CN110055020A - A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient - Google Patents

A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient Download PDF

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Publication number
CN110055020A
CN110055020A CN201910405098.1A CN201910405098A CN110055020A CN 110055020 A CN110055020 A CN 110055020A CN 201910405098 A CN201910405098 A CN 201910405098A CN 110055020 A CN110055020 A CN 110055020A
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parts
pouring sealant
agent
coupling agent
micron order
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CN201910405098.1A
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魏月秀
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to epoxy pouring sealant preparation technical fields, and disclose the epoxy pouring sealant and preparation method of a kind of high thermal conductivity coefficient, by the micron order boron nitride ceramic particles for adding the higher two kinds of different-grain diameters of thermal coefficient in the raw material components of epoxy resin, addition has the micron order MgO particle of gelatification simultaneously, each component is under the collective effect of silane coupling agent, titanate coupling agent, fumed silica anti-settling agent and isophorone diisocyanate curing agent, curing reaction is crosslinked, epoxy pouring sealant is prepared.The present invention solves epoxy pouring sealant in the prior art, while with superior dielectric performance, cannot achieve the technical issues of effectively radiating to the electronic component of encapsulating.

Description

A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient
Technical field
The present invention relates to epoxy pouring sealant preparation technical field, the epoxy pouring sealant and system of specially a kind of high thermal conductivity coefficient Preparation Method.
Background technique
In the manufacturing process of integrated circuit, the step that is very important is packaged to integrated circuit, encapsulation is exactly to make Each components of composition electronic equipment are assembled as requested with grouting material, electronic component is sealed, is made Electronic device is isolated with external environment.However the heat dissipation problem of electronic component, to electron pouring sealant, more stringent requirements are proposed, It is required that electron pouring sealant will not only have preferable electrical insulation capability, but also want thermal conductivity with higher.
Epoxy pouring sealant is using epoxy resin as main component, and one that some functional materials are formulated is added in cooperation Based epoxy resin liquid encapsulating material.Epoxy pouring sealant has excellent dielectric properties, and hardness is higher, can be obtained by modification Certain toughness has a good adhesive property to hard substrates such as metals, corrosion resistance and good, cure shrinkage and linear swollen Swollen coefficient is smaller.However, epoxy resin is the non-conductor of heat, thermal coefficient is generally 0.20W/mK or so, generally, thermally conductive The thermal coefficient of insulating materials is greater than 1W/mK or so, just can be applied to the heat dissipation of electronic device, so, epoxy pouring sealant is remote Thermally conductive requirement is far not achieved.
The present invention provides the epoxy pouring sealant and preparation method of a kind of high thermal conductivity coefficient, it is intended to solve ring in the prior art Oxygen casting glue cannot achieve the technology effectively to radiate to the electronic component of encapsulating and ask while with superior dielectric performance Topic.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of epoxy pouring sealant of high thermal conductivity coefficient and preparation method, It solves epoxy pouring sealant in the prior art, while with superior dielectric performance, cannot achieve the electronics member to encapsulating The technical issues of device effectively radiates.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of epoxy pouring sealant of high thermal conductivity coefficient, the raw material including following parts by weight proportion: 80 parts of epoxy resin, 19 Part silane coupling agent, 16 parts of titanate coupling agents, 8 portions of fumed silica anti-settling agents, 36 parts of isophorone diisocyanate are solid Agent, 25 parts of micron order boron nitride ceramic particles, 5 parts of micron order MgO gelling agents；
By the micron order nitridation for adding the higher two kinds of different-grain diameters of thermal coefficient in the raw material components of epoxy resin Boron ceramic particle, while the MgO with gelatification is added, each component is in silane coupling agent, titanate coupling agent, gas phase dioxy Under the collective effect of SiClx anti-settling agent and isophorone diisocyanate curing agent, curing reaction is crosslinked, epoxy is prepared Casting glue.
Preferably, the micron order boron nitride ceramic particles include: 15 parts of average grain diameter≤25um boron nitride ceramics Grain, 10 parts of average grain diameter≤10um boron nitride ceramic particles.
Preferably, the epoxy resin is epoxy resin E-44.
A kind of preparation method of the epoxy pouring sealant of high thermal conductivity coefficient, comprising the following steps:
(1) 19 parts of vinyltriethoxysilane coupling agents are weighed, addition is made of 5 parts of distilled water and 15 parts of dehydrated alcohols Solvent in, hydrolyze 30min at room temperature, preparation obtains coupling agent A；
(2) 8 parts of tetraisopropyl titanates are heated in 8 parts of atoleines, after completely dissolution, preparation obtains coupling agent B；
(3) 25 parts of micron order boron nitride ceramic particles, 5 parts of micron order MgO gelling agents are weighed, preparation obtains filler component；
(4) above-mentioned filler component is added in the reactor equipped with agitating device and heating device, 8 parts of gas phases two is added Silica anti-settling agent stirs at 80~100 DEG C, and revolving speed is 300~500rpm, stirs after coupling agent A and coupling agent B is added It is even, heat filling is prepared；
(5) 80 parts of epoxy resin E-44s are added in the reactor equipped with agitating device and heating device, are in temperature 120~150 DEG C, revolving speed be 300~500rpm stirring under, be slowly added to above-mentioned heat filling, switch to 600~800rpm Lower stirring 1h；
Under the stirring that temperature is 120~150 DEG C, revolving speed is 300~500rpm, it is different that 36 parts of isophorones two are added Cyanate curing agent switchs to stir evenly under 600~800rpm, and casting glue is transferred to Teflon mould after exhaust bubble In, epoxy pouring sealant is prepared in levelling, the curing process at 120~150 DEG C.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
By the micron order nitridation for adding the higher two kinds of different-grain diameters of thermal coefficient in the raw material components of epoxy resin Boron ceramic particle (BN), while the micron order MgO particle with gelatification is added, each component is in silane coupling agent, titanate esters Under the collective effect of coupling agent, fumed silica anti-settling agent and isophorone diisocyanate curing agent, solidification is crosslinked Reaction, prepares epoxy pouring sealant；
And the thermal coefficient for the epoxy pouring sealant prepared is 1.58~1.71W/mK, volume resistivity is 3.2 × 1012~ 4.9×1012Ω cm, to achieve while with excellent electrical insulation capability, realization has the electronic component of encapsulating Imitate the technical effect of heat dissipation.
Specific embodiment
Embodiment one:
(1) 19g vinyltriethoxysilane coupling agent is weighed, what addition was made of 5g distilled water and 15g dehydrated alcohol In solvent, 30min is hydrolyzed at room temperature, and preparation obtains coupling agent A；
(2) 8g tetraisopropyl titanate is heated in 8g atoleine, after completely dissolution, preparation obtains coupling agent B；
(3) 15g average grain diameter≤25um boron nitride ceramic particles (BN), 10g average grain diameter≤10um nitridation are weighed Boron ceramic particle (BN), 5g average grain diameter≤25um MgO, preparation obtain filler component；
(4) above-mentioned filler component is added in the reactor equipped with agitating device and heating device, 8g gas phase two is added Silica anti-settling agent stirs at 80 DEG C, revolving speed 300rpm, after being slowly added to coupling agent A, switchs to stir under 600rpm 10min；
Switch to stir under 300rpm, after being slowly added to coupling agent B, switchs to stir 10min under 600rpm；It discharges after cooling, Filler is placed in 120 DEG C of drying box, heat filling is prepared in dry 6h；
(5) 80g epoxy resin E-44 is added in the reactor equipped with agitating device and heating device, is in temperature 120 DEG C, revolving speed be 300rpm stirring under, be slowly added to above-mentioned heat filling, switch to stir 1h under 600rpm；
Under the stirring that temperature is 120 DEG C, revolving speed is 300rpm, the solidification of 36g isophorone diisocyanate is added Agent switchs to stir 1h under 600rpm, and bubble processing is exhausted to casting glue in a manner of vacuumizing deflation later, will after exhaust bubble Casting glue is transferred in Teflon mould, levelling, until casting glue surfacing, the curing process 2h at 120 DEG C, is made later It is standby to obtain epoxy pouring sealant；
(6) thermal coefficient of the above-mentioned epoxy pouring sealant prepared is 1.71W/mK, and volume resistivity is 4.5 × 1012 Ω·cm。
Embodiment two:
(1) 19g vinyltriethoxysilane coupling agent is weighed, what addition was made of 5g distilled water and 15g dehydrated alcohol In solvent, 30min is hydrolyzed at room temperature, and preparation obtains coupling agent A；
(2) 8g tetraisopropyl titanate is heated in 8g atoleine, after completely dissolution, preparation obtains coupling agent B；
(3) 25g average grain diameter≤25um boron nitride ceramic particles (BN), 5g average grain diameter≤25um MgO are weighed, are matched Filler component is made；
(4) above-mentioned filler component is added in the reactor equipped with agitating device and heating device, 8g gas phase two is added Silica anti-settling agent stirs at 100 DEG C, revolving speed 500rpm, after being slowly added to coupling agent A, switchs to stir under 800rpm 10min；
Switch to stir under 500rpm, after being slowly added to coupling agent B, switchs to stir 10min under 800rpm；It discharges after cooling, Filler is placed in 120 DEG C of drying box, heat filling is prepared in dry 6h；
(5) 80g epoxy resin E-44 is added in the reactor equipped with agitating device and heating device, is in temperature 150 DEG C, revolving speed be 500rpm stirring under, be slowly added to above-mentioned heat filling, switch to stir 1h under 800rpm；
Under the stirring that temperature is 150 DEG C, revolving speed is 500rpm, the solidification of 36g isophorone diisocyanate is added Agent switchs to stir 1h under 800rpm, and bubble processing is exhausted to casting glue in a manner of vacuumizing deflation later, will after exhaust bubble Casting glue is transferred in Teflon mould, levelling, until casting glue surfacing, the curing process 2h at 150 DEG C, is made later It is standby to obtain epoxy pouring sealant；
(6) thermal coefficient of the above-mentioned epoxy pouring sealant prepared is 1.66W/mK, and volume resistivity is 4.9 × 1012 Ω·cm。
Embodiment three:
(1) 19g vinyltriethoxysilane coupling agent is weighed, what addition was made of 5g distilled water and 15g dehydrated alcohol In solvent, 30min is hydrolyzed at room temperature, and preparation obtains coupling agent A；
(2) 8g tetraisopropyl titanate is heated in 8g atoleine, after completely dissolution, preparation obtains coupling agent B；
(3) 25g average grain diameter≤10um boron nitride ceramic particles (BN), 5g average grain diameter≤25um MgO are weighed, are matched Filler component is made；
(4) above-mentioned filler component is added in the reactor equipped with agitating device and heating device, 8g gas phase two is added Silica anti-settling agent stirs at 90 DEG C, revolving speed 400rpm, after being slowly added to coupling agent A, switchs to stir under 700rpm 10min；
Switch to stir under 400rpm, after being slowly added to coupling agent B, switchs to stir 10min under 700rpm；It discharges after cooling, Filler is placed in 120 DEG C of drying box, heat filling is prepared in dry 6h；
(5) 80g epoxy resin E-44 is added in the reactor equipped with agitating device and heating device, is in temperature 130 DEG C, revolving speed be 400rpm stirring under, be slowly added to above-mentioned heat filling, switch to stir 1h under 700rpm；
Under the stirring that temperature is 120~150 DEG C, revolving speed is 400rpm, 36g isophorone diisocyanate is added Curing agent switchs to stir 1h under 700rpm, and bubble processing, exhaust bubble is exhausted to casting glue in a manner of vacuumizing deflation later Casting glue is transferred in Teflon mould afterwards, levelling, until casting glue surfacing, the curing process at 130 DEG C later Epoxy pouring sealant is prepared in 2h；
(6) thermal coefficient of the above-mentioned epoxy pouring sealant prepared is 1.58W/mK, and volume resistivity is 3.2 × 1012 Ω·cm。

Claims (4)

1. a kind of epoxy pouring sealant of high thermal conductivity coefficient, which is characterized in that the raw material including following parts by weight proportion: 80 parts of rings Oxygen resin, 19 parts of silane coupling agents, 16 parts of titanate coupling agents, 8 portions of fumed silica anti-settling agents, 36 parts of isophorones two are different Cyanate curing agent, 25 parts of micron order boron nitride ceramic particles, 5 parts of micron order MgO gelling agents；
By adding the higher micron order boron nitride ceramic particles of thermal coefficient in the raw material components of epoxy resin, add simultaneously Micron order MgO particle with gelatification, each component are anti-settling in silane coupling agent, titanate coupling agent, fumed silica Under the collective effect of agent and isophorone diisocyanate curing agent, curing reaction is crosslinked, epoxy pouring sealant is prepared.
2. epoxy pouring sealant according to claim 1, which is characterized in that the micron order boron nitride ceramic particles include: 15 parts of average grain diameter≤25um boron nitride ceramic particles, 10 parts of average grain diameter≤10um boron nitride ceramic particles.
3. epoxy pouring sealant according to claim 1, which is characterized in that the epoxy resin is epoxy resin E-44.
4. a kind of preparation method of the epoxy pouring sealant of high thermal conductivity coefficient, which comprises the following steps:
(1) 19 parts of vinyltriethoxysilane coupling agents are weighed, addition is made of molten 5 parts of distilled water and 15 parts of dehydrated alcohols In agent, 30min is hydrolyzed at room temperature, and preparation obtains coupling agent A；
(2) 8 parts of tetraisopropyl titanates are heated in 8 parts of atoleines, after completely dissolution, preparation obtains coupling agent B；
(3) 25 parts of micron order boron nitride ceramic particles, 5 parts of micron order MgO gelling agents are weighed, preparation obtains filler component；
(4) above-mentioned filler component is added in the reactor equipped with agitating device and heating device, 8 parts of gas phase titanium dioxides is added Silicon anti-settling agent stirs at 80~100 DEG C, and revolving speed is 300~500rpm, stirs evenly after coupling agent A and coupling agent B is added, Heat filling is prepared；
(5) 80 parts of epoxy resin E-44s are added in the reactor equipped with agitating device and heating device, temperature be 120~ 150 DEG C, revolving speed be 300~500rpm stirring under, be slowly added to above-mentioned heat filling, switch to stir under 600~800rpm Mix 1h；
Under the stirring that temperature is 120~150 DEG C, revolving speed is 300~500rpm, 36 parts of isophorone diisocyanates are added Ester curing agent switchs to stir evenly under 600~800rpm, and casting glue is transferred in Teflon mould after exhaust bubble, is flowed Flat, epoxy pouring sealant is prepared in the curing process at 120~150 DEG C.
CN201910405098.1A 2019-05-16 2019-05-16 A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient Withdrawn CN110055020A (en)

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Application Number Priority Date Filing Date Title
CN201910405098.1A CN110055020A (en) 2019-05-16 2019-05-16 A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient

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CN110055020A true CN110055020A (en) 2019-07-26

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111134A (en) * 2020-08-26 2020-12-22 安徽国风塑业股份有限公司 High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
R.J.诺勃耳: "《胶乳工业》", 30 April 1958 *
徐思亭: "《塑料材料与助剂》", 31 July 2007 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111134A (en) * 2020-08-26 2020-12-22 安徽国风塑业股份有限公司 High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film

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