CN108219730A - The preparation method and its conductive adhesive of a kind of conductive adhesive - Google Patents
The preparation method and its conductive adhesive of a kind of conductive adhesive Download PDFInfo
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- CN108219730A CN108219730A CN201810040649.4A CN201810040649A CN108219730A CN 108219730 A CN108219730 A CN 108219730A CN 201810040649 A CN201810040649 A CN 201810040649A CN 108219730 A CN108219730 A CN 108219730A
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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
- C09J163/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- 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
- C09J11/08—Macromolecular additives
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- 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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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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
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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Abstract
The preparation method and its conductive adhesive of a kind of conductive adhesive, it belongs to conductive adhesive production field.Stromatolysis is carried out after present invention synthesis diamines, synthesis of polyimides; according to parts by weight weigh 50~120 parts polyimides, 100~200 parts of epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~20 parts of curing agent, 10~20 parts of accelerating agent; by polyimides, epoxy resin, activation dispersant under the protection of argon gas; it stirs evenly, the mixing of additive：After load weighted conductive filler, toughener, accelerating agent are added in the dispersion of high speed dispersor high speed grinding, by dissolved matrix, additive package and load weighted curing agent, it adds in high energy shear stirred autoclave, after stirring evenly, vacuum vibration deaeration after taking-up obtains the conductive adhesive.Normal temperature cure of the present invention is suitble to high-volume, assembly line application.
Description
Technical field
The invention belongs to conductive adhesive production fields；More particularly to the preparation method and its conduction of a kind of conductive adhesive
Adhesive.
Background technology
Conductive adhesive is to adapt to the adhesive kind that electronics industry development need occurs, it is used for electric appliance and electronic assemblies
The place of connection circuit is needed in the process, is welded with viscous generation.It needs to be heated at high temperature using solder welding, is sometimes prone to damage first device
Part；Control also is difficult to accurately to weld using minimal amount of solder or extremely.Conductive adhesive is more preferably connected than welding
Method, it can not only replace welding, but also electrocondution slurry can be made, using its good bonding performance to many materials,
Pattern line is printed on the wiring board of unlike material, as conducting wire.
The performance of conductive adhesive depend on select binder (resin) system, the type of conductive filler and content and
Hardening time.Conductive adhesive except with general adhesive should with performance in addition to, be exactly mainly its electric conductivity --- resistivity
(or its conductivity reciprocal), unit are Ω cm.Rule of thumb, solidification temperature is high, and hardening time is long, and resistivity is with regard to low.
Conductive adhesive is made of electroconductive stuffing, binder, solvent and additive.(1) electroconductive stuffing is common
Electroconductive stuffing has：Metal powder, graphite powder, acetylene carbon black and carbon fiber etc., wherein being most widely used with metal powder.In metal
In powder, bronze chemical stability is good, and electric conductivity is high, but at high price, be only used for requiring height reliability Aeronautics and Astronautics or
In military project etc. and thick film integrated circuit；Copper powder, aluminium powder, nickel powder are then oxidizable, and electric conductivity is unstable；Using it is most be silver
Powder.
Silver powder has excellent electric conductivity and corrosion resistance, aoxidizes in air extremely slowly, therefore is comparatively ideal conductive filler.
The size and shape of silver powder has a great impact to the electric conductivity for preparing conducting resinl.In general particle is smaller, shape more not
Regular (such as dendroid) its electric conductivity is better.The shortcomings that silver powder, is that density is big, easily precipitates, migration.Since migration can cause
Defective insulation, it was reported that adding in palladium can prevent from migrating.In addition, the resin material that glass transition temperature is high, hygroscopicity is low is selected to match glue
Migration can also be improved.Charcoal, graphite isodispersity are preferable, and price is low, but poorly conductive (ρ v=10-2~106Qcm), moisture-proof
Property is bad.If not cause specific does not use generally.Resin, solvent and additive is common one pack system and bi-component epoxy tree
Fat glue, because its solidfied material is tough and tensile, wear-resisting and heat-resisting, so being usually used in hardware.In use, diluent can be added in glue, with
Viscosity and rate of drying are adjusted, it is more usually using alcohols, esters solvent.
Invention content
It is an object of the present invention to provide the preparation methods and its conductive adhesive of a kind of conductive adhesive.
The invention is realized by the following technical scheme：
A kind of preparation method of conductive adhesive, includes the following steps：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weigh the bromo- 5- nitrotoleunes of Soquad, 2-,
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature by cyclodextrin, natrium carbonicum calcinatum afterwards
10~12h of back flow reaction, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 add in reaction vessel, add by distilled water,
The mixed solvent of acetone composition, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, and is adjusted
PH value after the reaction was continued 6~7h, stops heating to 3~4, then adds in hydrazine hydrate to adjust pH value to 8~9, stirs evenly,
Product is filtered while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetracarboxylic acid that step 1 synthesizes
Acid dianhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, will be mixed after reaction
Solution submerged in the water is closed, by the powder of precipitation, obtains polyimides after washing, drying, for use；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~
200 parts of epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~
20 parts of curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant in argon gas
It under protection, stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersion
After the dispersion of machine high speed grinding, for use；
The preparation of step 5, conductive adhesive：The mixing that dissolved matrix, step 4 that step 3 obtains are obtained is added
Agent and the load weighted curing agent of step 3 are added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration takes off after taking-up
Bubble obtains the conductive adhesive.
A kind of preparation method of conductive adhesive of the present invention, synthesizing for diamines is according to mass ratio in step 1
1：5：5：0.2 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, cyclodextrin, natrium carbonicum calcinatum, and load weighted material mixing is equal
The ethyl alcohol of 10 times of volumes is added in after even, under protection of argon gas high temperature reflux reacts 10h, after solution cooling, what washing reaction was precipitated
Solid and iron powder according to mass ratio are 1 after dry by solid：0.2 adds in reaction vessel, adds and is made of distilled water, acetone
Mixed solvent, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, adjust pH value to
After 3.5, the reaction was continued 6.5h, stop heating, then add in hydrazine hydrate to adjust pH value to 8.5, stir evenly, by product while hot
Filtering, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines.
A kind of preparation method of conductive adhesive of the present invention, in step 2 polyimides synthesize according to mole
Than being 1：2：9 weigh diamines, benzophenone tetracarboxylic dianhydride, the solvent that step 1 synthesizes, and add in reaction kettle after weighing, are protected in argon gas
Under shield, agitating and heating carries out back flow reaction, and the mixed solution submerged in the water after reaction washs, the powder of precipitation after drying
Obtain polyimides.
A kind of preparation method of conductive adhesive of the present invention, the epoxy resin in step 3 are polyurethane-modified more
First alcohol flexibilizing epoxy acrylic monoester or polyurethane-modified aliphatic acid flexibilizing epoxy acrylic monoester, activation dispersant are ethyoxyl
Bisphenol-A or diacrylate or ethoxylated glycerol triacrylate, conductive filler are nano-silver powder or carbon nanotube or carbon amounts
Sub-, toughener is methacryloxypropyl trimethoxy silane or mercaptopropyltriethoxysilane, and curing agent is tetrahydrochysene
Phthalic enhydride or hexahydro phthalic enhydride, accelerating agent are imidazoles or triethanolamine.
A kind of preparation method of conductive adhesive of the present invention, the parts by weight of raw material are 85 parts of step in step 3
Rapid 2 polyimides prepared, 135 parts of epoxy resin, 45 parts of activation dispersant, 70 parts of conductive filler, 8 parts of toughening
Agent, 8 parts of curing agent, 8 parts of accelerating agent.
A kind of preparation method of conductive adhesive of the present invention, the parts by weight of raw material are 105 parts of step in step 3
Rapid 2 polyimides prepared, 160 parts of epoxy resin, 66 parts of activation dispersant, 110 parts of conductive filler, 14 parts of toughening
Agent, 14 parts of curing agent, 14 parts of accelerating agent.
A kind of preparation method of conductive adhesive of the present invention, the power of step 4 high speed dispersion machine for 500~
1500W, rotating speed are 1000~5000r/min, 1~30min of rotation time.
A kind of preparation method of conductive adhesive of the present invention, the power of high energy shear reaction kettle is 2.2 in step 5
~5KW, rotating speed 2900r/min, 1~30min of rotation time.
A kind of conductive adhesive of the present invention, the adhesive is according to parts by weight by the raw material of following parts by weight
It is made：50~120 parts of polyimides, 100~200 parts of epoxy resin, 30~80 parts of activation dispersant, 15~150 parts
Conductive filler, 5~15 parts of toughener, 10~20 parts of curing agent, 10~20 parts of accelerating agent；The adhesive by with
Lower section method is made：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weigh the bromo- 5- nitrotoleunes of Soquad, 2-,
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature by cyclodextrin, natrium carbonicum calcinatum afterwards
10~12h of back flow reaction, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 add in reaction vessel, add by distilled water,
The mixed solvent of acetone composition, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, and is adjusted
PH value after the reaction was continued 6~7h, stops heating to 3~4, then adds in hydrazine hydrate to adjust pH value to 8~9, stirs evenly,
Product is filtered while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetracarboxylic acid that step 1 synthesizes
Acid dianhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, will be mixed after reaction
Solution submerged in the water is closed, by the powder of precipitation, obtains polyimides after washing, drying, for use；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~
200 parts of epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~
20 parts of curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant in argon gas
It under protection, stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersion
After the dispersion of machine high speed grinding, for use；
The preparation of step 5, conductive adhesive：The mixing that dissolved matrix, step 4 that step 3 obtains are obtained is added
Agent and the load weighted curing agent of step 3 are added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration takes off after taking-up
Bubble obtains the conductive adhesive.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive of the present invention carries out contact resistance survey
30mm × 30mm × 10mm copper billets with 80# water-proof abrasive papers are polished, are cleaned with alcohol wipe by examination in advance, with clamping dress after drying
It puts and clamps test naked copper contact resistance, then uniformly coating conductive film again, its contact is electric with same torque clamping test again
Resistance, comparison record smear contact resistance variation size before and after conductive film, and every group of data test is averaged for 10 times, conductive gluing
The volume resistivity minimum 2.36 × 10 of agent-5Ωcm。
Conductive adhesive prepared by a kind of preparation method of conductive adhesive of the present invention carries out brine soaking experiment
Test, conductive adhesive is coated uniformly on copper billet contact interface, then with gripping means grips are made by oneself, is immersed at room temperature dense
It spends for 48 hours in 5%NaCl solution, the variation of contact resistance before and after test is impregnated；It is surveyed again after further impregnating 7 days again
Measure contact resistance.Every group of test measurement is averaged for 10 times in experiment, and the resistivity of conductive adhesive can subtract after saline sook
Small, conductive adhesive can react generation chelate with ionizable metal salt, so as to reduce the volume resistivity of conductive adhesive.
Therefore salt water immersion test is caused not generate the effect of corrosion to copper billet not only, instead results in contact resistance reduction, so this
A kind of invention conductive adhesive also is able to have corrosion-resistant effect to metal coated.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive of the present invention, can protect metal to contact
Contact (area) pattern between surface is not corroded, and conventional method is to the protection Shortcomings of contact (area) pattern, it is impossible to effectively long-term to make
Contact resistance stabilization is in lower value level.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive of the present invention, substantially prolongs applicable
Phase, there is good high temperature resistance, corrosion resistance has higher thermal conductivity, conductivity and high temperature resistance, Neng Gou
It is fully cured at room temperature.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive of the present invention, it is solvent-free, it is easy to operate,
Joining Technology is convenient, is suitble to high-volume, assembly line application.
Specific embodiment
Specific embodiment one：
A kind of preparation method of conductive adhesive, includes the following steps：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weigh the bromo- 5- nitrotoleunes of Soquad, 2-,
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature by cyclodextrin, natrium carbonicum calcinatum afterwards
10~12h of back flow reaction, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 add in reaction vessel, add by distilled water,
The mixed solvent of acetone composition, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, and is adjusted
PH value after the reaction was continued 6~7h, stops heating to 3~4, then adds in hydrazine hydrate to adjust pH value to 8~9, stirs evenly,
Product is filtered while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetracarboxylic acid that step 1 synthesizes
Acid dianhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, will be mixed after reaction
Solution submerged in the water is closed, by the powder of precipitation, obtains polyimides after washing, drying, for use；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~
200 parts of epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~
20 parts of curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant in argon gas
It under protection, stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersion
After the dispersion of machine high speed grinding, for use；
The preparation of step 5, conductive adhesive：The mixing that dissolved matrix, step 4 that step 3 obtains are obtained is added
Agent and the load weighted curing agent of step 3 are added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration takes off after taking-up
Bubble obtains the conductive adhesive.
A kind of preparation method of conductive adhesive described in present embodiment, diamines synthesizes according to quality in step 1
Than being 1：5：5：0.2 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, cyclodextrin, natrium carbonicum calcinatum, and load weighted substance is mixed
The ethyl alcohol of 10 times of volumes is added in after closing uniformly, under protection of argon gas high temperature reflux reacts 10h, after solution cooling, washing reaction analysis
Solid and iron powder according to mass ratio are 1 after dry by the solid gone out：0.2 adds in reaction vessel, adds by distilled water, acetone
Under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to for the mixed solvent of composition, adjusts pH value
To 3.5, after the reaction was continued 6.5h, stop heating, then add in hydrazine hydrate to adjust pH value to 8.5, stir evenly, product is taken advantage of
Heat filtering is recrystallized with ethanol water, after vacuum drying, synthesizes diamines.
A kind of preparation method of conductive adhesive described in present embodiment, in step 2 polyimides synthesize according to
Molar ratio is 1：2：9 weigh diamines, benzophenone tetracarboxylic dianhydride, the solvent that step 1 synthesizes, and are added in reaction kettle after weighing, in argon
Under gas shielded, agitating and heating carries out back flow reaction, and by the mixed solution submerged in the water after reaction, by the powder of precipitation, washing is done
Polyimides is obtained after dry.
A kind of preparation method of conductive adhesive described in present embodiment, the epoxy resin in step 3 change for polyurethane
Property polyalcohol flexibilizing epoxy acrylic monoester or polyurethane-modified aliphatic acid flexibilizing epoxy acrylic monoester, activation dispersant is second
Oxygroup bisphenol-A or diacrylate or ethoxylated glycerol triacrylate, conductive filler for nano-silver powder or carbon nanotube or
Carbon quantum dot, toughener are methacryloxypropyl trimethoxy silane or mercaptopropyltriethoxysilane, and curing agent is
Tetrahydrochysene phthalic enhydride or hexahydro phthalic enhydride, accelerating agent are imidazoles or triethanolamine.
A kind of preparation method of conductive adhesive described in present embodiment, the parts by weight of raw material are 85 parts in step 3
Step 2 prepare polyimides, 135 parts of epoxy resin, 45 parts activation dispersant, 70 parts of conductive filler, 8 parts of increasing
Tough dose, 8 parts of curing agent, 8 parts of accelerating agent.
A kind of preparation method of conductive adhesive described in present embodiment, the power of step 4 high speed dispersion machine are
1500W, rotating speed 5000r/min, rotation time 5min.
A kind of preparation method of conductive adhesive described in present embodiment, the power of high energy shear reaction kettle in step 5
For 5KW, rotating speed 2900r/min, rotation time 10min.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive described in present embodiment carries out contact resistance
30mm × 30mm × 10mm copper billets with 80# water-proof abrasive papers are polished, are cleaned with alcohol wipe, with clamping after drying by test in advance
Device clamping test naked copper contact resistance, then uniformly coating conductive film again, with same torque clamping test, its contact is electric again
Resistance, comparison record smear contact resistance variation size before and after conductive film, and every group of data test is averaged test result 10 times
As shown in table 1：It can convert and obtain from table 1, the volume resistivity of conductive adhesive is 2.36 × 10-5Ωcm。
Contact resistance contrast table (unit μ Ω) before and after a kind of conductive adhesive described in 1 present embodiment of table is smeared
Conductive adhesive prepared by a kind of preparation method of conductive adhesive described in present embodiment carries out saline sook
Conductive adhesive is coated uniformly on copper billet contact interface by experiment test, then with gripping means grips are made by oneself, is impregnated at room temperature
48 hours in a concentration of 5%NaCl solution, the variation of contact resistance before and after test is impregnated；After further impregnating 7 days again again
Secondary measurement contact resistance.Every group of test measurement is averaged for 10 times in experiment, and test result is as shown in table 2：It is led after saline sook
The resistivity of electric adhesive can reduce, main cause be a kind of conductive adhesive described in present embodiment can and metal salt
Ionic reaction generates chelate, so as to reduce the volume resistivity of conductive adhesive.Therefore lead to salt water immersion test not only
The effect of corrosion is not generated to copper billet, contact resistance reduction is instead resulted in, so a kind of conducting resinl described in present embodiment
Stick also is able to have corrosion-resistant effect to metal coated.
Contact resistance contrast table (unit μ Ω) before and after a kind of conductive adhesive saline sook described in 2 present embodiment of table
Specific embodiment two：
A kind of preparation method of conductive adhesive, includes the following steps：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：1 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, ring paste
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature reflux by essence, natrium carbonicum calcinatum afterwards
12h is reacted, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.5 adds in reaction vessel, adds by distilled water, acetone group
Into mixed solvent, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, adjust pH value to
After 4, the reaction was continued 7h, stop heating, then add in hydrazine hydrate to adjust pH value to 9, stir evenly, product is filtered while hot,
It is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：10 weigh diamines, the benzophenone tetrabasic carboxylic acid two that step 1 synthesizes
Acid anhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, and the mixing after reaction is molten
Liquid submerged in the water by the powder of precipitation, obtains polyimides, for use after washing, drying；
Step 3, stromatolysis：Polyimides, 200 parts of the epoxy of 120 parts of step 2 preparation are weighed according to parts by weight
Resin, 80 parts of activation dispersant, 150 parts of conductive filler, 15 parts of toughener, 20 parts of curing agent, 20 parts of accelerating agent,
By load weighted polyimides, epoxy resin, activation dispersant under the protection of argon gas, stir evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersion
After the dispersion of machine high speed grinding, for use；
The preparation of step 5, conductive adhesive：The mixing that dissolved matrix, step 4 that step 3 obtains are obtained is added
Agent and the load weighted curing agent of step 3 are added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration takes off after taking-up
Bubble obtains the conductive adhesive.
A kind of preparation method of conductive adhesive described in present embodiment, the epoxy resin in step 3 change for polyurethane
Property polyalcohol flexibilizing epoxy acrylic monoester or polyurethane-modified aliphatic acid flexibilizing epoxy acrylic monoester, activation dispersant is second
Oxygroup bisphenol-A or diacrylate or ethoxylated glycerol triacrylate, conductive filler for nano-silver powder or carbon nanotube or
Carbon quantum dot, toughener are methacryloxypropyl trimethoxy silane or mercaptopropyltriethoxysilane, and curing agent is
Tetrahydrochysene phthalic enhydride or hexahydro phthalic enhydride, accelerating agent are imidazoles or triethanolamine.
A kind of preparation method of conductive adhesive described in present embodiment, the power of step 4 high speed dispersion machine are
500W, rotating speed 1000r/min, rotation time 30min.
A kind of preparation method of conductive adhesive described in present embodiment, the power of high energy shear reaction kettle in step 5
For 2.2KW, rotating speed 2900r/min, rotation time 10min.
Conductive adhesive prepared by a kind of preparation method of conductive adhesive described in present embodiment carries out contact resistance
30mm × 30mm × 10mm copper billets with 80# water-proof abrasive papers are polished, are cleaned with alcohol wipe, with clamping after drying by test in advance
Device clamping test naked copper contact resistance, then uniformly coating conductive film again, with same torque clamping test, its contact is electric again
Resistance, comparison record smear contact resistance variation size before and after conductive film, and every group of data test is averaged test result 10 times
As shown in table 3：It can convert and obtain from table 3, the volume resistivity of conductive adhesive is 5.98 × 10-5Ωcm。
Contact resistance contrast table (unit μ Ω) before and after a kind of conductive adhesive described in 3 present embodiment of table is smeared
Conductive adhesive prepared by a kind of preparation method of conductive adhesive described in present embodiment carries out saline sook
Conductive adhesive is coated uniformly on copper billet contact interface by experiment test, then with gripping means grips are made by oneself, is impregnated at room temperature
48 hours in a concentration of 5%NaCl solution, the variation of contact resistance before and after test is impregnated；After further impregnating 7 days again again
Secondary measurement contact resistance.Every group of test measurement is averaged for 10 times in experiment, and test result is as shown in table 4：It is led after saline sook
The resistivity of electric adhesive can reduce, main cause be a kind of conductive adhesive described in present embodiment can and metal salt
Ionic reaction generates chelate, so as to reduce the volume resistivity of conductive adhesive.Therefore lead to salt water immersion test not only
The effect of corrosion is not generated to copper billet, contact resistance reduction is instead resulted in, so a kind of conducting resinl described in present embodiment
Stick also is able to have corrosion-resistant effect to metal coated.
Contact resistance contrast table (unit μ Ω) before and after a kind of conductive adhesive saline sook described in 4 present embodiment of table
Specific embodiment three：
A kind of preparation method of conductive adhesive, includes the following steps：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weigh the bromo- 5- nitrotoleunes of Soquad, 2-,
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature by cyclodextrin, natrium carbonicum calcinatum afterwards
10~12h of back flow reaction, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 add in reaction vessel, add by distilled water,
The mixed solvent of acetone composition, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, and is adjusted
PH value after the reaction was continued 6~7h, stops heating to 3~4, then adds in hydrazine hydrate to adjust pH value to 8~9, stirs evenly,
Product is filtered while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetracarboxylic acid that step 1 synthesizes
Acid dianhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, will be mixed after reaction
Solution submerged in the water is closed, by the powder of precipitation, obtains polyimides after washing, drying, for use；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~
200 parts of epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~
20 parts of curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant in argon gas
It under protection, stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersion
After the dispersion of machine high speed grinding, for use；
The preparation of step 5, conductive adhesive：The mixing that dissolved matrix, step 4 that step 3 obtains are obtained is added
Agent and the load weighted curing agent of step 3 are added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration takes off after taking-up
Bubble obtains the conductive adhesive.
Specific embodiment four：
A kind of preparation method of conductive adhesive according to specific embodiment three, diamines synthesizes in step 1
It is 1 according to mass ratio：5：5：0.2 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, cyclodextrin, natrium carbonicum calcinatum, will weigh
Material mixing uniformly add in the ethyl alcohol of 10 times of volumes afterwards, high temperature reflux reacts 10h under protection of argon gas after solution cooling, is washed
It washs the solid that reaction is precipitated, by solid and iron powder according to mass ratio is 1 after dry：0.2 adds in reaction vessel, adds by distilling
The mixed solvent of water, acetone composition, under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to, and is adjusted
PH value is saved to 3.5, after the reaction was continued 6.5h, stops heating, hydrazine hydrate is then added in adjust pH value to 8.5, stirs evenly, it will
Product filters while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines.
Specific embodiment five：
A kind of preparation method of conductive adhesive according to specific embodiment three, the conjunction of polyimides in step 2
As according to molar ratio be 1：2：9 weigh diamines, benzophenone tetracarboxylic dianhydride, the solvent that step 1 synthesizes, and reaction kettle is added in after weighing
In, under protection of argon gas, agitating and heating carries out back flow reaction, by the mixed solution submerged in the water after reaction, by the powder of precipitation,
Polyimides is obtained after washing, drying.
Specific embodiment six：
A kind of preparation method of conductive adhesive according to specific embodiment three, the epoxy resin in step 3 are
Polyurethane-modified polyalcohol flexibilizing epoxy acrylic monoester or polyurethane-modified aliphatic acid flexibilizing epoxy acrylic monoester, activation point
Powder is ethoxylated bisphenol A or diacrylate or ethoxylated glycerol triacrylate, and conductive filler is nano-silver powder or carbon
Nanotube or carbon quantum dot, toughener be methacryloxypropyl trimethoxy silane or mercaptopropyltriethoxysilane,
Curing agent is tetrahydrochysene phthalic enhydride or hexahydro phthalic enhydride, and accelerating agent is imidazoles or triethanolamine.
Specific embodiment seven：
A kind of preparation method of conductive adhesive according to specific embodiment three, the parts by weight of raw material in step 3
Number is filled out for the polyimides of 85 parts of step 2 preparation, 135 parts of epoxy resin, 45 parts of activation dispersant, 70 parts of conduction
Material, 8 parts of toughener, 8 parts of curing agent, 8 parts of accelerating agent.
Specific embodiment eight：
A kind of preparation method of conductive adhesive according to specific embodiment three, the parts by weight of raw material in step 3
Number is filled out for the polyimides of 105 parts of step 2 preparation, 160 parts of epoxy resin, 66 parts of activation dispersant, 110 parts of conduction
Material, 14 parts of toughener, 14 parts of curing agent, 14 parts of accelerating agent.
Specific embodiment nine：
A kind of preparation method of conductive adhesive according to specific embodiment three, step 4 high speed dispersion machine
Power is 500~1500W, and rotating speed is 1000~5000r/min, 1~30min of rotation time.
Specific embodiment ten：
A kind of preparation method of conductive adhesive according to specific embodiment three, high energy shear is reacted in step 5
The power of kettle is 2.2~5KW, rotating speed 2900r/min, 1~30min of rotation time.
Specific embodiment 11：
Conductive adhesive prepared by a kind of preparation method of conductive adhesive according to specific embodiment three, it is described
Adhesive be made according to parts by weight of the raw material of following parts by weight：50~120 parts of polyimides, 100~200 parts of ring
Oxygen resin, 30~80 parts of activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~20 parts consolidate
Agent, 10~20 parts of accelerating agent.
Conductive adhesive described in present embodiment carries out contact resistance test, and 30mm × 30mm × 10mm copper billets is pre-
It is first polished with 80# water-proof abrasive papers, is cleaned with alcohol wipe, test naked copper contact resistance with gripping means grips after drying, then
Uniformly the conductive film of coating is clamped with same torque test its contact resistance again again, and comparison record connects before and after smearing conductive film
Touch resistance variations sizes, every group of data test is averaged for 10 times, the volume resistivity minimum 2.36 × 10 of conductive adhesive-5
Ωcm。
Conductive adhesive described in present embodiment carries out brine soaking experiment test, conductive adhesive is uniformly coated
On copper billet contact interface, then with gripping means grips are made by oneself, it is immersed at room temperature in a concentration of 5%NaCl solution 48 hours,
The variation of contact resistance before and after test is impregnated；Contact resistance is measured again after further impregnating 7 days again.Every group of experiment in experiment
Measure and be averaged for 10 times, the resistivity of conductive adhesive can reduce after saline sook, conductive adhesive can and metal salt
Ionic reaction generates chelate, so as to reduce the volume resistivity of conductive adhesive.Therefore lead to salt water immersion test not only
The effect of corrosion is not generated to copper billet, contact resistance reduction is instead resulted in, so a kind of conductive adhesive of the present invention
It also is able to that there is corrosion-resistant effect to metal coated.
Conductive adhesive described in present embodiment can protect the contact (area) pattern between metal-contacting surface not corroded,
And conventional method is to the protection Shortcomings of contact (area) pattern, it is impossible to which effectively long-term makes contact resistance stabilization in lower value level.
Conductive adhesive described in present embodiment, substantially prolongs working life, has good high temperature resistance, corrosion resistant
Corrosion energy has higher thermal conductivity, conductivity and high temperature resistance, can be fully cured at room temperature, and when use directly applies
It smears.
Conductive adhesive described in present embodiment, solvent-free, easy to operate, Joining Technology is convenient, is suitble to high-volume, stream
Waterline application.
Claims (9)
1. a kind of preparation method of conductive adhesive, it is characterised in that：Include the following steps：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, ring paste
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature reflux by essence, natrium carbonicum calcinatum afterwards
10~12h is reacted, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 adds in reaction vessel, adds by distilled water, acetone
Under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to for the mixed solvent of composition, adjusts pH value
To 3~4, after the reaction was continued 6~7h, stop heating, then add in hydrazine hydrate to adjust pH value to 8~9, stir evenly, will produce
Object filters while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetrabasic carboxylic acid two that step 1 synthesizes
Acid anhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, and the mixing after reaction is molten
Liquid submerged in the water by the powder of precipitation, obtains polyimides, for use after washing, drying；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~200 parts
Epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~20 parts
Curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant argon gas protection
Under, it stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersor height
After fast grinding distribution, for use；
The preparation of step 5, conductive adhesive：Additive package that dissolved matrix, step 4 that step 3 obtains are obtained and
The load weighted curing agent of step 3 is added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration deaeration after taking-up obtains
To the conductive adhesive.
2. a kind of preparation method of conductive adhesive according to claim 1, it is characterised in that：The conjunction of diamines in step 1
As according to mass ratio be 1：5：5：0.2 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, cyclodextrin, natrium carbonicum calcinatum, will claim
Measured material mixing uniformly adds in the ethyl alcohol of 10 times of volumes afterwards, under protection of argon gas high temperature reflux reacts 10h, solution cooling
Afterwards, solid and iron powder according to mass ratio are 1 after dry by the solid that washing reaction is precipitated：0.2 adds in reaction vessel, adds
The mixed solvent being made of distilled water, acetone, it is after being heated with stirring to reflux temperature, dilute hydrochloric acid is slow under the protection of argon gas
It adds in, adjusts pH value to 3.5, after the reaction was continued 6.5h, stop heating, then add in hydrazine hydrate to adjust pH value to 8.5, stirring
Uniformly, product is filtered while hot, is recrystallized with ethanol water, after vacuum drying, synthesize diamines.
3. a kind of preparation method of conductive adhesive according to claim 1, it is characterised in that：Polyimides in step 2
Synthesize according to molar ratio be 1：2：9 weigh diamines, benzophenone tetracarboxylic dianhydride, the solvent that step 1 synthesizes, and are added in after weighing anti-
It answers in kettle, under protection of argon gas, agitating and heating carries out back flow reaction, by the mixed solution submerged in the water after reaction, by precipitation
Powder obtains polyimides after washing, drying.
4. a kind of preparation method of conductive adhesive according to claim 1, it is characterised in that：Asphalt mixtures modified by epoxy resin in step 3
Fat is polyurethane-modified polyalcohol flexibilizing epoxy acrylic monoester or polyurethane-modified aliphatic acid flexibilizing epoxy acrylic monoester, is lived
It is nano-silver powder to change dispersant as ethoxylated bisphenol A or diacrylate or ethoxylated glycerol triacrylate, conductive filler
Or carbon nanotube or carbon quantum dot, toughener are methacryloxypropyl trimethoxy silane or mercapto propyl-triethoxysilicane
Alkane, curing agent are tetrahydrochysene phthalic enhydride or hexahydro phthalic enhydride, and accelerating agent is imidazoles or triethanolamine.
5. a kind of preparation method of conductive adhesive according to claim 1 or 4, it is characterised in that：Raw material in step 3
Polyimides prepared by the step 2 that parts by weight are 85 parts, 135 parts of epoxy resin, 45 parts of activation dispersant, 70 parts lead
Electric filler, 8 parts of toughener, 8 parts of curing agent, 8 parts of accelerating agent.
6. a kind of preparation method of conductive adhesive according to claim 1 or 4, it is characterised in that：Raw material in step 3
Polyimides prepared by the step 2 that parts by weight are 105 parts, 160 parts of epoxy resin, 66 parts of activation dispersant, 110 parts
Conductive filler, 14 parts of toughener, 14 parts of curing agent, 14 parts of accelerating agent.
7. a kind of preparation method of conductive adhesive according to claim 1, it is characterised in that：Step 4 high speed is disperseed
The power of machine is 500~1500W, and rotating speed is 1000~5000r/min, 1~30min of rotation time.
8. a kind of preparation method of conductive adhesive according to claim 1, it is characterised in that：High energy shear in step 5
The power of reaction kettle is 2.2~5KW, rotating speed 2900r/min, 1~30min of rotation time.
9. a kind of conductive adhesive, it is characterised in that：The adhesive is according to parts by weight by the raw material system of following parts by weight
Into：50~120 parts of polyimides, 100~200 parts of epoxy resin, 30~80 parts of activation dispersant, 15~150 parts
Conductive filler, 5~15 parts of toughener, 10~20 parts of curing agent, 10~20 parts of accelerating agent；
The adhesive is made of following methods：
Step 1, synthesis diamines：It is 1 according to mass ratio：5：5：0.1~1 weighs the bromo- 5- nitrotoleunes of Soquad, 2-, ring paste
Load weighted material mixing is uniformly added in the ethyl alcohol of 10 times of volumes, under protection of argon gas high temperature reflux by essence, natrium carbonicum calcinatum afterwards
10~12h is reacted, after solution cooling, the solid of washing reaction precipitation；
By solid and iron powder according to mass ratio it is 1 after drying：0.1~0.5 adds in reaction vessel, adds by distilled water, acetone
Under the protection of argon gas, after being heated with stirring to reflux temperature, dilute hydrochloric acid is slowly added to for the mixed solvent of composition, adjusts pH value
To 3~4, after the reaction was continued 6~7h, stop heating, then add in hydrazine hydrate to adjust pH value to 8~9, stir evenly, will produce
Object filters while hot, is recrystallized with ethanol water, after vacuum drying, synthesizes diamines, for use；
Step 2, synthesis of polyimides：It is 1 according to molar ratio：2：8~10 weigh diamines, the benzophenone tetrabasic carboxylic acid two that step 1 synthesizes
Acid anhydride, solvent are added in after weighing in reaction kettle, and under protection of argon gas, agitating and heating carries out back flow reaction, and the mixing after reaction is molten
Liquid submerged in the water by the powder of precipitation, obtains polyimides, for use after washing, drying；
Step 3, stromatolysis：According to parts by weight weigh 50~120 parts step 2 prepare polyimides, 100~200 parts
Epoxy resin, 30~80 parts activation dispersant, 15~150 parts of conductive filler, 5~15 parts of toughener, 10~20 parts
Curing agent, 10~20 parts of accelerating agent, by load weighted polyimides, epoxy resin, activation dispersant argon gas protection
Under, it stirs evenly, for use；
The mixing of step 4, additive：The load weighted conductive filler of step 3, toughener, accelerating agent are added in into high speed dispersor height
After fast grinding distribution, for use；
The preparation of step 5, conductive adhesive：Additive package that dissolved matrix, step 4 that step 3 obtains are obtained and
The load weighted curing agent of step 3 is added in high energy shear stirred autoclave, and after stirring evenly, vacuum vibration deaeration after taking-up obtains
To the conductive adhesive.
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| CN117645853A (en) * | 2023-11-17 | 2024-03-05 | 朗峰新材料(菏泽)有限公司 | Adhesive for nanocrystalline magnetic core and preparation method thereof |
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Application publication date: 20180629 |