CN111334233A - Adhesive for conductive cloth adhesive tape, preparation method and application thereof - Google Patents
Adhesive for conductive cloth adhesive tape, preparation method and application thereof Download PDFInfo
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- CN111334233A CN111334233A CN202010377141.0A CN202010377141A CN111334233A CN 111334233 A CN111334233 A CN 111334233A CN 202010377141 A CN202010377141 A CN 202010377141A CN 111334233 A CN111334233 A CN 111334233A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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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
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
Abstract
The invention discloses an adhesive for a conductive cloth adhesive tape, a preparation method and application thereof. The adhesive is prepared from the following raw materials in parts by weight: epoxy resin: 25-33 parts of silicone resin: 12-15 parts of flake silver powder: 78-106 parts of white carbon black: 3-5 parts of curing agent: 25-31 parts of accelerator: 17-25 parts of microcrystalline wax: 8-14 parts of pine tar: 3.6-6 parts of sorbitol: 2-7 parts; the preparation method comprises the following steps: (1) mixing epoxy resin, organic silicon resin and a curing agent to prepare a resin matrix with uniform components; (2) dissolving white carbon black and flake silver powder in the resin matrix prepared in the step (1), stirring for 1-2h, and ultrasonically dispersing for 2-4h to obtain a mixture of the resin matrix and the conductive filler; (3) adding the mixture obtained in the step (2) into microcrystalline wax, stirring for 20-45min at the temperature of 100-145 ℃, adding pine tar and sorbitol, and uniformly mixing to obtain the product; has the advantages of excellent thermal stability, moderate flexibility and bonding strength; the adhesive for the conductive cloth adhesive tape can be used for the conductive cloth adhesive tape.
Description
Technical Field
The invention relates to the field of adhesives and application, in particular to an adhesive for a conductive cloth adhesive tape, a preparation method and application thereof.
Background
The adhesive for the conductive cloth adhesive tape is an adhesive with certain conductive performance after being cured or dried, and generally takes a resin matrix and conductive filler, namely conductive particles as main components, and the conductive particles are combined together through the bonding action of the resin matrix to form a conductive path so as to realize the conductive connection of the bonded materials; the conductive cloth adhesive tape is an adhesive tape made of conductive cloth, and has the characteristic that the adhesive property is added on the basis of the conductive cloth, so that the magnetic shielding effect is achieved, and the conductive cloth adhesive tape is widely applied to various electronic machine parts and used for forming conductor wiring. The resin matrix of the adhesive for the conductive cloth adhesive tape is an adhesive, so that the conductive cloth adhesive tape can be bonded by selecting an appropriate curing temperature.
In the adhesion of an integrated circuit chip to a substrate or a circuit module to a printed wiring board, an epoxy resin is required to be an ideal adhesive base material and one of the most widely used adhesive base materials so far, because the conductive adhesive is required to have not only good conductivity but also very high adhesion strength.
Chinese patent CN1238459C describes a thermosetting conductive adhesive with high bonding strength, which is prepared by taking glycidyl ester epoxy resin as a matrix, micron-sized flaky silver powder as a conductive filler, diamine as a curing agent, a silane coupling agent (3-glycidyl ether oxypropyl trimethoxy silane) as a dispersing agent and nano-sized silicon dioxide as a toughening agent, and compared with an adhesive without silicon dioxide, the bonding strength of the thermosetting conductive adhesive is increased by 30-50%.
The adhesive has high bonding strength at normal temperature, but the cured colloid is hard and has poor flexibility.
Disclosure of Invention
The first purpose of the invention is to provide an adhesive for conductive cloth adhesive tape, which has the advantages of moderate flexibility and bonding strength.
The second purpose of the invention is to provide a preparation method of the adhesive for the conductive cloth adhesive tape.
A third object of the present invention is to provide a conductive cloth tape coated with the adhesive of the present invention.
The fourth object of the present invention is to provide a method for preparing a conductive cloth tape coated with the adhesive of the present invention.
In order to achieve the first object, the invention provides the following technical scheme: the adhesive for the conductive cloth adhesive tape is prepared from the following raw materials in parts by weight:
epoxy resin: 25 to 33 portions of the components are mixed,
silicone resin: 12-15 parts of (by weight),
flake silver powder: 78 to 106 portions of the raw materials are mixed,
white carbon black: 3-5 parts of (A) a water-soluble polymer,
curing agent: 25 to 31 portions of the components are added,
accelerator (b): 17-25 parts of (a) a water-soluble polymer,
microcrystalline wax: 8-14 parts of (by weight),
pine tar: 3.6 to 6 portions of the raw materials,
sorbitol: 2-7 parts.
By adopting the technical scheme, the epoxy resin has large intermolecular attraction, large effective crosslinking density and high mechanical strength, but has larger brittleness, low peeling strength and poor heat resistance, the organic silicon resin has small intermolecular attraction, low effective crosslinking density, weaker mechanical strength and poor adhesion, the phenyl contained in the molecular structure of the organic silicon resin can improve the heat resistance and weather resistance of a resin matrix, the cured epoxy resin and the cured organic silicon resin have excellent mechanical property, electrical property, heat resistance and oxidation resistance under the action of an accelerator and a curing agent, the microcrystalline wax is miscible with the resin and has excellent adhesion, toughness, flexibility and tensile strength, the pine tar can increase the plasticity of the adhesive, the dispersing of a compounding agent in a sizing material is facilitated, the viscosity of the adhesive is increased, the processing into a required shape is facilitated, and the cold-resistant anti-scorching and slow-curing performance of the adhesive can be improved, the white carbon black has porosity and large specific surface area, can endow the adhesive with higher tensile strength, elongation, elasticity, heat resistance and tearing strength, the sorbitol has stable chemical property, is not easily oxidized by air, and has better thermal stability, the flaky silver powder refers to flaky powder with one-dimensional thickness less than 100 nm, the flaky silver powder has good conductivity, the shape of silver particles has close relation with the conductivity, the flaky silver powder is arranged in a flaky structure, the fluidity among particles is better, the contact surface between flaky silver powder particles is large because the contact is surface contact or line contact, so the resistance of the flaky silver powder is relatively lower, the conductivity is better, the specific surface area of the flaky silver powder is relatively larger, the specific surface energy is lower, the oxidation degree and the oxidation tendency of the flaky silver powder are lower, in addition, the flaky silver powder has wider deflection range and fracture and stretching resistance, and the reliability of electronic components is improved, the coating area of the flake silver powder is larger, so that the flake silver powder can save the using amount of the silver powder and reduce the thickness of a coating on the other hand, and is beneficial to the miniaturization of electronic components; the adhesive prepared by the scheme has the effects of excellent thermal stability, moderate flexibility and bonding strength.
The invention is further configured to: the epoxy resin comprises one or more of bisphenol a type epoxy resin and acrylic epoxy resin.
By adopting the technical scheme, the bisphenol A epoxy resin molecules contain hydroxyl, epoxy, methylene, ether bond and other groups, so that the bisphenol A epoxy resin has strong adhesive force to fabrics and other materials used by the conductive cloth, and has the advantages of high adhesive strength, small shrinkage, stable size, good electrical insulation, easiness in forming and thermal stability; acrylic epoxy resin: because the molecular structure contains methacrylate, the epoxy acrylate modified epoxy resin has the advantages of anaerobic property, long working life in air, small curing shrinkage, excellent chemical stability of a cured product, good hardness and adhesive force, good compatibility with other resins and strong weather resistance.
The invention is further configured to: the average relative molecular mass of the bisphenol A type epoxy resin is 300-700, the polymerization degree n is less than 2, and the softening point is lower than 50 ℃.
The invention is further configured to: the epoxy value mol/100g of the bisphenol A type epoxy resin is 0.5-0.54.
By adopting the technical scheme, the lower the epoxy value, the lower the dosage of the corresponding curing agent, the lower the crosslinking density of the cured product, the lower the brittleness and the higher the toughness, so the corresponding tensile shear strength is higher.
The invention is further configured to: the organic silicon resin is vinyl-terminated T-type phenyl polysiloxane.
By adopting the technical scheme, the molecular structure of the organic silicon resin contains phenyl to improve the heat resistance and weather resistance of the resin matrix, and the existence of the phenyl enables the adhesive to destroy the crystallinity of the high polymer in a certain temperature range, so that the high oxidation stability is realized; the arrangement of methyl groups in the molecule makes the adhesive hydrophobic, the water absorption of the adhesive is small, even if water is absorbed, the adhesive can be rapidly released and recovered to the original state, and the methyl groups make the adhesive have high thermal stability and good demoulding property.
The invention is further configured to: the vinyl content of the organic silicon resin is 1.8-2.2 mmol/g.
By adopting the technical scheme, the vinyl can improve the curing property of the resin and endow the resin with coupling property.
The invention is further configured to: the curing agent comprises a curing agent 1 and a curing agent 2, wherein the curing agent 1 comprises one or more of trimellitic anhydride and 2-ethyl-4-methylimidazole, and the curing agent 2 comprises one or more of ethyl orthosilicate and dibutyltin dilaurate.
By adopting the technical scheme, the trimellitic anhydride has high reaction activity, and the condensate has excellent mechanical property, electrical property and chemical resistance, and the 2-ethyl-4-methylimidazole can be cured at a lower temperature to obtain the condensate with excellent heat resistance and mechanical and physical properties, so that the condensate has thermal oxidation resistance, chemical resistance and acid resistance; ethyl orthosilicate and/or dibutyltin dilaurate are/is used as a curing agent of the organic silicon resin, so that a cured product has excellent mechanical properties.
The invention is further configured to: the curing agent is a mixture of 1.2-2.1 weight portions and 0.5-0.8 weight portions of 2 curing agent.
The invention is further configured to: the promoter is one or more of N, N-dimethylaniline and 2, 4, 6-tri (dimethylaminomethyl) phenol.
By adopting the technical scheme, the 2, 4, 6-tri (dimethylaminomethyl) phenol is liquid phenol with hydroxyl and tertiary amino, and the 2, 4, 6-tri (dimethylaminomethyl) phenol and/or N, N-dimethylaniline is used as an accelerator of the epoxy resin, so that the reaction time of the epoxy resin can be shortened, the curing temperature of the epoxy resin can be reduced, the using amount of a curing agent can be reduced, and the physical and mechanical properties of the adhesive are improved.
The invention is further configured to: the white carbon black is precipitated silica.
The invention is further configured to: the concentration of the sorbitol is more than 60%.
By adopting the technical scheme, the resistance of the sorbitol to microorganisms is stronger, the sorbitol is not easily polluted by the microorganisms with the concentration of more than 60 percent, and the weather resistance of the adhesive is further improved.
In order to achieve the second object, the invention provides the following technical scheme:
a preparation method of an adhesive for a conductive cloth adhesive tape comprises the following steps:
(1) mixing epoxy resin, organic silicon resin and a curing agent to prepare a resin matrix with uniform components;
(2) sequentially dissolving the white carbon black and the flake silver powder in the resin matrix prepared in the step (1), mechanically stirring for 1-2h, and ultrasonically dispersing for 2-4h to obtain a mixture of the resin matrix and the conductive filler;
(3) and (3) adding the mixture obtained in the step (2) into microcrystalline wax, stirring for 20-45min at the temperature of 100-145 ℃, then adding pine tar and sorbitol, and uniformly mixing to prepare the adhesive for the conductive cloth adhesive tape.
In order to achieve the third object, the invention provides the following technical solutions:
the conductive cloth adhesive tape comprises conductive cloth, the adhesive prepared by the method and tinned copper foil covering the adhesive, wherein the adhesive is coated on the conductive cloth.
In order to achieve the fourth object, the invention provides the following technical solutions:
the preparation method of the conductive cloth tape comprises the following steps:
s1, coating adhesive on the surface of the conductive cloth, wherein the coating speed is 7-10m/min, and the adhesive coating amount is 5-9g/m2；
S2, feeding the conductive cloth coated with the adhesive into an oven, heating and naturally cooling;
and S3, covering a layer of tinned copper foil on the dried adhesive to obtain the conductive cloth adhesive tape.
The invention is further configured to: the thickness of the adhesive layer on the surface of the conductive cloth is 20-25 μm.
In conclusion, the invention has the following beneficial effects:
firstly, as the epoxy resin and the organic silicon resin are compounded, the adhesiveness of the epoxy resin is strong and is complementary with the poorer adhesiveness of the organic silicon resin, and the microcrystalline wax, the pine tar, the white carbon black and the sorbitol are used for enhancing various performances of the resin matrix, so that the adhesive for the conductive cloth adhesive tape prepared by the invention obtains higher tensile strength, elongation, toughness and thermal stability, and the adhesive prepared by the scheme has moderate effects of excellent thermal stability, flexibility and adhesive strength.
Secondly, as the flake silver powder is adopted, the flake silver powder has larger specific surface area and contact surface, the usage amount of the flake silver powder is saved while the better conductivity is ensured, and the use cost of the invention is reduced.
Detailed Description
The present invention will be described in further detail with reference to examples.
Bisphenol A epoxy resin, manufactured by Shanghai resin factory Co., Ltd, with a product type of 618 and an epoxy value mol/100g of 0.5-0.54.
The acrylic epoxy resin is manufactured by Mitsubishi chemical company, and the model is BR-116.
The organic silicon resin is prepared from Jiaxing combined chemical company Limited, and has the following model: 5000 cs.
The flake silver powder is produced by Xuzhou Jie Chuang Innovation materials science and technology Co., Ltd, and has the specification type of B116 and the granularity of 4-8 microns.
The white carbon black is produced by a new dilute metallurgy chemical industry Co., Ltd, Guangzhou, and the mesh range is 400-1250.
The microcrystalline wax is produced by Jingmen Guangming chemical Co., Ltd, and has a mark number of 80.
The pine tar is produced by Dushui Kerui oil chemical trade company Limited.
Sorbitol is produced by Guangzhou Haosheng chemical industry Co., Ltd, and the content of effective substances is 70%.
Example 1
An adhesive for a conductive cloth adhesive tape is prepared from the following raw materials in parts by weight: epoxy resin: 28 parts, silicone resin: 14 parts of flake silver powder: 89 parts of white carbon black: 3.5 parts, curing agent: 25 parts, accelerator: 18 parts, microcrystalline wax: 10 parts of pine tar: 3.6 parts, sorbitol: 5 parts of the raw materials.
The epoxy resin comprises bisphenol A type epoxy resin and acrylic acid epoxy resin, wherein the average relative molecular mass of the bisphenol A type epoxy resin is 300-700, the polymerization degree n is less than 2, and the softening point is lower than 50 ℃. The organic silicon resin is vinyl-terminated T-type phenyl polysiloxane. The accelerator comprises N, N-dimethylaniline and 2, 4, 6-tris (dimethylaminomethyl) phenol.
The white carbon black is precipitated silica. The concentration of sorbitol is more than 60%.
The curing agent is a mixture consisting of a curing agent 1 for epoxy resin and a curing agent 2 for organic silicon resin in a weight ratio of 1.2:0.5, wherein the curing agent 1 comprises trimellitic anhydride and 2-ethyl-4-methylimidazole, and the curing agent 2 comprises ethyl orthosilicate and dibutyltin dilaurate.
A preparation method of an adhesive for a conductive cloth adhesive tape comprises the following steps:
(1) mixing epoxy resin, organic silicon resin and a curing agent to prepare a resin matrix with uniform components;
(2) sequentially dissolving the white carbon black and the flake silver powder into the resin matrix prepared in the step (1), mechanically stirring for 1.5 hours, and ultrasonically dispersing for 3 hours to obtain a mixture of the resin matrix and the conductive filler;
(3) and (3) adding the microcrystalline wax into the mixture obtained in the step (2), stirring for 20min at the temperature of 115 ℃, then adding pine tar and sorbitol, and uniformly mixing to prepare the adhesive for the conductive cloth adhesive tape.
Examples 2 to 6
The raw material amounts of the adhesives of examples 2 to 6 were different from those of the adhesive of example 1, and specifically, see table 1;
the adhesives of examples 2-6 are different from the adhesive of example 1 in the components of epoxy resin, accelerator, curing agent 1 and curing agent 2 in the raw materials, and in the weight ratio of curing agent 1 to curing agent 2, see table 2 specifically;
the adhesives of examples 2 to 6 were prepared according to the method of preparing the adhesive of example 1, except that the stirring time and the ultrasonic dispersion time in step (2) were different, and the stirring temperature and the stirring time in step (3) were different, as shown in table 3.
Comparative example 1
The difference from example 1 is that the curing agent is a mixture of curing agent 1 and curing agent 2 in a weight ratio of 0.7:1.5, so that the weight fraction of the weight of curing agent 1 in comparative example 1 is less than that of any of examples 1-6, and the weight fraction of curing agent 2 is greater than that of any of examples 1-6. Except for this, an adhesive for a conductive cloth tape was obtained in the same manner as in example 1.
Comparative example 2
The difference from example 1 is that the curing agent is a mixture of curing agent 1 and curing agent 2 in a weight ratio of 3:0.2, so that the weight fraction of curing agent 1 in comparative example 2 is greater than the weight fraction of any of examples 1-6, and the weight of curing agent 2 is less than the weight fraction of any of examples 1-6. Except for this, an adhesive for a conductive cloth tape was obtained in the same manner as in example 1.
Comparative example 3
The difference from example 1 is that the weight part of the accelerator is 9 parts, so that the weight fraction of the accelerator in comparative example 3 is less than that of any of examples 1 to 6. Except for this, an adhesive for a conductive cloth tape was obtained in the same manner as in example 1.
Comparative example 4
The difference from example 1 is that no microcrystalline wax, pine tar and sorbitol were added in comparative example 4. Except for this, an adhesive for a conductive cloth tape was obtained in the same manner as in example 1.
The raw material amounts of the adhesives of comparative examples 1 to 4 are specifically shown in Table 1.
TABLE 1 raw material amounts (weight/kg) of adhesives in examples 1 to 6 and comparative examples 1 to 4
TABLE 2 Components of epoxy resin, Accelerator, curing agent 1 and curing agent 2 and weight ratio of curing agent 1 to curing agent 2 in raw materials of adhesives in examples 1 to 6
TABLE 3 preparation of Adhesives in examples 1-6 with respect to the parameters of stirring time, ultrasonic dispersion time, stirring temperature, and stirring time
Application example 1
The adhesive obtained in example 1 was applied to the conductive cloth tape of application example 1, which includes a conductive cloth, an adhesive coated on the conductive cloth, and a tin-plated copper foil covering the adhesive.
The preparation method of the conductive cloth tape comprises the following steps:
s1, coating adhesive on the surface of the conductive cloth, wherein the coating speed is 7-10m/min, and the adhesive coating amount is 5-9g/m2；
S2, feeding the conductive cloth coated with the adhesive into an oven, heating and naturally cooling;
and S3, covering a layer of tinned copper foil on the dried adhesive to obtain the conductive cloth adhesive tape.
Wherein the thickness of the adhesive layer on the surface of the conductive cloth is 20-25 μm.
Application examples 2 to 6
The adhesive obtained in examples 2 to 6 was applied to the conductive cloth tape of application examples 2 to 6, which contained conductive cloth, an adhesive coated on the conductive cloth, and a tin-plated copper foil covering the adhesive.
The steps of the methods for preparing the conductive fabric tape of application examples 2 to 6 are the same as those of the method for preparing the conductive fabric tape of application example 1, except that the coating rate, the coating amount and the thickness of the adhesive layer on the surface of the conductive fabric are different in S1, as shown in table 4.
Application of comparative examples 1 to 4
The adhesives obtained in comparative examples 1 to 4 were applied to the conductive cloth tapes of application examples 1 to 4, and the conductive cloth tapes were obtained in the same manner as in application example 1 using comparative examples 1 to 4.
Table 4 parameters of coating rate, coating amount, and thickness of adhesive layer in the method for preparing the conductive cloth tape of application examples 1 to 6
Performance test
The tensile property at normal temperature (20 ℃) is tested according to GB7124-86 adhesive tensile shear strength test method, the tensile property at low temperature (-50 ℃) is tested according to GJ1709 GJB1709-1993 adhesive low-temperature tensile shear strength test method, and the thermal stability is determined according to G16978 GB/T16978-1997 hot melt adhesive thermal stability; the conductive cloth adhesive tapes prepared in application examples 1-6 and application comparative examples 1-4 are tested according to the test method of the peeling strength of the adhesive tape GB/T2792-.
As can be seen from table 5, the adhesive of examples 1 to 6 exhibited no discoloration in terms of thermal stability, because the methyl group in the silicone resin imparted the resin matrix with high thermal stability, and the phenyl group in the silicone resin imparted the resin matrix with high oxidation stability, while the epoxy resin, white carbon and pine tar also enhanced the thermal stability of the resin matrix, so that the adhesive of examples 1 to 6 exhibited no discoloration in appearance; on the contrary, the adhesives of comparative examples 1 to 3 showed yellowing because the curing agent 1 of comparative example 1 was contained in a smaller amount than those of examples 1 to 6, and the accelerator of comparative example 3 was contained in a smaller amount than those of examples 1 to 6, so that the epoxy resin in the adhesives of comparative examples 1 and 3 was less likely to exert the thermal stability, while the curing agent 2 of comparative example 2 was contained in a smaller amount than those of examples 1 to 6, so that the silicone resin in the adhesive of comparative example 2 was less likely to exert the thermal stability, thereby resulting in the adhesives of comparative examples 1 to 3 showing yellowing in appearance; the adhesive of comparative example 4 appeared yellowish, because no microcrystalline wax, sorbitol and pine tar were added to the adhesive of comparative example 4, which also had a certain heat resistance.
In terms of tensile shear strength, the greater the tensile shear strength, the better the toughness of the adhesive, and the lower the tensile shear strength, the poorer the toughness. The tensile shear strength of the adhesive of examples 1 to 6 is 4MPa or more at normal temperature and 7.5MPa or more at low temperature, and it can be seen that the adhesive of examples 1 to 6 shows better toughness against shear impact of external force load; comparative example 1 and comparative example 3 showed better toughness than examples 1 to 6, because the curing agent in comparative example 1 and the accelerator in comparative example 3 were less than those in examples 1 to 6, resulting in a cured product having a lower crosslinking density, less brittleness and higher tensile shear strength, resulting in comparative example 1 and comparative example 3 showing better toughness; in contrast, comparative example 2 and comparative example 4 showed inferior toughness to examples 1 to 6 because the curing agent 2 in comparative example 2 was less than those in examples 1 to 5, while comparative example 4 showed inferior toughness to examples 1 to 6 because of the lack of microcrystalline wax, sorbitol and pine tar, making it more difficult for a resin matrix to exert the corresponding mechanical properties.
In terms of peel strength, the greater the peel strength, the poorer the toughness of the adhesive, but the better the bond strength. The peel strength of the application examples 1-6 is more than 10MPa, and the conductive cloth adhesive tapes of the application examples 1-6 show better bonding strength; the application comparative example 1 and the application comparative example 3 showed better toughness and poorer adhesive strength, and the application comparative example 2 and the application comparative example 4 showed poorer toughness and better adhesive strength than the examples 1 to 6.
In terms of volume resistivity, the smaller the volume resistivity vertically, the better the conductivity is exhibited, and the volume resistivities of application examples 1 to 6 are all less than 3 x 10-4Omega cm, excellent conductive performance is shown, however, the conductive performance of the application examples 1-4 is poorer than that of the application examples 1-6, because the flake silver powder which is at a certain distance before curing is contacted in the curing shrinkage process of the resin matrix, so that the flake silver powder is changed from non-conductive to conductive, the tunneling resistance is greatly reduced, and meanwhile, the contacted silver powder is deformed under the curing shrinkage force, so that the contact area is further increased, and the transmission of electrons between the flake silver powders is easierThe concentrated resistance is reduced, so that the resistance of the conductive adhesive is reduced, and the conductivity is improved; meanwhile, the quantity of functional groups of the epoxy resin and the addition amount of the curing agent both affect the volume resistivity of the conductive colloid, the volume resistivity is gradually reduced along with the increase of the quantity of the functional groups of the epoxy resin, the curing shrinkage rate is increased along with the addition of the quality of the curing agent, and the volume resistivity is reduced, so that when the mass ratio of the epoxy resin to the curing agent is too small, the curing is incomplete, the adhesive force of the adhesive is low, the density of the conductive filler is reduced, and the conductivity is poor, but if the mass ratio of the epoxy resin to the curing agent is too large, the mass fraction of the conductive filler is reduced on one hand, and on the other hand, the resistivity of the epoxy resin per se is also increased along with the increase of the curing degree; the microcrystalline wax is mixed with the resin, so that the adhesive has excellent adhesiveness, the pine tar is beneficial to the dispersion of the compounding agent in the rubber material, the viscosity of the adhesive is increased, the white carbon black has porosity and large specific surface area, and the contact area between the silver powder is increased, so that the microcrystalline wax, the pine tar and the white carbon black can reduce the volume resistivity.
In conclusion, the adhesives of examples 1-6 exhibited moderate toughness and bonding strength, and had excellent conductive effect and thermal stability.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. An adhesive for a conductive cloth adhesive tape, which is characterized in that,
the adhesive is prepared from the following raw materials in parts by weight:
epoxy resin: 25 to 33 portions of the components are mixed,
silicone resin: 12-15 parts of (by weight),
flake silver powder: 78 to 106 portions of the raw materials are mixed,
white carbon black: 3-5 parts of (A) a water-soluble polymer,
curing agent: 25 to 31 portions of the components are added,
accelerator (b): 17-25 parts of (a) a water-soluble polymer,
microcrystalline wax: 8-14 parts of (by weight),
pine tar: 3.6 to 6 portions of the raw materials,
sorbitol: 2-7 parts.
2. The adhesive for conductive cloth tapes as claimed in claim 1, wherein the epoxy resin comprises one or more of bisphenol a type epoxy resin and acrylic epoxy resin.
3. The adhesive for conductive cloth tapes as claimed in claim 1, wherein the silicone resin is vinyl terminated T-type phenyl polysiloxane.
4. The adhesive for conductive fabric tapes as claimed in claim 1, wherein the curing agent comprises a curing agent 1 and a curing agent 2, the curing agent 1 comprises one or more of trimellitic anhydride and 2-ethyl-4-methylimidazole, and the curing agent 2 comprises one or more of ethyl orthosilicate and dibutyltin dilaurate.
5. The adhesive for the conductive cloth adhesive tape as claimed in claim 1, wherein the curing agent is a mixture of (1.2-2.1): (0.5-0.8) curing agent 1 and 2.
6. The adhesive for conductive fabric tapes as claimed in claim 1, wherein the accelerator is one or more of N, N-dimethylaniline, 2, 4, 6, -tris (dimethylaminomethyl) phenol.
7. The adhesive for conductive fabric tapes as recited in claim 1, wherein said silica is precipitated silica.
8. The method for preparing the adhesive for the conductive cloth tape according to any one of claims 1 to 7, characterized by comprising the steps of:
(1) mixing epoxy resin, organic silicon resin and a curing agent to prepare a resin matrix with uniform components;
(2) sequentially dissolving the white carbon black and the flake silver powder in the resin matrix prepared in the step (1), mechanically stirring for 1-2h, and ultrasonically dispersing for 2-4h to obtain a mixture of the resin matrix and the conductive filler;
(3) adding the mixture obtained in the step (2) into microcrystalline wax, stirring for 20-45min at the temperature of 100-145 ℃, adding pine tar and sorbitol, and uniformly mixing to obtain the product.
9. A conductive cloth tape comprising a conductive cloth, an adhesive agent coated on the conductive cloth, and a tin-plated copper foil covering the adhesive agent, wherein the adhesive agent is the adhesive agent for conductive cloth tapes according to any one of claims 1 to 7.
10. The method for preparing the conductive cloth tape of claim 9, comprising the steps of: s1, coating adhesive on the surface of the conductive cloth, wherein the coating speed is 7-10m/min, and the adhesive coating amount is 5-9g/m2；
S2, feeding the conductive cloth coated with the adhesive into an oven, heating and naturally cooling;
and S3, covering a layer of tinned copper foil on the dried adhesive to obtain the conductive cloth adhesive tape.
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| CN202010377141.0A CN111334233A (en) | 2020-05-07 | 2020-05-07 | Adhesive for conductive cloth adhesive tape, preparation method and application thereof |
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Application publication date: 20200626 |