CN108424742A - A kind of preparation method of nonisulated heat conduction adhesive - Google Patents
A kind of preparation method of nonisulated heat conduction adhesive Download PDFInfo
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- CN108424742A CN108424742A CN201810278051.9A CN201810278051A CN108424742A CN 108424742 A CN108424742 A CN 108424742A CN 201810278051 A CN201810278051 A CN 201810278051A CN 108424742 A CN108424742 A CN 108424742A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
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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
- C09J11/06—Non-macromolecular additives organic
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0856—Iron
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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
- C08K2201/001—Conductive additives
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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
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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Abstract
The invention discloses a kind of preparation methods of nonisulated heat conduction adhesive, belong to chemical material technical field.After nanometer compounding metal-powder is first scattered in absolute ethyl alcohol by the present invention, dopamine solution is added, metal-powder dispersion liquid is made, butyl titanate dispersant liquid drop is added in metal-powder dispersion liquid again, and ammonium hydroxide is added, it is stirred for reacting, metal-powder suspension is made；After ethyl orthosilicate and absolute ethyl alcohol are mixed, with salt acid for adjusting pH, boric acid is added, constant temperature is stirred to react, and hydrolyzate is made, then by hydrolyzate, acrylamide, after crosslinking agent and initiator hybrid reaction, impregnated with sodium hydroxide solution, then after copper-bath impregnates, it is dry, and mixed in epobond epoxyn, then through vacuum impregnation to get nonisulated heat conduction adhesive.The nonisulated heat conduction adhesive of gained of the invention has excellent heat conductivility.
Description
Technical field
The invention discloses a kind of preparation methods of nonisulated heat conduction adhesive, belong to chemical material technical field.
Background technology
In electric field, due to the development of integrated technology and micro-packaging technology, electronic component and electronic equipment to
Miniaturization and micromation direction develop, the consequence of this trend be more heats are produced in limited volume, if
Heat cannot timely lose, and heat accumulation will excessively cause component operating temperature to increase, and influence its normal work, sternly
It can also make electronic component failure when weight.Most of metal material radiating rate than comparatively fast, disclosure satisfy that a certain extent
Heat conduction demand, but metal material have than it is great, conductive, intolerant to burn into different shape thermally-conductive interface bad adaptability the shortcomings that,
Limit its application in specific area.Therefore, in the research and development of vast scientific research personnel steering thermal conductive adhesive.By
It is low in the thermal conductivity of adhesive itself, heat conductivility is bad, so the high thermal conductivity for how improving adhesive cause it is vast
More and more concerns of researcher.Currently, the method for improving adhesive high-termal conductivity mainly adds people in adhesive
Suitable high heat conduction filler, such as Al, Cu, Ag metal powder class filler；Al2O3, the metal oxide-types filler such as MgO；SiC、AIN、
Si3N4Nonmetallic heat conductives filler is waited to realize.Thermal conductive adhesive can be divided into insulating heat-conductive adhesive and non-according to its electrical insulating property
Insulating heat-conductive adhesive two major classes, main application is in transistor ceramic substrate and the bonding of copper seat, the protection of die, shell
Sealing, rectifier, thermal resistor heat conductive insulating, multiple-plate heat conductive insulating and chemical industry heat exchanger in micro- packaging
The fields such as bonding and heat conduction embedding.
Nonisulated thermal conductive adhesive customary filler has silver, copper, tin, aluminium powder and graphite, carbon fiber etc..Currently, the type glue
Stick is mainly used for the bonding of the nonisulated occasion of heat conduction.For current heat conduction adhesive there is also heat conductivility bad ask
Topic, need to study it.
Invention content
The present invention solves the technical problem of：It is bad for conventional thermal conductive adhesive heat conductivility and electric conductivity
Problem provides a kind of preparation method of nonisulated heat conduction adhesive.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It is 1 that nanometer, which is compounded metal-powder and absolute ethyl alcohol in mass ratio,：10~1：After 50 mixing, ultrasonic disperse adds
The dopamine solution that 0.1~0.3 times of absolute ethyl alcohol quality, after continuing ultrasonic disperse, heating stirring mixes 10~15h, obtains metal
Powder dispersion；
（2）It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：8~1：10 ultrasonic mixings obtain butyl titanate dispersion liquid,
It counts in parts by weight again, takes 60~80 parts of metal-powder dispersion liquids, 10~20 parts of butyl titanate dispersion liquids, 6~8 parts of ammonia successively
Butyl titanate dispersion liquid is first added dropwise to 3~5mL/min rates in metal-powder dispersion liquid by water, waits for butyl titanate point
After dispersion liquid is added dropwise, then with 2~4mL/min rates ammonium hydroxide is added dropwise in metal-powder dispersion liquid, waits for that ammonium hydroxide is added dropwise,
In be stirred to react 16 under room temperature~for 24 hours after, obtain metal-powder suspension；
（3）It is 1 in mass ratio by ethyl orthosilicate and absolute ethyl alcohol：20~1：30 mixing after, with dilute hydrochloric acid adjust pH to 3.2~
3.4, the boric acid solution of 0.2~0.4 times of absolute ethyl alcohol quality is added, constant temperature is stirred to react, and obtains hydrolyzate；
（4）It counts in parts by weight, takes 80~120 parts of hydrolyzates, 40~50 parts of metal-powder suspension, 10~30 parts of propylene successively
Amide, 4~6 parts of N, N '-methylene-bisacrylamides, 0.6~0.8 part of ammonium persulfate, after mixing, heating stirring reaction obtains wet
Gel, then by after the drying of gained wet gel, be impregnated in sodium hydroxide solution, after being ultrasonically treated 40~60min, obtain single-steeping
Wet gel；
（5）Single-steeping wet gel is washed with water to after neutrality and copper-bath mixes, after 60~90min of ultrasonic immersing,
Successively through being filtered, washed and dried drying, double-steeping xerogel is obtained；
（6）It is 1 in mass ratio by epobond epoxyn and double-steeping xerogel：1~3：1 mixing, then after vacuum impregnation,
Discharging is to get nonisulated heat conduction adhesive.
Step（1）It is 50 in mass ratio that the nanometer compounding metal-powder, which is by nanometer iron powder and nanometer aluminium powder,：1~100：
1 compounds.
Step（6）The epobond epoxyn is compounded by the raw material of following parts by weight：80~120 parts of epoxies
Resin E-42,20~30 parts of benzyl alcohols, 10~15 parts of ethylenediamines, 3~5 parts of dibutyl phthalates.
The beneficial effects of the invention are as follows：
（1）The present invention uses dopamine and metal-powder to mix first, in water solution system, the catechol group of dopamine
It is easily oxidized, and in nano metal powder surface formation poly-dopamine composite layer, the compound layer formation process, can compete
Oxygen in absorption system avoids oxygen that active nano metal powder is made to aoxidize, furthermore, the formation of poly-dopamine can be carried effectively
The absorption property of high nano metal powder, to the titanium dioxide that adsorption of hydrolyzation generates, for nano metal powder, surface is lived
Property it is high, easily reunite, if being directly appended in heat conduction adhesive, can not effectively disperse, and the present invention by
Its adsorption layer of titanium dioxide makes the dispersibility of nano metal powder while improving nano metal powder inoxidizability
It effectively improves, in subsequent preparation process, is gathered by the way that monomer is added in the metal-powder suspension after coated by titanium dioxide
It closes in reaction process, to which the metal powder particles of suspension is fixed in crosslink polymer network gelinite, further increases
Its dispersibility；Furthermore the formation of metal-powder surface poly-dopamine layer can effectively improve inorganic nano metal powder and have
The compatibility of the macromolecule epoxy resin of machine avoids influencing there are excessive hole in metal-powder and resin-bonded interface
The heat conduction of product and electric conductivity；
（2）The present invention passes through step（4）Impregnated using sodium hydroxide solution, in dipping process, aluminium powder in system gradually and
Sodium hydroxide solution reacts, and generates gas, to get through the hole in gel network, is conducive to each ingredient in gel network
Scattering and permeating in hole, with step（5）The dipping of copper-bath can make the nanometer iron powder in system and copper-bath hair
Raw displacement reaction, to make the copper of atomic radius bigger replace part iron, and is filled in hole, hole is made gradually to be densified,
And copper heat conduction and electric conductivity be superior to iron, the generation of copper can be such that the heat conductivility of system and electric conductivity is effectively carried
It rises.
Specific implementation mode
It is 1 in mass ratio：10~1：50 pour into nanometer compounding metal-powder and absolute ethyl alcohol mixing in No. 1 beaker, and
Beaker is moved into ultrasonic disperse instrument, under the conditions of supersonic frequency is 45~50kHz, after 2~4h of ultrasonic disperse, then to No. 1 beaker
The dopamine solution that the middle mass concentration that 0.1~0.3 times of absolute ethyl alcohol quality is added is 2g/L, continuation ultrasonic disperse 45~
After 60min, No. 1 beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, is 35~45 DEG C in temperature, rotating speed is 400~600r/
Under the conditions of min, heating stirring mixes 10~15h, obtains metal-powder dispersion liquid；In mass ratio by butyl titanate and absolute ethyl alcohol
It is 1：8~1：No. 2 beakers are poured into 10 mixing, and No. 2 beakers are moved into sonic oscillation instrument, in supersonic frequency be 45~50kHz items
Under part, 45~60min of sonic oscillation obtains butyl titanate dispersion liquid, then counts in parts by weight, takes 60~80 parts of metal powders successively
Dispersion liquid, 10~20 parts of butyl titanate dispersion liquids, the ammonium hydroxide that 6~8 parts of mass fractions are 10~15%, first by metal-powder
Three-necked flask is added in dispersion liquid, is under 200~400r/min stirrings, by dropping funel with 3~5mL/min then at rotating speed
Rate is added dropwise in three-necked flask, drips ammonium hydroxide after butyl titanate dispersion liquid is added dropwise, then with 2~4mL/min rates
Add in three-necked flask, after ammonium hydroxide is added dropwise, in be stirred to react 16 under room temperature~for 24 hours, obtain metal-powder suspension；
It is 1 in mass ratio by ethyl orthosilicate and absolute ethyl alcohol：20~1：30 mixing pour into No. 3 beakers, with mass fraction be 10~
12% dilute hydrochloric acid is adjusted in No. 3 beakers after material pH to 3.2~3.4, then be added into No. 3 beakers absolute ethyl alcohol quality 0.2~
The boric acid solution that 0.4 times of mass fraction is 8~10% is then 30~35 DEG C in temperature, and rotating speed is 300~500r/min items
Under part, constant temperature is stirred to react 2~4h, obtains hydrolyzate；It counts in parts by weight, takes 80~120 parts of hydrolyzates, 40~50 parts of gold successively
Category powder suspension, 10~30 parts of acrylamides, 4~6 parts of N, N '-methylene-bisacrylamides, 0.6~0.8 part of ammonium persulfate,
Mixing pour into reaction kettle, in temperature be 80~85 DEG C, rotating speed be 600~800r/min under the conditions of, heating stirring reaction 4~
6h, obtains wet gel, then by gained wet gel under the conditions of temperature is 105~110 DEG C, dry to constant weight, obtains xerogel, and by institute
Xerogel and mass fraction be 4~8% sodium hydroxide solution be placed in No. 1 sink, in supersonic frequency be 55~60kHz items
Under part, after being ultrasonically treated 40~60min, single-steeping wet gel is obtained, gained single-steeping wet gel is washed with deionized
Be in neutrality to cleaning solution, then by after washing single-steeping wet gel and mass fraction be 8~15% copper-bath pour into 2
In number sink, and under the conditions of being 50~60kHz with frequency, after 60~90min of ultrasonic immersing, filtering obtains filter cake, anhydrous second is used in combination
Alcohol washs filter cake 4~6 times, then the filter cake after washing is transferred in baking oven, under the conditions of temperature is 80~90 DEG C, dry 3~5h,
Obtain double-steeping xerogel；It is 1 in mass ratio by epobond epoxyn and double-steeping xerogel：1~3：1 mixing is poured into mixed
In material machine, after rotating speed is 600~800r/min stirrings, 3~5h, under the conditions of vacuum degree is 60~80Pa, vacuum impregnation 3~
5h discharges to get nonisulated heat conduction adhesive.The nanometer compounding metal-powder is by nanometer iron powder and nanometer aluminium powder by quality
Than being 50：1~100：1 compounds.The epobond epoxyn is compounded by the raw material of following parts by weight：80~
120 parts of epoxy resin E-42,20~30 parts of benzyl alcohols, 10~15 parts of ethylenediamines, 3~5 parts of dibutyl phthalates.
It is 1 in mass ratio：Nanometer is compounded metal-powder and absolute ethyl alcohol by 50 to be mixed and pours into No. 1 beaker, and by beaker
Ultrasonic disperse instrument is moved into, under the conditions of supersonic frequency is 50kHz, after ultrasonic disperse 4h, then absolute ethyl alcohol is added into No. 1 beaker
The mass concentration that 0.3 times of quality is the dopamine solution of 2g/L, after continuing ultrasonic disperse 60min, No. 1 beaker is moved into digital display and is surveyed
Fast constant temperature blender with magnetic force is 45 DEG C in temperature, and under the conditions of rotating speed is 600r/min, heating stirring mixes 15h, obtains metal-powder
Dispersion liquid；It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：No. 2 beakers are poured into 10 mixing, and No. 2 beakers are moved into and are surpassed
Sound oscillation instrument, under the conditions of supersonic frequency is 50kHz, sonic oscillation 60min obtains butyl titanate dispersion liquid, then by weight
Several meters take 80 parts of metal-powder dispersion liquids, 20 parts of butyl titanate dispersion liquids, the ammonium hydroxide that 8 parts of mass fractions are 15%, elder generation successively
Three-necked flask is added in metal-powder dispersion liquid, is under 400r/min stirrings, by dropping funel with 5mL/ then at rotating speed
Min rates are added dropwise in three-necked flask, drip ammonium hydroxide after butyl titanate dispersion liquid is added dropwise, then with 4mL/min rates
It adds in three-necked flask, after ammonium hydroxide is added dropwise, in being stirred to react under room temperature for 24 hours, obtains metal-powder suspension；It will just
Silester and absolute ethyl alcohol are 1 in mass ratio：30 mixing are poured into No. 3 beakers, and the dilute hydrochloric acid for being 12% with mass fraction is adjusted
In No. 3 beakers after material pH to 3.4, then the boron that the mass fraction of 0.4 times of absolute ethyl alcohol quality is 10% is added into No. 3 beakers
Acid solution is then 35 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, obtains hydrolyzate；By weight
Number meter, takes 120 parts of hydrolyzates, 50 parts of metal-powder suspension, 30 parts of acrylamides, 6 parts of N, N '-methylene bisacrylamide acyls successively
Amine, 0.8 part of ammonium persulfate, mixing pour into reaction kettle, in temperature be 85 DEG C, rotating speed be 800r/min under the conditions of, heating stirring
6h is reacted, obtains wet gel, then by gained wet gel under the conditions of temperature is 110 DEG C, it is dry to constant weight, obtain xerogel, and by institute
It obtains the sodium hydroxide solution that xerogel and mass fraction are 8% to be placed in No. 1 sink, under the conditions of supersonic frequency is 60kHz, surpass
After sonication 60min, single-steeping wet gel is obtained, in gained single-steeping wet gel is washed with deionized being in cleaning solution
Property, then by after washing single-steeping wet gel and mass fraction be 15% copper-bath pour into No. 2 sinks, and with frequency
Under the conditions of rate is 60kHz, after ultrasonic immersing 90min, filtering obtains filter cake, absolute ethyl alcohol washing filter cake is used in combination 6 times, then will washing
Filter cake afterwards is transferred in baking oven, and under the conditions of temperature is 90 DEG C, dry 5h obtains double-steeping xerogel；Epoxy resin is bonded
Agent is 3 in mass ratio with double-steeping xerogel：1 mixing is poured into batch mixer, after rotating speed is 800r/min stirrings 5h, Yu Zhen
Under the conditions of reciprocal of duty cycle is 80Pa, vacuum impregnation 5h discharges to get nonisulated heat conduction adhesive.The nanometer compounds metal-powder
It is 100 in mass ratio by nanometer iron powder and nanometer aluminium powder：1 compounds.The epobond epoxyn is by following parts by weight
Several raw materials compound：120 parts of epoxy resin E-42,30 parts of benzyl alcohols, 15 parts of ethylenediamines, 5 parts of dibutyl phthalates.
It is 1 in mass ratio：Nanometer is compounded metal-powder and absolute ethyl alcohol by 50 to be mixed and pours into No. 1 beaker, and by beaker
Ultrasonic disperse instrument is moved into, under the conditions of supersonic frequency is 50kHz, after ultrasonic disperse 4h, No. 1 beaker is moved into digital display and is tested the speed constant temperature
Magnetic stirring apparatus is 45 DEG C in temperature, and under the conditions of rotating speed is 600r/min, heating stirring mixes 15h, obtains metal-powder dispersion
Liquid；It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：No. 2 beakers are poured into 10 mixing, and No. 2 beakers are moved into ultrasound and are shaken
Instrument is swung, under the conditions of supersonic frequency is 50kHz, sonic oscillation 60min obtains butyl titanate dispersion liquid, then counts in parts by weight,
80 parts of metal-powder dispersion liquids, 20 parts of butyl titanate dispersion liquids, the ammonium hydroxide that 8 parts of mass fractions are 15%, first by metal are taken successively
Three-necked flask is added in powder dispersion, is under 400r/min stirrings, by dropping funel with 5mL/min rates then at rotating speed
It is added dropwise in three-necked flask, ammonium hydroxide is added dropwise to three mouthfuls after butyl titanate dispersion liquid is added dropwise, then with 4mL/min rates
In flask, after ammonium hydroxide is added dropwise, in being stirred to react under room temperature for 24 hours, metal-powder suspension is obtained；By ethyl orthosilicate
It is 1 in mass ratio with absolute ethyl alcohol：30 mixing are poured into No. 3 beakers, and the dilute hydrochloric acid for being 12% with mass fraction adjusts No. 3 beakers
After middle material pH to 3.4, then the boric acid solution that the mass fraction of 0.4 times of absolute ethyl alcohol quality is 10% is added into No. 3 beakers,
It it is then 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, obtains hydrolyzate；It counts in parts by weight, according to
It is secondary to take 120 parts of hydrolyzates, 50 parts of metal-powder suspension, 30 parts of acrylamides, 6 parts of N, N '-methylene-bisacrylamides, 0.8
Part ammonium persulfate, mixing are poured into reaction kettle, are 85 DEG C in temperature, and under the conditions of rotating speed is 800r/min, heating stirring reacts 6h,
Wet gel, it is dry to constant weight then by gained wet gel under the conditions of temperature is 110 DEG C, obtain xerogel, and by gained xerogel
The sodium hydroxide solution for being 8% with mass fraction is placed in No. 1 sink, under the conditions of supersonic frequency is 60kHz, is ultrasonically treated
After 60min, single-steeping wet gel is obtained, gained single-steeping wet gel is washed with deionized to cleaning solution and is in neutrality, then
By after washing single-steeping wet gel and mass fraction be 15% copper-bath pour into No. 2 sinks, and be with frequency
Under the conditions of 60kHz, after ultrasonic immersing 90min, filtering obtains filter cake, absolute ethyl alcohol washing filter cake is used in combination 6 times, then will be after washing
Filter cake is transferred in baking oven, and under the conditions of temperature is 90 DEG C, dry 5h obtains double-steeping xerogel；By epobond epoxyn with
Double-steeping xerogel is 3 in mass ratio：1 mixing is poured into batch mixer, after rotating speed is 800r/min stirrings 5h, in vacuum degree
Under the conditions of 80Pa, vacuum impregnation 5h discharges to get nonisulated heat conduction adhesive.The nanometer compounding metal-powder is by receiving
Rice iron powder and nanometer aluminium powder are 100 in mass ratio：1 compounds.The epobond epoxyn is by following parts by weight
Raw material compounds：120 parts of epoxy resin E-42,30 parts of benzyl alcohols, 15 parts of ethylenediamines, 5 parts of dibutyl phthalates.
It is 1 in mass ratio：50 pour into nanometer iron powder and absolute ethyl alcohol mixing in No. 1 beaker, and beaker is moved into ultrasound
Separating apparatus after ultrasonic disperse 4h, then absolute ethyl alcohol quality 0.3 is added into No. 1 beaker under the conditions of supersonic frequency is 50kHz
Times mass concentration be 2g/L dopamine solution, after continuing ultrasonic disperse 60min, No. 1 beaker is moved into digital display and is tested the speed constant temperature
Magnetic stirring apparatus is 45 DEG C in temperature, and under the conditions of rotating speed is 600r/min, heating stirring mixes 15h, obtains metal-powder dispersion
Liquid；It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：No. 2 beakers are poured into 10 mixing, and No. 2 beakers are moved into ultrasound and are shaken
Instrument is swung, under the conditions of supersonic frequency is 50kHz, sonic oscillation 60min obtains butyl titanate dispersion liquid, then counts in parts by weight,
80 parts of metal-powder dispersion liquids, 20 parts of butyl titanate dispersion liquids, the ammonium hydroxide that 8 parts of mass fractions are 15%, first by metal are taken successively
Three-necked flask is added in powder dispersion, is under 400r/min stirrings, by dropping funel with 5mL/min rates then at rotating speed
It is added dropwise in three-necked flask, ammonium hydroxide is added dropwise to three mouthfuls after butyl titanate dispersion liquid is added dropwise, then with 4mL/min rates
In flask, after ammonium hydroxide is added dropwise, in being stirred to react under room temperature for 24 hours, metal-powder suspension is obtained；By ethyl orthosilicate
It is 1 in mass ratio with absolute ethyl alcohol：30 mixing are poured into No. 3 beakers, and the dilute hydrochloric acid for being 12% with mass fraction adjusts No. 3 beakers
After middle material pH to 3.4, then the boric acid solution that the mass fraction of 0.4 times of absolute ethyl alcohol quality is 10% is added into No. 3 beakers,
It it is then 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, obtains hydrolyzate；It counts in parts by weight, according to
It is secondary to take 120 parts of hydrolyzates, 50 parts of metal-powder suspension, 30 parts of acrylamides, 6 parts of N, N '-methylene-bisacrylamides, 0.8
Part ammonium persulfate, mixing are poured into reaction kettle, are 85 DEG C in temperature, and under the conditions of rotating speed is 800r/min, heating stirring reacts 6h,
Wet gel, it is dry to constant weight then by gained wet gel under the conditions of temperature is 110 DEG C, obtain xerogel, and by gained xerogel
The sodium hydroxide solution for being 8% with mass fraction is placed in No. 1 sink, under the conditions of supersonic frequency is 60kHz, is ultrasonically treated
After 60min, single-steeping wet gel is obtained, gained single-steeping wet gel is washed with deionized to cleaning solution and is in neutrality, then
By after washing single-steeping wet gel and mass fraction be 15% copper-bath pour into No. 2 sinks, and be with frequency
Under the conditions of 60kHz, after ultrasonic immersing 90min, filtering obtains filter cake, absolute ethyl alcohol washing filter cake is used in combination 6 times, then will be after washing
Filter cake is transferred in baking oven, and under the conditions of temperature is 90 DEG C, dry 5h obtains double-steeping xerogel；By epobond epoxyn with
Double-steeping xerogel is 3 in mass ratio：1 mixing is poured into batch mixer, after rotating speed is 800r/min stirrings 5h, in vacuum degree
Under the conditions of 80Pa, vacuum impregnation 5h discharges to get nonisulated heat conduction adhesive.The epobond epoxyn is by following
The raw material of parts by weight compounds：120 parts of epoxy resin E-42,30 parts of benzyl alcohols, 15 parts of ethylenediamines, 5 parts of phthalic acids
Dibutyl ester.
It is 1 in mass ratio：Nanometer is compounded metal-powder and absolute ethyl alcohol by 50 to be mixed and pours into No. 1 beaker, and by beaker
Ultrasonic disperse instrument is moved into, under the conditions of supersonic frequency is 50kHz, after ultrasonic disperse 4h, then absolute ethyl alcohol is added into No. 1 beaker
The mass concentration that 0.3 times of quality is the dopamine solution of 2g/L, after continuing ultrasonic disperse 60min, No. 1 beaker is moved into digital display and is surveyed
Fast constant temperature blender with magnetic force is 45 DEG C in temperature, and under the conditions of rotating speed is 600r/min, heating stirring mixes 15h, obtains metal-powder
Dispersion liquid；It is 1 in mass ratio by ethyl orthosilicate and absolute ethyl alcohol：30 mixing are poured into No. 3 beakers, are 12% with mass fraction
Dilute hydrochloric acid adjust in No. 3 beakers after material pH to 3.4, then the quality point of 0.4 times of absolute ethyl alcohol quality is added into No. 3 beakers
Number is 10% boric acid solution, is then 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, must hydrolyze
Liquid；It counts in parts by weight, takes 120 parts of hydrolyzates successively, 50 parts of metal-powder dispersion liquids, 30 parts of acrylamides, 6 parts of N, N '-are sub-
Bisacrylamide, 0.8 part of ammonium persulfate, mixing are poured into reaction kettle, are 85 DEG C in temperature, rotating speed is 800r/min conditions
Under, heating stirring reacts 6h, obtains wet gel, then by gained wet gel under the conditions of temperature is 110 DEG C, dry to constant weight, obtains dry
Gel, and the sodium hydroxide solution that gained xerogel and mass fraction are 8% is placed in No. 1 sink, it is in supersonic frequency
Under the conditions of 60kHz, after being ultrasonically treated 60min, single-steeping wet gel is obtained, gained single-steeping wet gel is washed with deionized water
Wash to cleaning solution and be in neutrality, then by after washing single-steeping wet gel and mass fraction be 15% copper-bath pour into No. 2
In sink, and with frequency under the conditions of 60kHz, after ultrasonic immersing 90min, filtering obtains filter cake, and absolute ethyl alcohol is used in combination to wash filter cake
6 times, then the filter cake after washing is transferred in baking oven, under the conditions of temperature is 90 DEG C, dry 5h obtains double-steeping xerogel；It will
Epobond epoxyn is 3 in mass ratio with double-steeping xerogel：1 mixing pour into batch mixer, in rotating speed be 800r/min
After stirring 5h, under the conditions of vacuum degree is 80Pa, vacuum impregnation 5h discharges to get nonisulated heat conduction adhesive.The nanometer is multiple
With metal-powder be by nanometer iron powder and nanometer aluminium powder it is 100 in mass ratio：1 compounds.The epobond epoxyn is
It is compounded by the raw material of following parts by weight：120 parts of epoxy resin E-42,30 parts of benzyl alcohols, 15 parts of ethylenediamines, 5 parts of adjacent benzene
Dibutyl carboxylic acid.
It is 1 in mass ratio：Nanometer is compounded metal-powder and absolute ethyl alcohol by 50 to be mixed and pours into No. 1 beaker, and by beaker
Ultrasonic disperse instrument is moved into, under the conditions of supersonic frequency is 50kHz, after ultrasonic disperse 4h, then absolute ethyl alcohol is added into No. 1 beaker
The mass concentration that 0.3 times of quality is the dopamine solution of 2g/L, after continuing ultrasonic disperse 60min, No. 1 beaker is moved into digital display and is surveyed
Fast constant temperature blender with magnetic force is 45 DEG C in temperature, and under the conditions of rotating speed is 600r/min, heating stirring mixes 15h, obtains metal-powder
Dispersion liquid；It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：No. 2 beakers are poured into 10 mixing, and No. 2 beakers are moved into and are surpassed
Sound oscillation instrument, under the conditions of supersonic frequency is 50kHz, sonic oscillation 60min obtains butyl titanate dispersion liquid, then by weight
Several meters take 80 parts of metal-powder dispersion liquids, 20 parts of butyl titanate dispersion liquids, the ammonium hydroxide that 8 parts of mass fractions are 15%, elder generation successively
Three-necked flask is added in metal-powder dispersion liquid, is under 400r/min stirrings, by dropping funel with 5mL/ then at rotating speed
Min rates are added dropwise in three-necked flask, drip ammonium hydroxide after butyl titanate dispersion liquid is added dropwise, then with 4mL/min rates
It adds in three-necked flask, after ammonium hydroxide is added dropwise, in being stirred to react under room temperature for 24 hours, obtains metal-powder suspension；It will just
Silester and absolute ethyl alcohol are 1 in mass ratio：30 mixing are poured into No. 3 beakers, and the dilute hydrochloric acid for being 12% with mass fraction is adjusted
In No. 3 beakers after material pH to 3.4, then the boron that the mass fraction of 0.4 times of absolute ethyl alcohol quality is 10% is added into No. 3 beakers
Acid solution is then 35 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, obtains hydrolyzate；By weight
Number meter, takes 120 parts of hydrolyzates, 50 parts of metal-powder suspension, 30 parts of acrylamides, 6 parts of N, N '-methylene bisacrylamide acyls successively
Amine, 0.8 part of ammonium persulfate, mixing pour into reaction kettle, in temperature be 85 DEG C, rotating speed be 800r/min under the conditions of, heating stirring
6h is reacted, obtains wet gel, then by gained wet gel under the conditions of temperature is 110 DEG C, it is dry to constant weight, obtain xerogel, and by institute
It obtains the sodium hydroxide solution that xerogel and mass fraction are 8% to be placed in No. 1 sink, under the conditions of supersonic frequency is 60kHz, surpass
After sonication 60min, single-steeping wet gel is obtained, is 3 in mass ratio by epobond epoxyn and single-steeping wet gel：1
Mixing is poured into batch mixer, is after 800r/min stirs 5h in rotating speed, under the conditions of vacuum degree is 80Pa, vacuum impregnation 5h goes out
Material is to get nonisulated heat conduction adhesive.The nanometer compounding metal-powder is to be in mass ratio by nanometer iron powder and nanometer aluminium powder
100：1 compounds.The epobond epoxyn is compounded by the raw material of following parts by weight：120 parts of epoxy resin
E-42,30 parts of benzyl alcohols, 15 parts of ethylenediamines, 5 parts of dibutyl phthalates.
It is 3 in mass ratio by epobond epoxyn and nanometer compounding metal-powder：1 mixing pour into batch mixer, in turn
Speed is after 800r/min stirs 5h, and under the conditions of vacuum degree is 80Pa, vacuum impregnation 5h discharges to get nonisulated heat conduction gluing
Agent.It is 100 in mass ratio that the nanometer compounding metal-powder, which is by nanometer iron powder and nanometer aluminium powder,：1 compounds.The epoxy
Resin binder is compounded by the raw material of following parts by weight：120 parts of epoxy resin E-42,30 parts of benzyl alcohols, 15 parts of second
Diamines, 5 parts of dibutyl phthalates.
Comparative example：The heat conduction adhesive of Liyang adhesive product factory production.
1 to 6 gained heat conduction adhesive of example and comparative example product are subjected to performance detection, specific detection method is as follows：
Thermal coefficient：It is measured using thermal conductivity coefficient measurement instrument.Each sample testing 3 times, results are averaged.Specific detection
The results are shown in Table 1：
Table 1：Performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example |
| Thermal coefficient/W（m·K）-1 | 1.17 | 0.81 | 0.75 | 0.78 | 0.83 | 0.82 | 0.52 |
By 1 testing result of table it is found that the nonisulated heat conduction adhesive of present invention gained has excellent heat conductivility.
Claims (3)
1. a kind of preparation method of nonisulated heat conduction adhesive, it is characterised in that specifically preparation process is：
（1）It is 1 that nanometer, which is compounded metal-powder and absolute ethyl alcohol in mass ratio,：10~1：After 50 mixing, ultrasonic disperse adds
The dopamine solution that 0.1~0.3 times of absolute ethyl alcohol quality, after continuing ultrasonic disperse, heating stirring mixes 10~15h, obtains metal
Powder dispersion；
（2）It is 1 in mass ratio by butyl titanate and absolute ethyl alcohol：8~1：10 ultrasonic mixings obtain butyl titanate dispersion liquid,
It counts in parts by weight again, takes 60~80 parts of metal-powder dispersion liquids, 10~20 parts of butyl titanate dispersion liquids, 6~8 parts of ammonia successively
Butyl titanate dispersion liquid is first added dropwise to 3~5mL/min rates in metal-powder dispersion liquid by water, waits for butyl titanate point
After dispersion liquid is added dropwise, then with 2~4mL/min rates ammonium hydroxide is added dropwise in metal-powder dispersion liquid, waits for that ammonium hydroxide is added dropwise,
In be stirred to react 16 under room temperature~for 24 hours after, obtain metal-powder suspension；
（3）It is 1 in mass ratio by ethyl orthosilicate and absolute ethyl alcohol：20~1：30 mixing after, with dilute hydrochloric acid adjust pH to 3.2~
3.4, the boric acid solution of 0.2~0.4 times of absolute ethyl alcohol quality is added, constant temperature is stirred to react, and obtains hydrolyzate；
（4）It counts in parts by weight, takes 80~120 parts of hydrolyzates, 40~50 parts of metal-powder suspension, 10~30 parts of propylene successively
Amide, 4~6 parts of N, N '-methylene-bisacrylamides, 0.6~0.8 part of ammonium persulfate, after mixing, heating stirring reaction obtains wet
Gel, then by after the drying of gained wet gel, be impregnated in sodium hydroxide solution, after being ultrasonically treated 40~60min, obtain single-steeping
Wet gel；
（5）Single-steeping wet gel is washed with water to after neutrality and copper-bath mixes, after 60~90min of ultrasonic immersing,
Successively through being filtered, washed and dried drying, double-steeping xerogel is obtained；
（6）It is 1 in mass ratio by epobond epoxyn and double-steeping xerogel：1~3：1 mixing, then after vacuum impregnation,
Discharging is to get nonisulated heat conduction adhesive.
2. a kind of preparation method of nonisulated heat conduction adhesive according to claim 1, it is characterised in that：Step（1）Institute
It is 50 in mass ratio that state nanometer compounding metal-powder, which be by nanometer iron powder and nanometer aluminium powder,：1~100：1 compounds.
3. a kind of preparation method of nonisulated heat conduction adhesive according to claim 1, it is characterised in that：Step（6）Institute
Stating epobond epoxyn is compounded by the raw material of following parts by weight：80~120 parts of epoxy resin E-42,20~30 parts
Benzyl alcohol, 10~15 parts of ethylenediamines, 3~5 parts of dibutyl phthalates.
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| CN110330899A (en) * | 2019-06-27 | 2019-10-15 | 浙江森井科技股份有限公司 | A kind of adhesive and preparation method thereof for photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880399A (en) * | 2005-06-16 | 2006-12-20 | 鸿富锦精密工业（深圳）有限公司 | Thermally conductive glue and method of manufacturing same |
| CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880399A (en) * | 2005-06-16 | 2006-12-20 | 鸿富锦精密工业（深圳）有限公司 | Thermally conductive glue and method of manufacturing same |
| CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330899A (en) * | 2019-06-27 | 2019-10-15 | 浙江森井科技股份有限公司 | A kind of adhesive and preparation method thereof for photocatalyst |
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