CN106497448B - A kind of preparation method of fast Curing conductive adhesive - Google Patents
A kind of preparation method of fast Curing conductive adhesive Download PDFInfo
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- CN106497448B CN106497448B CN201610935828.5A CN201610935828A CN106497448B CN 106497448 B CN106497448 B CN 106497448B CN 201610935828 A CN201610935828 A CN 201610935828A CN 106497448 B CN106497448 B CN 106497448B
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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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
A kind of preparation method of fast Curing conductive adhesive, mass parts composition includes: 80~100 parts of bisphenol A type epoxy resin, 75~80 parts of flake silver powder, 5~40 parts of amine-adduct type latent curing agent, 10~40 parts of toughener, 5~40 parts of diluent.Preparation process is first to be heat-treated toughener 1 hour through 80 DEG C, then 30min is stirred with 400rpm speed through room temperature with bisphenol A type epoxy resin, after being subsequently added into diluent stirring 30min, amine-adduct type latent curing agent is added and stirs 30min, silver powder is added and stirs 1~3 hour；1200rpm speed deaeration 3min is pressed with centrifugal blender, obtains fast Curing conductive adhesive, the paste conduction adhesiveness of preparation is 10Pas (25 DEG C), storage period: 0~5 DEG C/1 year, room temperature/March, 30~35 DEG C/January.Cured article performance is volume resistivity (1~5) × 104Ω m, 10~14MPa of tensile shear strength.
Description
One, technical field
The present invention relates to a kind of preparation methods of fast Curing conductive adhesive, more particularly to a kind of bisphenol type epoxy tree
The preparation method of the quick-setting conducting resinl of rouge.
Two, background technique
It is many that conducting resinl is used for large-scale integrated circuit, wave detector, sensor, light-sensitive element, electron camera and waveguide etc.
The conductive connection between of the same race or dissimilar material between electrical component and component, has obtained good result.
In conducting resinl, epoxide resin conductive adhesive is most widely used conducting resinl.Epoxy resin has multiple material
Good adhesive property, can obtain compared with high-adhesive-strength, single component epoxy conducting resinl is also most widely used conducting resinl.
Using silver powder as the epoxide resin conductive adhesive of conducting particles, good conductivity, Long-Term Properties are more stable, have good
Good moisture resistance, it is most important kind in epoxide resin conductive adhesive.
The product DAD-87 type epoxide resin conductive adhesive of SHANGHAI RESEARCH INSTITUTE OF SYNTHETIC RESINS is a kind of single group containing solvent
Part paste, the electric conductivity having had, thermal conductivity and heat resistance, easy to use, impurity content is few.It can make at 40 DEG C~175 DEG C
With.It is short-term heat-resisting up to 350 DEG C, it can be used for the integrated circuit of Plastic Package, the load of middle low power transistor, diode lead
With the splicing of the electrical components such as PTC ceramics heater element.The condition of cure of the glue be 150 DEG C/4 hours, 175 DEG C/3 hours, 200
DEG C/2 hours, 250 DEG C/0.5~1 hour.Storage period is 0~5 DEG C/1 year, 20 DEG C/March, 30 DEG C~35 DEG C/January.
Recent user claims under conditions of original product epoxide resin conductive adhesive properties of product are constant, shortens solidification
The cure cycle of conducting resinl and time.So researching and developing fast cured epoxy resin conducting resinl has just put on agenda.
Three, summary of the invention
The present inventors have done specially to prepare properties of product similar to the rapid-curing conductive of epoxide resin conductive adhesive
Research with great concentration, has completed overall technical architecture, be prepared for it is a kind of can be in 130 DEG C/0.5hr, 175 DEG C/0.5hr is cured fast
Fast Curing conductive adhesive.Complete technical solution is:
The mass parts composition of a kind of preparation method of fast Curing conductive adhesive, the fast Curing conductive adhesive includes: bisphenol type epoxy
80~100 parts of resin, 75~80 parts of flake silver powder, 5~40 parts of amine-adduct type latent curing agent, 5~40 parts of diluent, increase
Tough dose 10~40 parts；The amine-adduct type latent curing agent is the adduct of imidazoles and epoxy resin；Preparation process is
Toughener is heat-treated 1 hour through 80 DEG C first, 30min is then stirred with 400rpm speed through room temperature with bisphenol A type epoxy resin,
After being subsequently added into diluent stirring 30min, amine-adduct type latent curing agent is added and stirs 30min, flake silver powder is added and stirs
It mixes 1~3 hour；1200rpm speed deaeration 3min is pressed with centrifugal blender, obtains fast Curing conductive adhesive, canned refrigeration makes for user
With；The condition of cure of this fast Curing conductive adhesive is 130 DEG C/0.5 hour, 175 DEG C/0.5 hour.
Heretofore described bisphenol A type epoxy resin is the E-51 low viscosity epoxy resin of Shanghai Resin Factory's production.
The partial size of heretofore described flake silver powder is 2~5 μm.
Heretofore described toughener is from dimer acid modified epoxy resin, Pioloform, polyvinyl acetal, polybutadiene epoxy
It chooses any one kind of them in resin.
Heretofore described diluent is from tertiary carbonic acid glycidyl ester, propylene oxide propylene ether, propylene oxide butyl
It chooses any one kind of them in ether.
The amine-adduct type latent curative is the adduct of imidazoles and epoxy resin, or with tertiary amino
The adduct of compound and epoxy resin.This kind of adduct is the strength curing accelerator of dicyandiamide, the present invention using imidazoles and
The adduct of epoxy resin, Typical Representative are Japanese Ajincomoto Co., Inc's product Ajicure PN-23.
The preparation process of this rapid-curing conductive is: first by toughener in 80 DEG C be heat-treated 1 hour, followed by with bis-phenol
A type epoxy resin stirs 30min in room temperature with 400rpm speed, and after being subsequently added into diluent stirring 30min, amine adduct is added
Type latent curing agent stirs 30min, and silver powder is added and stirs 1~3hr, presses 1200rpm speed deaeration 3min with centrifugal blender,
Fast Curing conductive adhesive is obtained, canned refrigeration is for users to use；The condition of cure of the glue be 130 DEG C/0.5hr, 175 DEG C/0.5hr.
The fast Curing conductive adhesive properties of product prepared according to technical solution of the present invention are as follows:
Viscosity (25 DEG C) 10Pas
Silver content >=75%
Volume resistivity (1~5) × 104Ω·m
10~14MPa of tensile shear strength
Storage period: 0~5 DEG C/1 year, room temperature/March, 30~35 DEG C/January
Amine-adduct type latent curing agent of the present invention is suitable for the curing agent of other epoxy resin, such as:
It can make the curing agent of acrylic acid epoxy resin, novolac epoxy resin and polyurethane modified epoxy resin.
Four, specific embodiment
For the better implementation present invention, special illustration, but embodiment is not limitation of the present invention.
Embodiment 1
The dimer acid modified epoxy resin of 30g toughener is heat-treated 1 hour in 80 DEG C, in room temperature and 100g bisphenol type epoxy
Resin is stirred 30min in 400rpm speed, is subsequently added into 40g diluent tertiary carbonic acid glycidyl ester and continues to stir 30min,
40g amine-adduct type latent curing agent Ajicure PN-23 is added, it is Ajincomoto Co., Inc's product, stirs 30min
Afterwards, it is that 2~5 μm of flake silver powders continue stirring 1~3 hour that 80g partial size, which is added, with centrifugal blender in 1200rpm speed deaeration
3min obtains fast Curing conductive adhesive, and canned refrigeration is for users to use；The condition of cure of this fast Curing conductive adhesive are as follows: 130 DEG C/0.5
Hour, 175 DEG C/0.5 hour.Viscosity (25 DEG C) 10Pas of paste conducting resinl, storage period: 0~5 DEG C/1 year, room temperature/March,
30~35 DEG C/January.The performance indicator of the cured article of fast Curing conductive adhesive are as follows: volume resistivity 1 × 104Ω m, stretching are cut
Shearing stress 12MPa.
Embodiment 2
Except the fast curing conductive glue formula of change are as follows: bisphenol A type epoxy resin 90g, partial size are 2~5 μm of flake silver powder 70g,
Adduct curing agent 25g with tertiary ammonia based compound and bisphenol A type epoxy resin, toughener Pioloform, polyvinyl acetal 40g, dilution
Outside agent propylene oxide propylene ether 30g, other operating process and the same manner as in Example 1, the cured article of fast Curing conductive adhesive of formula
Performance is volume resistivity 2 × 104Ω m, tensile shear strength 14MPa.
Embodiment 3
Except the fast curing conductive glue formula of change are as follows: bisphenol A type epoxy resin 80g, partial size are 2~5 μm of flake silver powder 60g,
40g amine-adduct type latent curing agent Ajicure PN-23, toughener polybutadiene epoxy resin 5g, diluent epoxy third
Outside alkane butyl ether 5g, other operating process and it is formulated the same manner as in Example 1, the cured article performance of fast Curing conductive adhesive is 5 ×
104Ω m, tensile shear strength 13MPa.
Embodiment 4
Except the fast curing conductive glue formula of change are as follows: bisphenol A type epoxy resin 90g, partial size are 2~5 μm of flake silver powder 70g,
25g amine-adduct type latent curing agent Ajicure PN-23, toughener Pioloform, polyvinyl acetal 40g, diluent propylene oxide fourth
Outside base ether 30g, other operating process and formula are the same manner as in Example 1, and the cured article performance of fast Curing conductive adhesive is 3 × 104
Ω m, tensile shear strength 14MPa.
Claims (3)
1. a kind of preparation method of fast Curing conductive adhesive, which is characterized in that by the dimer acid modified epoxy resin of 30g toughener in 80
DEG C heat treatment 1 hour, be stirred 30min in 400rpm speed in room temperature and 100gE-51 bisphenol A type epoxy resin, then plus
Enter 40g diluent tertiary carbonic acid glycidyl ester to continue to stir 30min, 40g amine-adduct type latent curing agent Ajicure is added
PN-23, it is Ajincomoto Co., Inc's product, and after stirring 30min, it is that 2~5 μm of flake silver powders continue stirring 1 that 80g partial size, which is added,
~3 hours, with centrifugal blender in 1200rpm speed deaeration 3min, fast Curing conductive adhesive is obtained, canned refrigeration is for users to use；
The condition of cure of this fast Curing conductive adhesive are as follows: 130 DEG C/0.5 hour, 175 DEG C/0.5 hour；At 25 DEG C, paste conducting resinl
Viscosity 10Pas, storage period: 0~5 DEG C/1 year, room temperature/March, 30~35 DEG C/January；The cured article of fast Curing conductive adhesive
Performance indicator are as follows: volume resistivity 1 × 104Ω m, tensile shear strength 12MPa.
2. a kind of preparation method of fast Curing conductive adhesive, which is characterized in that by 5g toughener polybutadiene epoxy resin in 80 DEG C
Heat treatment 1 hour is stirred 30min in 400rpm speed in room temperature and 80g E-51 bisphenol A type epoxy resin, is subsequently added into
Diluent epoxy propane butyl ether 5g continues to stir 30min, 40g amine-adduct type latent curing agent Ajicure PN- is added
23, it is Ajincomoto Co., Inc's product, and after stirring 30min, it is that 2~5 μm of flake silver powders continue stirring 1~3 that 60g partial size, which is added,
Hour, with centrifugal blender in 1200rpm speed deaeration 3min, fast Curing conductive adhesive is obtained, canned refrigeration is for users to use；It is this
The condition of cure of fast Curing conductive adhesive are as follows: 130 DEG C/0.5 hour, 175 DEG C/0.5 hour；At 25 DEG C, the viscosity of paste conducting resinl
10Pas, storage period: 0~5 DEG C/1 year, room temperature/March, 30~35 DEG C/January；The performance of the cured article of fast Curing conductive adhesive
Index are as follows: volume resistivity 5 × 104Ω m, tensile shear strength 13MPa.
3. a kind of preparation method of fast Curing conductive adhesive, which is characterized in that by 40g toughener Pioloform, polyvinyl acetal at 80 DEG C of heat
Reason 1 hour is stirred 30min in 400rpm speed in room temperature and 90g E-51 bisphenol A type epoxy resin, is subsequently added into dilution
Agent epoxy propane butyl ether 30g continues to stir 30min, 25g amine-adduct type latent curing agent Ajicure PN-23 is added,
It is Ajincomoto Co., Inc's product, and after stirring 30min, it is that continue stirring 1~3 small for 2~5 μm of flake silver powders that 70g partial size, which is added,
When, with centrifugal blender in 1200rpm speed deaeration 3min, fast Curing conductive adhesive is obtained, canned refrigeration is for users to use；It is this fast
The condition of cure of Curing conductive adhesive are as follows: 130 DEG C/0.5 hour, 175 DEG C/0.5 hour；At 25 DEG C, the viscosity of paste conducting resinl
10Pas, storage period: 0~5 DEG C/1 year, room temperature/March, 30~35 DEG C/January；The performance of the cured article of fast Curing conductive adhesive
Index are as follows: volume resistivity 3 × 104Ω m, tensile shear strength 14MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610935828.5A CN106497448B (en) | 2016-11-01 | 2016-11-01 | A kind of preparation method of fast Curing conductive adhesive |
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| CN201610935828.5A CN106497448B (en) | 2016-11-01 | 2016-11-01 | A kind of preparation method of fast Curing conductive adhesive |
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| CN106497448B true CN106497448B (en) | 2019-09-24 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580685A (en) * | 2009-06-05 | 2009-11-18 | 烟台德邦科技有限公司 | High-reliability fast curing underfill adhesive and preparation method thereof |
| CN101935510A (en) * | 2010-09-21 | 2011-01-05 | 长春永固科技有限公司 | Epoxy resin conductive silver colloid with high adhesive strength |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629643B (en) * | 2015-03-06 | 2017-11-28 | 廊坊市高瓷电子技术有限公司 | Conducting resinl, its preparation method and wiring board |
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- 2016-11-01 CN CN201610935828.5A patent/CN106497448B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580685A (en) * | 2009-06-05 | 2009-11-18 | 烟台德邦科技有限公司 | High-reliability fast curing underfill adhesive and preparation method thereof |
| CN101935510A (en) * | 2010-09-21 | 2011-01-05 | 长春永固科技有限公司 | Epoxy resin conductive silver colloid with high adhesive strength |
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Effective date of registration: 20170313 Address after: 201702 Shanghai City, Qingpu West Road, No. 1251 Applicant after: SHANGHAI RESEARCH INSTITUTE OF SYNTHETIC RESINS CO., LTD. Address before: 201702 Shanghai City, Qingpu West Road, No. 1251 Applicant before: Co., Ltd of Shanghai Plastic Inst. |
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Effective date of registration: 20210219 Address after: No. 1251, Zhulu West Road, Xujing Town, Qingpu District, Shanghai, 201702 Patentee after: SHANGHAI PLASTICS RESEARCH INSTITUTE Co.,Ltd. Address before: No. 1251, Zhulu West Road, Qingpu District, Shanghai, 201702 Patentee before: SHANGHAI RESEARCH INSTITUTE OF SYNTHETIC RESINS Co.,Ltd. |