CN115322714A - Glue for copper bush glue dispensing - Google Patents
Glue for copper bush glue dispensing Download PDFInfo
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- CN115322714A CN115322714A CN202210891986.0A CN202210891986A CN115322714A CN 115322714 A CN115322714 A CN 115322714A CN 202210891986 A CN202210891986 A CN 202210891986A CN 115322714 A CN115322714 A CN 115322714A
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- glue
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- epoxy resin
- weight
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- Pending
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- 239000003292 glue Substances 0.000 title claims abstract description 78
- 241000227287 Elliottia pyroliflora Species 0.000 title claims abstract description 14
- 239000003822 epoxy resin Substances 0.000 claims abstract description 57
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 57
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000012745 toughening agent Substances 0.000 claims abstract description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- 239000003085 diluting agent Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 33
- 239000004952 Polyamide Substances 0.000 claims description 19
- 229920002647 polyamide Polymers 0.000 claims description 19
- 229920001971 elastomer Polymers 0.000 claims description 14
- 239000005060 rubber Substances 0.000 claims description 14
- 239000005077 polysulfide Substances 0.000 claims description 13
- 229920001021 polysulfide Polymers 0.000 claims description 13
- 150000008117 polysulfides Polymers 0.000 claims description 13
- 229920000459 Nitrile rubber Polymers 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- VMSIYTPWZLSMOH-UHFFFAOYSA-N 2-(dodecoxymethyl)oxirane Chemical compound CCCCCCCCCCCCOCC1CO1 VMSIYTPWZLSMOH-UHFFFAOYSA-N 0.000 claims description 7
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 7
- 229920001451 polypropylene glycol Polymers 0.000 claims description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910021487 silica fume Inorganic materials 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 23
- 229910052802 copper Inorganic materials 0.000 abstract description 23
- 239000010949 copper Substances 0.000 abstract description 23
- 229910052751 metal Inorganic materials 0.000 abstract description 18
- 239000002184 metal Substances 0.000 abstract description 18
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 13
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 238000009736 wetting Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 230000001070 adhesive effect Effects 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 glycidyl ether compound Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- 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
- C08G59/44—Amides
-
- 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
-
- 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
- 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
- C08G2170/00—Compositions for adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to glue for copper bush glue dispensing, which comprises the following components in parts by weight: 100-120 parts of epoxy resin, 10-20 parts of curing agent, 7-10 parts of toughening agent, 0.5-1 part of silane coupling agent, 30-40 parts of filler and 10-15 parts of diluent. The invention optimizes and designs the combination of the epoxy resin, the curing agent and the toughening agent in the glue, adds the additive on the basis to improve the bonding performance of the glue to the copper sleeve and the metal alloy, and improves the bonding performance and the durability of the glue to the metal by adding the silane coupling agent; the bonding strength of the glue is improved by adding the filler; the wetting property and the toughness of the glue are improved by adding the diluent, so that the bonding strength of the glue to metal is improved.
Description
Technical Field
The invention relates to the field of metal glue, in particular to glue for copper bush glue.
Background
The small metal alloy fittings and the copper bush are small in size, so that the copper bush is generally fixed on the small metal alloy fittings in a glue bonding mode, specifically, glue dispensing operation is performed on the copper bush, and then the glued copper bush is attached and bonded with the small metal alloy fittings.
Most metal alloys are subjected to surface treatment, such as electroplating or chemical plating, a plating layer is generally zinc, nickel and chromium, the stability of inert metal molecules such as zinc, nickel and chromium is relatively high, meanwhile, copper belongs to a material which is difficult to bond, the bonding of a copper sleeve and a metal alloy accessory is difficult to realize by using general metal glue, the bonding force between the copper sleeve and the metal alloy accessory is poor by using the existing metal glue, and the copper sleeve is easy to fall off from the metal alloy accessory.
Disclosure of Invention
Aiming at the technical problems in the prior art and aiming at solving the problems that the existing metal adhesive is weak in bonding strength and easy to fall off after being bonded with a metal alloy accessory after copper bush dispensing, the invention provides glue for copper bush dispensing, which comprises the following components in parts by weight: 100-120 parts of epoxy resin, 10-20 parts of curing agent, 7-10 parts of toughening agent, 0.5-1 part of silane coupling agent, 30-40 parts of filler and 10-15 parts of diluent.
The metal glue at present generally comprises three types of epoxy resin glue, polyurethane glue and acrylate glue, wherein in the three types of metal glue, the epoxy resin has the advantages of high bonding strength, small shrinkage rate, capability of being applied to harsh environments, low modification difficulty and the like, so the main components of the epoxy resin glue with better comprehensive performance are epoxy resin, a curing agent and a toughening agent, the main components of the epoxy resin glue are improved and optimized, and a silane coupling agent, a filler and a diluent are added on the basis to enhance the bonding performance of the epoxy resin adhesive to the copper bush and the metal alloy.
Further, the epoxy resin comprises one or more of E-44 epoxy resin, E-51 epoxy resin, D-17 epoxy resin and AG-80 (4, 4' -diaminodiphenylmethane epoxy resin).
The epoxy resin is screened, and has the advantages of strong adhesion to metal and high bonding strength.
Further, the curing agent includes a low molecular polyamide.
The curing agent is used for carrying out chemical reaction with the epoxy resin, and can enable linear molecules to form a net-shaped or body-shaped structure, so that the epoxy resin is cured. The low molecular polyamide has better compatibility with the epoxy resin, can be used for curing the epoxy resin at lower temperature, can be used as a curing agent or a toughening agent in an epoxy resin system, and is a multifunctional agent. The inventors have experimentally confirmed that the low molecular polyamide is selected from the group consisting of low molecular polyamide 200 and low molecular polyamide 300.
Further, the toughening agent comprises any one of polysulfide rubber and liquid carboxyl-terminated nitrile rubber.
The toughening agent is used for reacting with active groups in the epoxy resin, and can reduce the curing shrinkage rate of the epoxy resin, and improve the shear strength, the peel strength and the flexibility. Polysulfide rubber is a common epoxy resin toughening agent, after the polysulfide rubber is mixed with epoxy resin, thiol groups and epoxy groups in the polysulfide rubber react to endow the epoxy resin with good flexibility, and preferably, the relative molecular mass of the polysulfide rubber is 1000-4000; liquid carboxyl terminated nitrile butadiene rubber (CTBN) is also a commonly used epoxy toughener, preferably, CTBN has a relative molecular weight of 3500-4000.
Further, the silane coupling agent is any one of KH-560, KH-550, KH-580 and KH-590.
The silane coupling agent is a multifunctional agent, can be used as a tackifier in epoxy resin to improve the adhesive property and the durability of the epoxy resin to metal, and can improve the dispersion property and the wettability of filler in the epoxy resin.
Further, the filler comprises one or more of silicon carbide whiskers, silicon micropowder, micron carbon fibers and alumina powder (300-400 meshes).
The filler can reduce the expansion coefficient and the curing shrinkage of a cured product and reduce internal stress. When the epoxy resin cracks under the overload action, the filler can prevent the cracks from expanding, so that the bonding strength of the epoxy resin is improved.
Further, the diluent is any one of polypropylene glycol diglycidyl ether, phenyl glycidyl ether, and dodecyl glycidyl ether.
The thinner can improve the wettability and toughness of the epoxy resin and is beneficial to improving the bonding strength of the epoxy resin to metal. The invention selects the glycidyl ether compound with an epoxy structure as the diluent which participates in the curing reaction of the epoxy resin, so that not only can the viscosity of a curing system be reduced, but also the cured epoxy resin has good flexibility, impact resistance and thermal shock resistance.
Further, the preparation method of the glue comprises the following steps:
s1, adding the epoxy resin, the toughening agent, the diluent and the silane coupling agent into a reaction kettle, and stirring for 1h at the temperature of 70-90 ℃;
s2, adding the filler into the reaction kettle when the temperature is reduced to 25-30 ℃, and stirring for 50min;
and S3, adding the curing agent into the reaction kettle at the temperature of 60 ℃, and stirring for 2 hours.
Compared with the prior art, the technical scheme of the invention has at least the following beneficial effects:
1. the epoxy resin with better comprehensive performance is selected as the main component of the glue for dispensing the copper bush, the epoxy resin glue is called as a universal glue and can be applied to the bonding between metals and nonmetal, and the glue provided by the invention has the possibility of being applied to other fields, namely the glue provided by the invention expands the varieties of the epoxy resin glue;
2. the combination of the epoxy resin, the curing agent and the toughening agent in the glue is optimized and designed, the epoxy resin with strong metal adsorption capacity and high performance is selected to match with the low-molecular polyamide with good compatibility and toughening and curing effects, and the polysulfide rubber or the liquid carboxyl-terminated butadiene-acrylonitrile rubber is matched on the basis to improve the flexibility of the glue, so that the glue is ensured to have certain bonding performance on the copper bush and the metal alloy;
3. the additive is added on the basis of the epoxy resin glue to improve the bonding performance of the glue to the copper sleeve and the metal alloy, and the bonding performance and the durability of the glue to the metal are improved by adding the silane coupling agent; the bonding strength of the glue is improved by adding the filler; the wetting property and the toughness of the glue are improved by adding the diluent, so that the bonding strength of the glue to metal is improved.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
Weighing 100 parts by weight of E-44 epoxy resin, 7 parts by weight of polysulfide rubber, 10 parts by weight of polypropylene glycol diglycidyl ether and 0.5 part by weight of KH-560, adding into a reaction kettle, heating and stirring at 70 ℃ for 1 hour, reducing the temperature by 25 ℃, adding 30 parts by weight of silicon carbide whiskers into the reaction kettle, stirring for 50min, raising the temperature to 60 ℃, adding 10 parts by weight of low molecular polyamide 200 into the reaction kettle, and stirring for 2 hours to obtain the glue for copper sheath glue dispensing.
Example 2
Weighing 100 parts of E-51 epoxy resin, 7 parts of liquid terminal carboxyl nitrile rubber, 10 parts of phenyl glycidyl ether and 0.5 part of KH-550 in parts by weight, adding into a reaction kettle, heating and stirring at 80 ℃ for 1h, reducing the temperature by 25 ℃, adding 30 parts of silicon micropowder into the reaction kettle, stirring for 50min, raising the temperature to 60 ℃, adding 10 parts of low molecular polyamide 300 into the reaction kettle, and stirring for 2h to obtain the glue for copper sheath glue dispensing.
Example 3
Weighing 100 parts by weight of D-71 epoxy resin, 7 parts by weight of polysulfide rubber, 10 parts by weight of dodecyl glycidyl ether and 0.5 part by weight of KH-580, adding into a reaction kettle, heating and stirring at 70 ℃ for 1 hour, reducing the temperature by 25 ℃, adding 30 parts by weight of micron carbon fiber into the reaction kettle, stirring for 50min, increasing the temperature to 60 ℃, adding 10 parts by weight of low-molecular polyamide 200 into the reaction kettle, and stirring for 2 hours to obtain the glue for copper sheath glue dispensing.
Example 4
Weighing 100 parts by weight of AG-80, 7 parts by weight of liquid terminal carboxyl nitrile rubber, 10 parts by weight of dodecyl glycidyl ether and 0.5 part by weight of KH-590, adding into a reaction kettle, heating and stirring at 90 ℃ for 1 hour, reducing the temperature by 30 ℃, adding 30 parts by weight of alumina powder into the reaction kettle, stirring for 50min, raising the temperature to 60 ℃, adding 10 parts by weight of low molecular weight polyamide 300 into the reaction kettle, and stirring for 2 hours to obtain the glue for copper sheath glue dispensing.
Example 5
Weighing 90 parts by weight of E-44 epoxy resin, 20 parts by weight of D-71 epoxy resin, 8 parts by weight of polysulfide rubber, 13 parts by weight of dodecyl glycidyl ether and 0.8 part by weight of KH-560, adding the mixture into a reaction kettle, heating and stirring the mixture at 70 ℃ for 1 hour, reducing the temperature by 25 ℃, adding 33 parts by weight of silicon carbide whiskers into the reaction kettle, stirring the mixture for 50 minutes, heating the temperature to 60 ℃, adding 16 parts by weight of low-molecular polyamide 200 into the reaction kettle, and stirring the mixture for 2 hours to obtain the glue for copper sheath glue dispensing.
Example 6
Weighing 90 parts by weight of E-51 epoxy resin, 20 parts by weight of D-71 epoxy resin, 8 parts by weight of polysulfide rubber, 13 parts by weight of dodecyl glycidyl ether and 0.8 part by weight of KH-580, adding the mixture into a reaction kettle, heating and stirring the mixture at 80 ℃ for 1 hour, reducing the temperature by 25 ℃, adding 22 parts by weight of silicon micropowder and 11 parts by weight of micron carbon fiber into the reaction kettle, stirring the mixture for 50 minutes, increasing the temperature to 60 ℃, adding 16 parts by weight of low molecular weight polyamide 300 into the reaction kettle, and stirring the mixture for 2 hours to obtain the glue for copper sheath glue dispensing.
Example 7
Weighing 90 parts by weight of E-44 epoxy resin, 20 parts by weight of AG-80, 8 parts by weight of liquid terminal carboxyl nitrile rubber, 13 parts by weight of polypropylene glycol diglycidyl ether and 0.8 part by weight of KH-560, adding into a reaction kettle, heating and stirring at 90 ℃ for 1h, reducing the temperature to 30 ℃, adding 33 parts by weight of silicon carbide whiskers into the reaction kettle, stirring for 50min, heating to 60 ℃, adding 16 parts by weight of low molecular weight polyamide 200 into the reaction kettle, and stirring for 2h to obtain the glue for copper sheath glue dispensing.
Example 8
Weighing 70 parts of E-51 epoxy resin, 50 parts of E-44 epoxy resin, 10 parts of liquid terminal carboxyl nitrile rubber, 15 parts of polypropylene glycol diglycidyl ether and 1 part of KH-560 according to parts by weight, adding into a reaction kettle, heating and stirring for 1h at 80 ℃, reducing the temperature by 25 ℃, adding 30 parts of silicon micropowder and 10 parts of micron carbon fiber into the reaction kettle, stirring for 50min, raising the temperature to 60 ℃, adding 20 parts of low molecular weight polyamide 300 into the reaction kettle, and stirring for 2h to obtain the glue for copper sheath glue dispensing.
Example 9
Weighing 80 parts by weight of AG-80, 40 parts by weight of D-71 epoxy resin, 10 parts by weight of polysulfide rubber, 15 parts by weight of dodecyl glycidyl ether and 1 part by weight of KH-590, adding the mixture into a reaction kettle, heating and stirring the mixture at 90 ℃ for 1 hour, reducing the temperature by 30 ℃, adding 40 parts by weight of silicon carbide whiskers into the reaction kettle, stirring the mixture for 50 minutes, heating the temperature to 60 ℃, adding 20 parts by weight of low molecular polyamide 300 into the reaction kettle, and stirring the mixture for 2 hours to obtain the glue for copper sheath glue dispensing.
Comparative example 1
Comparative example 1 differs from example 8 in that no KH-560 was added and the other steps and parameters were in accordance with example 8.
Comparative example 2
Comparative example 2 differs from example 8 in that no polypropylene glycol diglycidyl ether is added and other steps and parameters remain the same as in example 8.
Comparative example 3
Comparative example 3 is a commercially available KH-508 epoxy adhesive. The KH-508 component contains E-44 epoxy resin, anhydride, titanium dioxide and glass powder.
The glue for copper sheath dispensing obtained in the above examples 1 to 9 and comparative examples 1 to 3 is coated on a copper bar and bonded with a metal alloy bar (aluminum alloy bar) to perform a shear strength test, the higher the shear strength is, the higher the adhesive strength of the glue is, wherein before the copper bar and the aluminum alloy bar are coated and bonded, the copper bar and the aluminum alloy bar need to be subjected to surface treatment, which sequentially comprises degreasing in a sodium hydroxide solution, activating in a dilute hydrochloric acid solution, corroding in a nitric acid corrosive solution until fine and rough pores are formed on the metal surface, and soaking and cleaning in deionized water.
The specific test operation of the shear strength test is as follows: and clamping the sample to be tested in an upper clamp and a lower clamp of a tensile testing machine, starting the sample testing machine to enable the clamp to load the sample to be tested at the speed of 5mm/min until the bonding layer of the copper strip and the aluminum alloy strip is completely damaged, and recording the shearing strength of the sample.
The test sample to be tested comprises the test sample to be tested before high-temperature aging, after high-temperature aging and after a neutral salt spray test for 72 hours, wherein the test sample to be tested before high-temperature aging refers to the test sample to be tested after a copper strip is attached to an aluminum alloy strip, the copper strip and the aluminum alloy strip are pressed for 15s by using 3kgf/cm to complete adhesion, and the test sample to be tested is kept stand for 3 hours; the sample to be tested after high-temperature aging is the sample to be tested which is baked for 3 hours at the temperature of 130 ℃ after standing; the sample to be tested after the 72-hour neutral salt spray test is the sample to be tested which is placed in a salt spray test box with 5% saline at 35 ℃ for 72 hours after the completion of standing.
The results of the above tests are shown in Table 1.
TABLE 1 test results of examples 1-9 and comparative examples 1-3
As can be seen from the test structures in table 1, the shear strength of the glue obtained in examples 1 to 9 before and after high-temperature aging and under the condition of a neutral salt spray test for 72 hours is better than that of comparative example 3, and it can be seen that the glue for copper sheathing glue provided by the invention has higher shear strength (bonding strength) compared with the existing metal glue, wherein the glue obtained in example 8 has the best bonding performance, the shear strength before high-temperature aging is 21.8MPa, the shear strength after high-temperature aging is 26.9MPa, and the shear strength after the neutral salt spray test for 72 hours is 25.8MPa. Compared with the example 8, the adhesive prepared by the comparative example 1 lacks the silane coupling agent KH-560, compared with the example 8, the adhesive prepared by the comparative example 2 lacks the diluent polypropylene glycol diglycidyl ether, the shear strength of the adhesive prepared by the comparative example 1 and the adhesive prepared by the comparative example 2 are reduced under the three test conditions, and the silane coupling agent and the diluent are beneficial to improving the bonding strength of the epoxy resin adhesive.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The glue for copper bush dispensing is characterized by comprising the following components in parts by weight: 100-120 parts of epoxy resin, 10-20 parts of curing agent, 7-10 parts of toughening agent, 0.5-1 part of silane coupling agent, 30-40 parts of filler and 10-15 parts of diluent.
2. The glue of claim 1, wherein the epoxy resin comprises one or more of E-44 epoxy, E-51 epoxy, D-17 epoxy, AG-80.
3. The glue of claim 1, wherein the curing agent comprises a low molecular weight polyamide.
4. The glue of claim 3, wherein the low molecular polyamide is any one of low molecular polyamide 200 and low molecular polyamide 300.
5. The glue of claim 1, wherein the toughening agent comprises any one of polysulfide rubber and liquid carboxyl-terminated nitrile rubber.
6. The glue of claim 5, wherein the polysulfide rubber has a relative molecular mass of 1000-4000, and the liquid carboxyl-terminated nitrile rubber has a relative molecular mass of 3500-4000.
7. The glue of claim 1, wherein the silane coupling agent is any one of KH-560, KH-550, KH-580 and KH-590.
8. The glue of claim 1, wherein the filler comprises one or more of silicon carbide whiskers, micro-silica powder, micro-carbon fibers and alumina powder.
9. The glue of claim 1, wherein the diluent is any one of polypropylene glycol diglycidyl ether, phenyl glycidyl ether and dodecyl glycidyl ether.
10. The glue of claim 1, wherein the preparation method of the glue comprises the following steps:
s1, adding the epoxy resin, the toughening agent, the diluent and the silane coupling agent into a reaction kettle, and stirring for 1h at the temperature of 70-90 ℃;
s2, when the temperature is reduced to 25-30 ℃, adding the filler into the reaction kettle, and stirring for 50min;
and S3, adding the curing agent into the reaction kettle at the temperature of 60 ℃, and stirring for 2 hours.
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Citations (3)
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CN103146334A (en) * | 2013-03-29 | 2013-06-12 | 黑龙江省科学院石油化学研究院 | Flame-retardant intermediate-temperature cured epoxy film and preparation method thereof |
CN109181607A (en) * | 2018-11-23 | 2019-01-11 | 深圳市欧科力科技有限公司 | A kind of construction material epoxy adhesive and preparation method thereof |
CN114292612A (en) * | 2022-01-07 | 2022-04-08 | 北京高盟新材料股份有限公司 | Single-component epoxy flexible adhesive and preparation method thereof |
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- 2022-07-27 CN CN202210891986.0A patent/CN115322714A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103146334A (en) * | 2013-03-29 | 2013-06-12 | 黑龙江省科学院石油化学研究院 | Flame-retardant intermediate-temperature cured epoxy film and preparation method thereof |
CN109181607A (en) * | 2018-11-23 | 2019-01-11 | 深圳市欧科力科技有限公司 | A kind of construction material epoxy adhesive and preparation method thereof |
CN114292612A (en) * | 2022-01-07 | 2022-04-08 | 北京高盟新材料股份有限公司 | Single-component epoxy flexible adhesive and preparation method thereof |
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