot strength has reached more than 61.06, has the combination property of excellence, it is possible to be well 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, it is also possible to make some simple deduction or replace,
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 novel seal heat-curing resin material, it is characterised in that in units of weight, be 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 170-270 part, styrene and Oleum Verniciae fordii based alkyd 55-75 part, o-cresol formaldehyde epoxy resin A45-56 part, adjacent benzene
Dioctyl phthalate dioctyl ester 25-28 part, phosphate ester 35-50 part, polysiloxanes 22-32 part, oil base potassium amino acid 20-26 part, metasilicic acid
Sodium 16-22 part, chlorinated 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, modification
Polyacrylate compatilizer 3-5 part, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol) 0.8-1.4 part, anhydrous gypsum
Tranquilizer 0.6-1.2 part, DCP bridging agent 0.6-1.2 part, esters of acrylic acid regulator 0.5-1 part, 701 powder hardening agent 0.4-0.6
Part, aluminium polychlorid flocculation agent 0.4-0.6 part, styrene butadiene thermoplasticelastomer toughener 0.5-0.8 part, adjacent benzene two
Formic acid two (2-ethyl hexyl) ester plasticiser 0.5-0.8 part, double-1-decane epoxide-2,2,6,6-tetramethyl piperidine-4-alcohol last of the ten Heavenly stems two
Acid esters stabilizer 0.3-0.4 part, antioxidant DLPP0.3-0.4 part, styrene terminator 0.2-0.3 part, azo two isopropylformic acid.
(acrylic acid ethylene glycol) ester initiator 0.3-0.5 part, di-t-butyl hexane peroxide cross-linking agent 0.3-0.4 part, polyester fiber are soft
Soft dose of 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, firming agent 0.6-1.2
Part, curing accelerator 0.2-0.4 part, releasing agent 0.3-0.5 part, coloring agent 0.4-0.8 part, viscosifier 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, acrylic acid methyl ester. 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, Pulvis Talci 0.4-0.8 part, aluminium oxide 0.4-0.6 part；
The preparation method of described novel seal heat-curing resin material, 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 glycidyl ethers, styrene and Oleum Verniciae fordii based alkyd, o-cresol formaldehyde epoxy resin A, dioctyl phthalate,
Phosphate ester, polysiloxanes mix, and are 240-255 DEG C in temperature, and rotating speed is stirring 6-8min under 300-400r/min, prepares mixing
Thing A；
S2: under nitrogen protection, adds oil base potassium amino acid, sodium metasilicate, chlorination stone in the mixture A that step 1 prepares
Wax, carbon fiber, poly maleimide, phthalic acid, silicon dioxide, N-2-(amino-ethyl)-3-amino propyl methyl diformazan
TMOS coupling agent, modified polyacrylate compatilizer, 2,2 '-methylene-bis--(4-ethyl-6-tert-butyl phenol), anhydrous
Gypsum Fibrosum tranquilizer, DCP bridging agent, esters of acrylic acid regulator, azo two isopropylformic acid. (acrylic acid ethylene glycol) ester initiator, two uncles
Butyl peroxy hexane cross-linking agent, catalyst, be 250-350W at microwave power, and temperature is 155-175 DEG C, and rotating speed is 250-
Stir 3-5h under 350r/min, prepare mixture B；
S3: add 701 powder hardening agents, aluminium polychlorid 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, viscosifier, super
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, firming 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
Curable 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 baker 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.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described catalyst is nickel
Catalyst.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described firming agent is benzene
Phenol linear phenolic resin B.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described curing accelerator
For diazabicylo C1.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described releasing agent is bar
Western palm wax W.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described coloring agent is charcoal
Black T.
Novel seal heat-curing resin material the most according to claim 1, it is characterised in that described viscosifier are virtue
Fragrant race Petropols.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117403804A (en) * | 2023-12-14 | 2024-01-16 | 国建绿色智慧工程设计研究院(天津)有限公司 | Novel assembled external wall panel and assembling method thereof |
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| 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 |
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| CN105778409A (en) * | 2014-12-18 | 2016-07-20 | 北京首科化微电子有限公司 | Epoxy resin composition for semiconductor packaging, and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117403804A (en) * | 2023-12-14 | 2024-01-16 | 国建绿色智慧工程设计研究院(天津)有限公司 | Novel assembled external wall panel and assembling method thereof |
| CN117403804B (en) * | 2023-12-14 | 2024-03-22 | 国建绿色智慧工程设计研究院(天津)有限公司 | Assembled external wall panel and assembling method thereof |
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Application publication date: 20161207 |