CN112760074A - High-toughness and heat and humidity resistant double-component epoxy transparent conductive adhesive and preparation method thereof - Google Patents

High-toughness and heat and humidity resistant double-component epoxy transparent conductive adhesive and preparation method thereof Download PDF

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CN112760074A
CN112760074A CN202110215802.4A CN202110215802A CN112760074A CN 112760074 A CN112760074 A CN 112760074A CN 202110215802 A CN202110215802 A CN 202110215802A CN 112760074 A CN112760074 A CN 112760074A
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CN112760074B (en
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魏芳芳
李峰
贺国新
张利文
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Yantai Xinyou New Material Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C09J163/10Epoxy resins modified by unsaturated compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
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    • C08K3/08Metals
    • C08K2003/0806Silver
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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Abstract

The invention relates to a high-toughness and humidity-heat-resistant double-component epoxy transparent conductive adhesive and preparation and use methods thereof, and relates to the field of conductive adhesives. The high-toughness and humidity-heat-resistant double-component epoxy transparent conductive adhesive comprises A, B two components, wherein the component A comprises 70-100 parts by weight of self-made acrylic modified epoxy resin containing an organic silicon long chain, 10-20 parts by weight of an epoxy diluent, 20-30 parts by weight of a conductive filler with high transparency and 1-10 parts by weight of a thixotropic agent; the component B comprises: 35-50 parts of polyether amine curing agent, 1-3 parts of silane coupling agent and 5-10 parts of curing accelerator. The conductive adhesive of the invention introduces a large amount of Si-O bonds, thus improving the flexibility and the humidity resistance of the adhesive. The adhesive can be widely applied to the adhesion of flexible electronic products, and has good application prospect.

Description

High-toughness and heat and humidity resistant double-component epoxy transparent conductive adhesive and preparation method thereof
Technical Field
The invention relates to the field of double-component conductive adhesives, in particular to a high-toughness and humidity-heat-resistant double-component epoxy transparent conductive adhesive and a preparation method thereof.
Background
At present, the conductive paste appearing on the market is basically prepared by filling conductive powder into a supply binder. The conductive adhesive system can be divided into an acrylic system, an epoxy system, an organic silicon system and the like. The acrylic acid system has the advantages of fast curing, high adhesion, wide Tg regulating range and the like, but has poor moisture resistance and aging resistance; the epoxy system has good adhesion and aging resistance, but the cured product has high hardness, poor flexibility and large stress; the silicone system cures quickly and has good aging resistance but poor adhesion.
In view of the problems of the three conductive adhesives at present, the invention prepares the acrylic acid modified epoxy resin containing the organosilicon long chain by carrying out organosilicon modification on the epoxy acrylate containing the acrylic double bond and the epoxy group at the same time, and adopts polyether amine with better flexibility to carry out curing, so that the cured glue has excellent flexibility, humidity and heat resistance and other aging resistance. The invention also enables the cured glue to have higher transparency by using the Ag nanowire and Ag nanoparticle composite conductive filler with better transparency.
Disclosure of Invention
The invention discloses a high-toughness, humidity-resistant and heat-resistant two-component epoxy transparent conductive adhesive and a preparation method thereof, and provides an acrylic modified epoxy resin containing an organic silicon long chain, which is used for preparing the high-toughness, humidity-resistant and heat-resistant two-component epoxy transparent conductive adhesive and has the advantages of high flexibility, bending resistance, excellent adhesive force and aging resistance.
In order to realize the technical effects, the invention discloses a high-toughness and humidity-heat-resistant double-component epoxy transparent conductive adhesive which is characterized by comprising A, B components, wherein the component A comprises the following raw materials in parts by weight:
70-100 parts of acrylic acid modified epoxy resin containing an organic silicon long chain;
10-20 parts of an epoxy diluent;
20-30 parts of high-transparency conductive filler;
1-10 parts of a thixotropic agent;
wherein the component B comprises the following raw materials in parts by weight:
35-50 parts of a polyether amine curing agent;
1-3 parts of a silane coupling agent;
5-10 parts of a curing accelerator;
the acrylic modified epoxy resin containing the organic silicon long chain has a structure shown in the following formula I,
Figure DEST_PATH_IMAGE001
formula I
Wherein R in formula I is
Figure 661465DEST_PATH_IMAGE002
Of bisphenol A epoxy structure or
Figure DEST_PATH_IMAGE003
One of bisphenol F epoxy structures.
Further, the acrylic acid modified epoxy resin containing the organosilicon long chain is prepared from epoxy acrylate and hydrogen-containing polydimethylsiloxane, wherein one end of the epoxy acrylate is provided with an acrylic double bond, and the other end of the epoxy acrylate is provided with two functional groups of an epoxy group, the hydrogen-containing polydimethylsiloxane has a structure shown in a formula II, the epoxy acrylate has a structure shown in a formula III,
Figure 60829DEST_PATH_IMAGE004
formula II
Figure DEST_PATH_IMAGE005
And (3) formula III.
Further, the acrylic modified epoxy resin containing the organosilicon long chain is prepared according to the following steps:
is provided with a general formula N2In a 250 mL four-neck flask with a device, a stirrer, a thermometer, a constant-pressure feeding funnel and a reflux condensing device, 100g of bisphenol A (or bisphenol F) epoxy acrylate and 15-25 g of hydrogen-containing Polydimethylsiloxane (PHMS) are added into 30-50 g of toluene solvent, the temperature is slowly increased to 65-80 ℃, 0.008-0.015 g of chloroplatinic acid isopropanol solution is added, and N is introduced2Stirring for 3-5 h under the condition of the rotating speed of 500-800 r/min under protection, testing the epoxy equivalent once every half hour, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing and evaporating to remove the solvent to obtain colorless transparent liquid, namely the organic silicon-containing liquidA chain acrylic modified epoxy resin.
Preferably, the mass fraction of the chloroplatinic acid in the chloroplatinic acid isopropanol solution is 2%.
Furthermore, the epoxy equivalent of the acrylic modified epoxy resin containing the organosilicon long chain is 200 g/eq-400 g/eq.
Further, the high-transparency conductive filler is a mixture of Ag nanowires and Ag nanoparticles with high conductivity and transparency, and the weight ratio of the Ag nanowires to the Ag nanoparticles is 7: 3-8: 2.
Furthermore, the diameter of the Ag nanowire is 10-100 nm, and the length of the Ag nanowire is 10-100 um; the diameter of the Ag nano particles is 10-50 nm.
Further, the polyether amine curing agent is selected from one or a mixture of any more of polyether amine D-230, polyether amine D-400, polyether amine D-2000 and polyether amine D-4000;
the curing accelerator is one or a mixture of DMP-30, triethanolamine and nonyl phenol.
The epoxy diluent is one or a mixture of any more of C12-14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, 1, 6-hexanediol diglycidyl ether and polypropylene glycol diglycidyl ether.
The thixotropic agent is fumed silica.
The coupling agent is one or a mixture of any more of 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane and 3-glycidoxypropyldiethoxysilane.
The invention also discloses a preparation method of the high-toughness damp-heat resistant double-component epoxy transparent conductive adhesive, which is characterized by comprising the following steps of:
wherein the component A is prepared by the following steps:
adding self-made acrylic acid modified epoxy resin containing an organic silicon long chain, an epoxy diluent and a high-transparency conductive filler into a stirring kettle, and stirring for 30min under the conditions of revolution of 10-50 r/min and rotation of 600-1000 r/min in a vacuum state; adding a thixotropic agent, stirring for 10-30 min under the condition of revolution of 10-30 r/min, and discharging to obtain a component A;
wherein the component B is prepared by the following steps:
adding the polyether amine curing agent, the silane coupling agent and the curing accelerator into a stirring kettle, revolving for 10-50 r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
The invention also discloses a use method of the high-toughness damp-heat resistant double-component epoxy transparent conductive adhesive, which is characterized in that the component A and the component B are mixed and stirred uniformly according to the mass ratio of (2.5-3.5) to 1, and the mixture is cured at room temperature.
The beneficial effects of the invention include:
(1) according to the invention, the epoxy acrylate containing acrylic double bonds and epoxy groups is subjected to organic silicon modification by a hydrosilylation method, so that the acrylic modified epoxy resin containing organic silicon long chains, which retains the epoxy bonds and has an epoxy equivalent of 200 g/eq-400 g/eq, is prepared.
(2) According to the invention, the acrylic acid modified epoxy resin containing the organosilicon long chain is added into the adhesive, so that the cured adhesive has the hardness of 50-60 Shore A, the tensile strength of more than 10 MPa, the elongation at break of more than 150%, the retention rate of cold and hot impact strength of 240 cycles of more than 95%, the retention rate of double 85@500h strength of more than 90%, and good flexibility and aging resistance.
(3) According to the invention, the composite conductive filler of the Ag nanowires and the Ag nanoparticles with a specific proportion specification is added, so that the glue has conductivity and transmittance higher than 90%.
(4) The invention can be solidified at room temperature, and has simple operation and long applicable period.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Preparation of matrix resin component (A component): adding 90 parts of self-made acrylic modified epoxy resin containing an organic silicon long chain, 15 parts of C12-C14 alkyl glycidyl ether agent, 15 parts of Ag nanowires and 5 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 3 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-230, 15 parts of polyetheramine D-2000, 1 part of 3-glycidyl ether oxypropyltriethoxysilane and 9 parts of DMP-30 into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
And accurately weighing 25g of the prepared component A and 10g of the component B, stirring for 10min to prepare glue, and testing the performance of the glue.
The acrylic acid modified epoxy resin containing the organic silicon long chain is prepared according to the following steps:
is provided with a general formula N2In a 250 mL four-neck flask equipped with a stirrer, a thermometer, a constant pressure addition funnel and a reflux condenser, 100g of bisphenol A epoxy acrylate and 20g of hydrogenous Polydimethylsiloxane (PHMS) were added to 40g of a toluene solvent, the temperature was slowly raised to 65 ℃, 0.015g of an isopropyl alcohol chloroplatinic acid solution was added, and N was introduced2Under protection, stirring for 5 hours at the rotating speed of 800r/min, testing the epoxy equivalent once every half hour, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing, and evaporating to remove the solvent to obtain colorless transparent liquid, namely the acrylic modified epoxy resin containing the organic silicon long chain.
Example 2
(1) Preparation of matrix resin component (A component): adding 75 parts of self-made acrylic modified epoxy resin containing an organic silicon long chain, 20 parts of ethylene glycol diglycidyl ether, 20 parts of Ag nanowires and 5 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 2 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-400, 10 parts of polyetheramine D-2000, 1.5 parts of 3-glycidyl ether oxypropyltrimethoxysilane and 8 parts of triethanolamine into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
And (3) accurately weighing 30g of the prepared component A and 10g of the prepared component B, stirring for 10min to prepare glue, and testing the performance of the glue.
The acrylic acid modified epoxy resin containing the organic silicon long chain is prepared according to the following steps:
is provided with a general formula N2In a 250 mL four-necked flask equipped with an apparatus, a stirrer, a thermometer, a constant pressure addition funnel and a reflux condenser, 100g of bisphenol F epoxy acrylate and 20g of hydrogenous Polydimethylsiloxane (PHMS) were added to 40g of a toluene solvent, the temperature was slowly raised to 70 ℃, 0.01g of an isopropyl alcohol chloroplatinic acid solution was added, and N was introduced2Under protection, stirring for 4 hours at the rotating speed of 600r/min, testing the epoxy equivalent once every half hour, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing, and evaporating to remove the solvent to obtain colorless transparent liquid, namely the acrylic modified epoxy resin containing the organic silicon long chain.
Example 3
(1) Preparation of matrix resin component (A component): adding 75 parts of self-made acrylic acid modified epoxy resin containing an organic silicon long chain, 15 parts of 1, 6-hexanediol diglycidyl ether, 17 parts of Ag nanowires and 5 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and rotation at 600r/min in a vacuum state; adding 2 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-230, 10 parts of polyetheramine D-4000, 1.5 parts of 3-glycidyl ether oxypropyl methyldimethoxysilane and 6 parts of nonylphenol into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
Accurately weighing 35g of the prepared component A and 10g of the component B, stirring for 10min to prepare glue, and testing the performance of the glue.
The acrylic acid modified epoxy resin containing the organic silicon long chain is prepared according to the following steps:
is provided with a general formula N2In a 250 mL four-necked flask equipped with an apparatus, stirrer, thermometer, constant-pressure addition funnel and reflux condenser, 100g of bisphenol A epoxy acrylate and 22g of hydrogenous Polydimethylsiloxane (PHMS) were charged into 40g of a toluene solvent, the temperature was slowly raised to 75 ℃, 0.009g of chloroplatinic acid isopropanol solution was added, and N was introduced2Under protection, stirring for 4 hours at the rotating speed of 600r/min, testing the epoxy equivalent once every half hour, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing, and evaporating to remove the solvent to obtain colorless transparent liquid, namely the acrylic modified epoxy resin containing the organic silicon long chain.
Example 4
(1) Preparation of matrix resin component (A component): adding 85 parts of self-made acrylic acid modified epoxy resin containing an organic silicon long chain, 10 parts of polypropylene glycol diglycidyl ether, 18 parts of Ag nanowires and 7 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 1.5 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-400, 15 parts of polyetheramine D-4000, 1.5 parts of 3-glycidyl ether oxypropyldiethoxysilane and 8 parts of DMP-30 into a stirring kettle, revolving for 20r/min under a vacuum state, stirring for 30min, and discharging to obtain the component B.
28g of the prepared component A and 10g of the prepared component B are accurately weighed, stirred for 10min to prepare glue, and the performance of the glue is tested.
The acrylic acid modified epoxy resin containing the organic silicon long chain is prepared according to the following steps:
is provided with a general formula N2100g of bisphenol F epoxy acrylate and 20g of hydrogenous Polydimethylsiloxane (PHMS) are added into 40g of toluene solvent in a 250 mL four-neck flask with a device, a stirrer, a thermometer, a constant-pressure feeding funnel and a reflux condensing device, the temperature is slowly raised to 80 ℃, 0.008g of chloroplatinic acid isopropanol solution is added, and N is introduced2Under protection, stirring for 3 hours at the rotating speed of 500r/min, testing the epoxy equivalent once every half hour, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing, and evaporating to remove the solvent to obtain colorless transparent liquid, namely the acrylic modified epoxy resin containing the organic silicon long chain.
Comparative example 1
(1) Preparation of matrix resin component (A component): adding 90 parts of bisphenol A epoxy acrylate (containing double bonds and epoxy groups), 15 parts of C12-C14 alkyl glycidyl ether, 15 parts of Ag nanowires and 5 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 3 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-230, 15 parts of polyetheramine D-2000, 1 part of 3-glycidyl ether oxypropyltriethoxysilane and 9 parts of DMP-30 into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
And accurately weighing 25g of the prepared component A and 10g of the component B, stirring for 10min to prepare glue, and testing the performance of the glue.
Comparative example 2
(1) Preparation of matrix resin component (A component): adding 75 parts of bisphenol F epoxy acrylate (containing double bonds and epoxy groups), 20 parts of ethylene glycol diglycidyl ether and 25 parts of flaky conductive silver powder into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 2 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 30 parts of polyetheramine D-400, 10 parts of polyetheramine D-2000, 1.5 parts of 3-glycidyl ether oxypropyltrimethoxysilane and 8 parts of triethanolamine into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
And (3) accurately weighing 30g of the prepared component A and 10g of the prepared component B, stirring for 10min to prepare glue, and testing the performance of the glue.
Comparative example 3
(1) Preparation of matrix resin component (A component): adding 75 parts of E51 epoxy resin, 15 parts of 1, 6-hexanediol diglycidyl ether, 17 parts of Ag nanowires and 5 parts of Ag nanoparticles into a stirring kettle, and stirring for 30min under the conditions of revolution at 30 r/min and autorotation at 600r/min in a vacuum state; adding 2 parts of fumed silica, stirring for 30min under the condition of revolution of 20r/min, and discharging to obtain the component A.
(2) Preparation of the curing agent component (B component): adding 25 parts of polyetheramine D-400, 10 parts of polyetheramine D-2000, 1.5 parts of 3-glycidyl ether oxypropyldiethoxysilane and 5 parts of nonylphenol into a stirring kettle, revolving for 20r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
And (3) accurately weighing 30g of the prepared component A and 10g of the prepared component B, stirring for 10min to prepare glue, and testing the performance of the glue.
The beneficial effects of the present invention are further illustrated below in conjunction with experimental data:
1, materials and methods:
1.1 test site: futai Xinyou New Material Co, Ltd laboratory.
1.2 test detection:
hardness testing instrument: a hardness tester.
The transmittance test method comprises the following steps: and (5) curing the circular glue block with the thickness of 0.3mm, and testing the light transmittance of the glue by using a light transmittance instrument.
Tensile shear strength: the test is carried out according to GB/T7124-2008 standard, the tensile shear strength of PC to PC is tested, and the curing condition is 80 ℃ and 60 min.
Elongation at break: and performing sample preparation detection according to GB/T2567-.
Retention rate of cold and hot impact strength: the solidified test piece is put into the temperature of minus 40 ℃ to 120 ℃ and is circulated for 240 times, and each time lasts for 1 hour. After the end of the cycle, the tensile shear strength was measured and the strength retention was calculated.
Double 85 strength retention: the cured test piece was placed at 85 ℃ and 85% humidity for 500 hours. After completion, the tensile shear strength was measured and the strength retention was calculated.
1.3 test materials: comparative examples 1 to 3, examples 1 to 4.
The experiment was conducted in a consistent manner except for the different experimental treatments.
Figure 309408DEST_PATH_IMAGE006
Compared with the hardness data of comparative examples 1-3 in the table, the hardness of the glue is obviously lower than that of comparative examples 1-3 after curing, the elongation at break of the glue is obviously higher than that of the comparative examples, and the glue has better flexibility. Compared with the retention rate of the cold and hot impact strength and the retention rate of the double 85 strength of the invention in comparative examples 1 to 3 in the table, the humidity resistance of the invention can be obviously improved by the self-made acrylic modified epoxy resin containing the organosilicon long chain. The invention has a transmittance higher than 90%. Therefore, the conductive adhesive prepared by the invention has the advantages of high flexibility, high transparency and humidity resistance, and has a plurality of potential applications in the field of bonding of flexible electronic products.
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.

Claims (10)

1. The high-toughness and humidity-heat-resistant double-component epoxy transparent conductive adhesive is characterized by comprising A, B components, wherein the component A comprises the following raw materials in parts by weight:
70-100 parts of acrylic acid modified epoxy resin containing an organic silicon long chain;
10-20 parts of an epoxy diluent;
20-30 parts of high-transparency conductive filler;
1-10 parts of a thixotropic agent;
wherein the component B comprises the following raw materials in parts by weight:
35-50 parts of a polyether amine curing agent;
1-3 parts of a silane coupling agent;
5-10 parts of a curing accelerator;
the acrylic modified epoxy resin containing the organic silicon long chain has a structure shown in the following formula I,
Figure 34725DEST_PATH_IMAGE001
formula I
Wherein R in formula I is
Figure DEST_PATH_IMAGE002
Of bisphenol A epoxy structure or
Figure 279762DEST_PATH_IMAGE003
One of bisphenol F epoxy structures.
2. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 1, characterized in that: the acrylic acid modified epoxy resin containing the organic silicon long chain is prepared from epoxy acrylate and hydrogen-containing polydimethylsiloxane, wherein one end of the epoxy acrylate is provided with an acrylic double bond, and the other end of the epoxy acrylate is provided with two functional groups of an epoxy group, the hydrogen-containing polydimethylsiloxane has a structure shown in a formula II, the epoxy acrylate has a structure shown in a formula III,
Figure DEST_PATH_IMAGE004
formula II
Figure 528341DEST_PATH_IMAGE005
And (3) formula III.
3. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 2, characterized in that: the acrylic acid modified epoxy resin containing the organic silicon long chain is prepared according to the following steps:
is provided with a general formula N2Adding 100g of epoxy acrylate and hydrogen-containing polydimethylsiloxane into 30-50 g of toluene solvent in a reaction container flask of a device and a reflux condensing device, slowly heating to 65-80 ℃, adding 0.008-0.015 g of chloroplatinic acid isopropanol solution, introducing N2Under protection, stirring for 3-5 h at the rotating speed of 500-800 r/min, testing the epoxy equivalent at intervals, stopping stirring when the epoxy equivalent tends to be constant, vacuumizing, decompressing, and evaporating to remove the solvent to obtain colorless transparent liquid, namely the acrylic modified epoxy resin containing the organic silicon long chain.
4. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 3, characterized in that: the mass fraction of chloroplatinic acid in the chloroplatinic acid isopropanol solution is 2%.
5. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 1, characterized in that: the acrylic modified epoxy resin containing the organosilicon long chain has an epoxy equivalent of 200 g/eq-400 g/eq.
6. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 1, characterized in that: the high-transparency conductive filler is a mixture of Ag nanowires and Ag nanoparticles with high conductivity and transparency, and the weight ratio of the Ag nanowires to the Ag nanoparticles is 7: 3-8: 2.
7. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 6, characterized in that: the diameter of the Ag nanowire is 10-100 nm, and the length of the Ag nanowire is 10-100 um; the diameter of the Ag nano particles is 10-50 nm.
8. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to claim 1, characterized in that: the polyether amine curing agent is selected from one or a mixture of any more of polyether amine D-230, polyether amine D-400, polyether amine D-2000 and polyether amine D-4000;
the curing accelerator is one or a mixture of DMP-30, triethanolamine and nonyl phenol.
9. The preparation method of the high-toughness humidity-heat resistant double-component epoxy transparent conductive adhesive according to any one of claims 1 to 8, characterized in that:
wherein the component A is prepared by the following steps:
adding self-made acrylic acid modified epoxy resin containing an organic silicon long chain, an epoxy diluent and a high-transparency conductive filler into a stirring kettle, and stirring for 30min under the conditions of revolution of 10-50 r/min and rotation of 600-1000 r/min in a vacuum state; adding a thixotropic agent, stirring for 10-30 min under the condition of revolution of 10-30 r/min, and discharging to obtain a component A;
wherein the component B is prepared by the following steps:
adding the polyether amine curing agent, the silane coupling agent and the curing accelerator into a stirring kettle, revolving for 10-50 r/min in a vacuum state, stirring for 30min, and discharging to obtain the component B.
10. The high-toughness humidity-resistant two-component epoxy transparent conductive adhesive according to any one of claims 1 to 8, characterized in that: and (3) uniformly mixing and stirring the component A and the component B according to the mass ratio of (2.5-3.5) to 1, and curing the mixture at room temperature.
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CN102703009A (en) * 2012-07-05 2012-10-03 黑龙江省科学院石油化学研究院 Preparation method of nano silicon dioxide/polyacrylate modified epoxy resin adhesive
CN112358841A (en) * 2020-12-29 2021-02-12 烟台信友新材料有限公司 Flexible UV-thermal dual-curing transparent conductive adhesive and preparation method thereof

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US20060039889A1 (en) * 2002-12-26 2006-02-23 Rhodia Chimie Anti-fouling cationically crosslinkable varnish compositions and support substrates coated therewith
US20090264035A1 (en) * 2005-12-09 2009-10-22 Bluestar Silicones France Anti-fouling polyaddition silicone varnish, application of this varnish to a support and support thus treated
CN102516916A (en) * 2011-12-12 2012-06-27 东莞市派乐玛新材料技术开发有限公司 Liquid crystal sealant composition
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