CN112852379A - High-toughness, heat and humidity resistant ultraviolet curing conductive adhesive and preparation method thereof - Google Patents
High-toughness, heat and humidity resistant ultraviolet curing conductive adhesive and preparation method thereof Download PDFInfo
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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
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- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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Abstract
The invention relates to a high-toughness moisture-heat-resistant ultraviolet-curable conductive adhesive and a preparation method thereof, and relates to the field of conductive adhesives. The adhesive is prepared from the following raw materials in parts by weight: 30-50 parts of self-made epoxy acrylate containing an organic silicon long chain, 10-20 parts of an organic silicon active diluent, 15-35 parts of an acrylic monomer, 3-8 parts of a photoinitiator, 0.05-0.2 part of a polymerization inhibitor, 1-3 parts of a silane coupling agent, 0-5 parts of a thixotropic agent and 12-25 parts of a conductive filler. According to the invention, the self-made epoxy acrylate containing the organic silicon long chain and the conductive filler with higher transparency are added into the colloid, so that the conductive adhesive based on the invention has the advantages of good transparency, good toughness, bending resistance, excellent humidity resistance and heat resistance, excellent high temperature resistance and wide application range.
Description
Technical Field
The invention relates to the field of conductive adhesives, in particular to a high-toughness moisture-heat-resistant ultraviolet-curable conductive adhesive and a preparation method thereof.
Background
The conductive adhesive is an adhesive with both adhesive and conductive properties. In recent years, conductive adhesive is used to replace Pb/Sn solder connecting materials and is increasingly applied to the fields of microelectronic packaging, printed circuit boards, conductive circuit bonding, electromagnetic shielding and the like.
At present, the conductive paste appearing on the market is basically prepared by filling conductive powder into an adhesive. 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, and the transparency of the glue is poor due to the addition of a large amount of metal conductive filler, so that the acrylic acid system is generally made into acrylic acid thermosetting glue or dual-curing glue.
CN 111087941A adopts the ion type conducting compound to replace traditional inorganic filler to realize the electrically conductive mode, changes traditional electron conduction into ion transmission conduction, realizes performances such as viscidity, electric conductivity, transparency, stability simultaneously. However, the solvent toluene is used in the preparation process, and heating for curing is required.
Disclosure of Invention
The invention discloses a high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive and a preparation method thereof, and provides epoxy acrylate containing an organic silicon long chain and a preparation method thereof, which are used for preparing the high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive, and the high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive has the advantages of good transparency, good toughness, bending resistance, excellent humidity resistance and high temperature resistance, and wide application range.
In order to achieve the technical effects, the invention discloses a high-toughness, heat and humidity resistant and ultraviolet light curing conductive adhesive which is characterized by being capable of curing under the irradiation of ultraviolet light with the wavelength of 200-420 nm and comprising the following raw materials in parts by weight:
30-50 parts of epoxy acrylate containing an organic silicon long chain; 10-20 parts of an organic silicon reactive diluent; 15-35 parts of an acrylic monomer; 3-8 parts of a photoinitiator; 0.05-0.2 part of polymerization inhibitor; 1-3 parts of a silane coupling agent and 12-25 parts of a conductive filler; 0-5 parts of a thixotropic agent;
wherein the epoxy acrylate containing the organosilicon long chain has the structure shown in the formula I,
wherein R in formula I is
Of bisphenol A epoxy structure or
One of bisphenol F epoxy structures.
Furthermore, the epoxy acrylate containing the organosilicon long chain is prepared by epoxy acrylate with an acrylic double bond at one end and an epoxy group at the other end and hydroxy-terminated polydimethylsiloxane under the catalysis of an organic tin catalyst, wherein the hydroxy-terminated polydimethylsiloxane has a structure shown in a formula II, the epoxy acrylate has a structure shown in a formula III,
further, the epoxy acrylate containing the organosilicon long chain is prepared according to the following steps:
weighing 100g of bisphenol A (or bisphenol F) epoxy acrylate, putting the epoxy acrylate into a 250mL four-neck flask provided with a mechanical stirring paddle, a thermometer, a constant-pressure dropping funnel and a reflux condensing device, adding 30-50 g of toluene, slowly heating to 90-110 ℃, adding 0.3-0.6 g of dibutyltin dilaurate as a reaction catalyst, gradually dropping 15-20 g of hydroxyl-terminated polydimethylsiloxane through the constant-pressure dropping funnel in the mechanical stirring process, keeping the temperature at 90-110 ℃, stirring for 4-6 hours at the rotating speed of 300-500 r/min, stopping stirring when the temperature of a system is reduced to 50 ℃, vacuumizing, decompressing and evaporating a solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
Further, the organic silicon reactive diluent is an organic silicon monomer containing a terminal acrylic acid structure. Preferably one or a mixture of KR-513, X-40-2672B and X-40-9272B available from shin-Etsu chemical Co., Ltd.
The acrylic monomer is one or a mixture of any more of isobornyl acrylate, isobornyl methacrylate, isooctyl acrylate, isooctyl methacrylate, isodecyl acrylate, tetrahydrofuran methacrylate, tricyclodecane dimethanol diacrylate, 1, 6-hexanediol diacrylate and tricyclopropyl oxide trimethylolpropane triacrylate.
The photoinitiator is selected from one or a mixture of any more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl benzophenone, bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide, 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-one, alpha' -dimethyl benzil ketal, isopropyl thioxanthone, benzophenone, 2,4, 6-trimethylbenzoyl benzene-diphenyl phosphine oxide and 2,4, 6-trimethylbenzoyl diphenyl phosphine oxide.
The polymerization inhibitor is one or a mixture of any more of hydroquinone, p-hydroxyanisole and 2, 6-di-tert-butyl-p-cresol.
The coupling agent is one or a mixture of any several of KH551, KH172, KH560 and KH 570.
The thixotropic agent is fumed silica.
Further, the high-transparency conductive filler is a mixture of Ag nanowires and Ag nanoparticles with high conductivity and transparency.
Preferably, 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.
More preferably, the weight ratio of the Ag nanowires to the Ag nanoparticles is 7: 3-8: 2.
The invention also discloses a preparation method of the high-toughness, heat and humidity resistant ultraviolet curing conductive adhesive, which comprises the following steps:
adding 30-50 parts of self-made epoxy acrylate containing an organic silicon long chain, 10-20 parts of an organic silicon reactive diluent, 15-35 parts of an acrylic monomer, 3-8 parts of a photoinitiator, 0.05-0.2 part of a polymerization inhibitor and 1-3 parts of a silane coupling agent into a stirring kettle, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 600-1000 r/min in a vacuum and light-proof state; adding 12-25 parts of conductive filler, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 600-1000 r/min in a vacuum and light-proof state; and adding 0-5 parts of thixotropic agent, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 300-800 r/min in a vacuum and dark state to obtain the high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive.
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 copolymerization modification method, so that the epoxy groups are replaced, and the epoxy acrylate containing organic silicon long chains and acrylic double bonds is prepared.
(2) According to the invention, the epoxy acrylate containing the organosilicon long chain is added into the adhesive, so that the cured adhesive has an elastic modulus lower than 1000MPa at 40 ℃ below zero, a tensile strength higher than 15MPa, a breaking elongation of 200%, a retention rate of 240 cycle strengths of cold and heat shock of more than 95%, a retention rate of double 85@500h strength of more than 85%, and good flexibility and aging resistance.
(3) According to the invention, the composite conductive filler of the Ag nano wires and the Ag nano particles is added, so that the glue has conductivity and transmittance higher than 90%.
(4) The invention can be solidified by ultraviolet light, and has simple operation and long working life.
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
Adding 40 parts of self-made epoxy acrylate containing an organic silicon long chain, 15 parts of KR-513, 20 parts of 1, 6-hexanediol diacrylate, 3 parts of 1-hydroxycyclohexyl benzophenone, 1.5 parts of bis (2,4, 6-trimethylbenzoyl) phenyl phosphine oxide, 0.1 part of hydroquinone and 1 part of silane coupling agent KH172 into a stirring kettle, and stirring for 30min under the conditions of vacuum and light shielding, revolution for 30r/min and rotation for 800 r/min; adding 15 parts of Ag nano wires and 5 parts of Ag nano particles, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and dark state; adding 1 part of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive.
The self-made epoxy acrylate containing the organic silicon long chain is prepared according to the following steps:
weighing 100g of bisphenol A epoxy acrylate, putting the bisphenol A epoxy acrylate into a 250mL four-neck flask provided with a mechanical stirring paddle, a thermometer, a constant-pressure dropping funnel and a reflux condensing device, adding 35g of toluene, slowly heating to 110 ℃, adding 0.3g of dibutyltin dilaurate as a reaction catalyst, gradually dropwise adding 15g of hydroxyl-terminated polydimethylsiloxane through the constant-pressure dropping funnel in the mechanical stirring process, keeping the temperature at 110 ℃, stirring for 4 hours under the condition that the rotating speed is 400r/min, stopping stirring when the temperature of a system is reduced to 50 ℃, vacuumizing, decompressing and evaporating a solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
Example 2
Adding 45 parts of self-made epoxy acrylate containing an organic silicon long chain, 10 parts of X-40-2672B, 20 parts of tetrahydrofuran methacrylate, 4 parts of 1-hydroxycyclohexyl benzophenone, 1.8 parts of 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-acetone, 0.05 part of p-hydroxyanisole and 1.5 parts of silane coupling agent KH560 into a stirring kettle, and stirring for 30min under the conditions of vacuum and light-proof state, revolution of 40r/min and rotation of 600 r/min; adding 17 parts of Ag nano wires and 5 parts of Ag nano particles, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and light-proof state; adding fumed silica, and stirring for 30min under vacuum and dark state under the conditions of revolution of 20r/min and rotation of 300r/min to obtain the high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive.
The self-made epoxy acrylate containing the organic silicon long chain is prepared according to the following steps:
weighing 100g of bisphenol F epoxy acrylate, putting the bisphenol F epoxy acrylate into a 250mL four-neck flask provided with a mechanical stirring paddle, a thermometer, a constant-pressure dropping funnel and a reflux condensing device, adding 35g of toluene, slowly heating to 100 ℃, adding 0.4g of dibutyltin dilaurate as a reaction catalyst, gradually dropwise adding 16g of hydroxyl-terminated polydimethylsiloxane through the constant-pressure dropping funnel in the mechanical stirring process, keeping the temperature at 100 ℃, stirring for 5 hours under the condition that the rotating speed is 400r/min, stopping stirring when the temperature of a system is reduced to 50 ℃, vacuumizing, decompressing and evaporating a solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
Example 3
Adding 50 parts of self-made epoxy acrylate containing an organic silicon long chain, 5 parts of X-40-9272B, 25 parts of isooctyl methacrylate, 4 parts of 2-hydroxy-2-methyl-1-phenyl acetone, 2 parts of 2,4, 6-trimethylbenzoylbenzene-diphenylphosphine oxide, 0.05 part of 2, 6-di-tert-butyl-p-cresol and 2 parts of a silane coupling agent KH570 into a stirring kettle, and stirring for 30min under the conditions of revolution of 40r/min and rotation of 600r/min in a vacuum and dark state; adding 20 parts of Ag nano-wires and 5 parts of Ag nano-particles, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and dark state; adding 1 part of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness, humidity-heat-resistant and ultraviolet-curable conductive adhesive.
The self-made epoxy acrylate containing the organic silicon long chain is prepared according to the following steps:
weighing 100g of bisphenol A epoxy acrylate, putting the bisphenol A epoxy acrylate into a 250mL four-neck flask provided with a mechanical stirring paddle, a thermometer, a constant-pressure dropping funnel and a reflux condensing device, adding 35g of toluene, slowly heating to 95 ℃, adding 0.5g of dibutyltin dilaurate as a reaction catalyst, gradually dropwise adding 18g of hydroxyl-terminated polydimethylsiloxane through the constant-pressure dropping funnel in the mechanical stirring process, keeping the temperature at 95 ℃, stirring for 5 hours under the condition that the rotating speed is 400r/min, stopping stirring when the temperature of a system is reduced to 50 ℃, vacuumizing, decompressing and evaporating a solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
Example 4
Adding 45 parts of self-made epoxy acrylate containing an organic silicon long chain, 15 parts of KR-513, 15 parts of tricyclopropyl oxide trimethylolpropane triacrylate, 4 parts of 1-hydroxycyclohexyl benzophenone, 2 parts of 2,4, 6-trimethylbenzoylbenzene-diphenylphosphine oxide, 0.05 part of 2, 6-di-tert-butyl-p-cresol and 2 parts of a silane coupling agent KH551 into a stirring kettle, and stirring for 30min under the conditions of vacuum and light shielding, revolution of 40r/min and rotation of 600 r/min; adding 18 parts of Ag nano wires and 7 parts of Ag nano particles, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and dark state; adding 1 part of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness, humidity-heat-resistant and ultraviolet-curable conductive adhesive.
The self-made epoxy acrylate containing the organic silicon long chain is prepared according to the following steps:
weighing 100g of bisphenol F epoxy acrylate, putting the bisphenol F epoxy acrylate into a 250mL four-neck flask provided with a mechanical stirring paddle, a thermometer, a constant-pressure dropping funnel and a reflux condensing device, adding 35g of toluene, slowly heating to 90 ℃, adding 0.6g of dibutyltin dilaurate as a reaction catalyst, gradually dropwise adding 20g of hydroxyl-terminated polydimethylsiloxane through the constant-pressure dropping funnel in the mechanical stirring process, keeping the temperature at 90 ℃, stirring for 6 hours under the condition that the rotating speed is 400r/min, stopping stirring when the temperature of a system is reduced to 50 ℃, vacuumizing, decompressing and evaporating a solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
Comparative example 1
Adding 40 parts of bisphenol A epoxy acrylate (containing double bonds and epoxy groups), 15 parts of KR-513, 20 parts of 1, 6-hexanediol diacrylate, 3 parts of 1-hydroxycyclohexyl benzophenone, 1.5 parts of bis (2,4, 6-trimethylbenzoyl) phenyl phosphine oxide, 0.1 part of hydroquinone and 1 part of silane coupling agent KH172 into a stirring kettle, and stirring for 30min under the conditions of vacuum and dark state, revolution for 30r/min and rotation for 800 r/min; adding 15 parts of Ag nano wires and 5 parts of Ag nano particles, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and dark state; adding 1 part of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive.
Comparative example 2
Adding 45 parts of bisphenol F epoxy acrylate (containing double bonds and epoxy groups), 10 parts of X-40-2672B, 20 parts of tetrahydrofuran methacrylate, 4 parts of 1-hydroxycyclohexyl benzophenone, 1.8 parts of 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-acetone, 0.05 part of p-hydroxyanisole and 1.5 parts of silane coupling agent KH560 into a stirring kettle, and stirring for 30min under the conditions of vacuum and dark conditions of revolution of 40r/min and rotation of 600 r/min; adding 25 parts of flaky conductive silver powder, and stirring for 30min under the conditions of revolution at 30r/min in a vacuum and dark state; adding 2 parts of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness humidity-heat-resistant ultraviolet-cured conductive adhesive.
Comparative example 3
Adding 45 parts of bifunctional urethane acrylate oligomer ETERCURE DR-U384, 15 parts of KR-513, 15 parts of isooctyl methacrylate, 4 parts of 1-hydroxycyclohexyl benzophenone, 2 parts of 2,4, 6-trimethylbenzoylbenzene-diphenylphosphine oxide, 0.05 part of 2, 6-di-tert-butyl-p-cresol and 1 part of silane coupling agent KH570 into a stirring kettle, and stirring for 30min under the conditions of vacuum and light shielding, revolution of 40r/min and rotation of 600 r/min; adding 25 parts of Ag nano wire, and stirring for 30min under the conditions of vacuum and light-proof state and revolution for 30 r/min; adding 1 part of fumed silica, and stirring for 30min under the conditions of revolution at 20r/min and rotation at 300r/min in a vacuum and dark state to obtain the high-toughness, humidity-heat-resistant and ultraviolet-curable conductive adhesive.
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:
elastic modulus test instrument: and (7) DMA.
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: testing the tensile shear strength of PC to PC according to GB/T7124-2008 standard, and testing the LED 365nm 100mw/cm under the curing condition2×20S。
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.
2 results and analysis:
compared with the elastic modulus data of comparative examples 1-3 in the table, the elastic modulus of the invention is obviously lower than that of comparative examples 1-3, the invention has better flexibility, the elastic modulus of the invention at minus 40 degrees is less than 1000MPa, and the elastic modulus of the invention is obviously lower than that of the comparative examples, which shows that the invention has better low temperature resistance. 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-prepared epoxy acrylate containing the organosilicon long chain. Compared with the transmittance data of comparative example 2 and the invention in the table, the invention has transmittance higher than 90% and can be cured by ultraviolet light. Therefore, the adhesive has the advantages of high flexibility, high transparency and humidity resistance.
According to the invention, the epoxy acrylate containing the organosilicon long chain is prepared by modifying the epoxy acrylate containing the acrylic double bond and the epoxy group, and the organosilicon and the epoxy resin chain segment enable the cured glue to have excellent flexibility, bonding force and humidity resistance. The invention also enables the glue to be subjected to ultraviolet curing by using the Ag nanowire and Ag nanoparticle composite conductive filler with better transparency. The method has many potential applications in the fields of flexible electronic components, soft functional material bonding and the like.
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 (9)
1. The high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive is characterized by being capable of being cured under the irradiation of ultraviolet light with the wavelength of 200-420 nm and comprises the following raw materials in parts by weight:
30-50 parts of epoxy acrylate containing an organic silicon long chain;
10-20 parts of an organic silicon reactive diluent;
15-35 parts of an acrylic monomer;
3-8 parts of a photoinitiator;
0.05-0.2 part of polymerization inhibitor;
1-3 parts of silane coupling agent
12-25 parts of conductive filler;
0-5 parts of a thixotropic agent;
wherein the epoxy acrylate containing the organosilicon long chain has the structure shown in the formula I,
wherein R in formula I is
Of bisphenol A epoxy structure or
One of bisphenol F epoxy structures.
2. The high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 1, wherein: the epoxy acrylate containing the organosilicon long chain is prepared by epoxy acrylate with an acrylic double bond at one end and an epoxy group at the other end and hydroxy-terminated polydimethylsiloxane under the catalysis of an organotin catalyst, wherein the hydroxy-terminated polydimethylsiloxane has a structure shown in a formula II, the epoxy acrylate has a structure shown in a formula III,
3. the high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 2, wherein: the epoxy acrylate containing the organosilicon long chain is prepared according to the following steps:
weighing 100g of bisphenol A epoxy acrylate, placing the bisphenol A epoxy acrylate into a reaction device, adding 30-50 g of toluene, slowly heating to 90-110 ℃, adding 0.3-0.6 g of dibutyltin dilaurate as a reaction catalyst, gradually dropwise adding 15-20 g of hydroxyl-terminated polydimethylsiloxane in the mechanical stirring process, keeping the temperature of 90-110 ℃, stirring for 4-6 h under the condition that the rotating speed is 300-500 r/min, stopping stirring when the temperature of the system is reduced to 50 ℃, vacuumizing, decompressing and evaporating to remove the solvent to obtain a transparent viscous liquid, namely the epoxy acrylate containing the organic silicon long chain.
4. The high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 1, wherein: the organic silicon reactive diluent is an organic silicon monomer containing a terminal acrylic acid structure.
5. The high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 1, wherein: the photoinitiator is selected from one or a mixture of any more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl benzophenone, bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide, 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-one, alpha' -dimethyl benzil ketal, isopropyl thioxanthone, benzophenone, 2,4, 6-trimethylbenzoyl benzene-diphenyl phosphine oxide and 2,4, 6-trimethylbenzoyl diphenyl phosphine oxide.
6. The high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 1, wherein: the high-transparency conductive filler is a mixture of Ag nanowires and Ag nanoparticles with high conductivity and transparency.
7. The high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to claim 6, wherein: 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-heat-resistant ultraviolet-curable conductive adhesive according to claim 6, wherein: the weight ratio of the Ag nanowires to the Ag nanoparticles is 7: 3-8: 2.
9. The preparation method of the high-toughness humidity-heat-resistant ultraviolet-curable conductive adhesive according to any one of claims 1 to 8, which is characterized by comprising the following steps:
adding 30-50 parts of self-made epoxy acrylate containing an organic silicon long chain, 10-20 parts of an organic silicon reactive diluent, 15-35 parts of an acrylic monomer, 3-8 parts of a photoinitiator, 0.05-0.2 part of a polymerization inhibitor and 1-3 parts of a silane coupling agent into a stirring kettle, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 600-1000 r/min in a vacuum and light-proof state; adding 12-25 parts of conductive filler, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 600-1000 r/min in a vacuum and light-proof state; and adding 0-5 parts of thixotropic agent, and stirring for 30min under the conditions of revolution of 30-50 r/min and rotation of 300-800 r/min in a vacuum and dark state to obtain the high-toughness humidity-heat-resistant ultraviolet-curing conductive adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110215812.8A CN112852379B (en) | 2021-02-26 | 2021-02-26 | High-toughness, heat and humidity resistant ultraviolet curing conductive adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110215812.8A CN112852379B (en) | 2021-02-26 | 2021-02-26 | High-toughness, heat and humidity resistant ultraviolet curing conductive adhesive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112852379A true CN112852379A (en) | 2021-05-28 |
| CN112852379B CN112852379B (en) | 2022-05-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115725262A (en) * | 2022-11-16 | 2023-03-03 | 广州回天新材料有限公司 | Adhesive and preparation method and application thereof |
| CN115785874A (en) * | 2022-12-20 | 2023-03-14 | 清远职业技术学院 | Light-cured epoxy acrylic resin conductive adhesive and preparation method thereof |
| CN115820201A (en) * | 2022-12-13 | 2023-03-21 | 烟台泰盛精化科技有限公司 | Ultraviolet light-moisture dual-curing adhesive and preparation method thereof |
| CN117106402A (en) * | 2023-10-19 | 2023-11-24 | 山东凯恩新材料科技有限公司 | Organic silicon composite ultraviolet curing adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057514A (en) * | 2019-12-23 | 2020-04-24 | 烟台信友新材料有限公司 | High-strength moisture-heat-resistant photocuring adhesive and preparation method thereof |
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111057514A (en) * | 2019-12-23 | 2020-04-24 | 烟台信友新材料有限公司 | High-strength moisture-heat-resistant photocuring adhesive and preparation method thereof |
| 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115725262A (en) * | 2022-11-16 | 2023-03-03 | 广州回天新材料有限公司 | Adhesive and preparation method and application thereof |
| CN115820201A (en) * | 2022-12-13 | 2023-03-21 | 烟台泰盛精化科技有限公司 | Ultraviolet light-moisture dual-curing adhesive and preparation method thereof |
| CN115785874A (en) * | 2022-12-20 | 2023-03-14 | 清远职业技术学院 | Light-cured epoxy acrylic resin conductive adhesive and preparation method thereof |
| CN117106402A (en) * | 2023-10-19 | 2023-11-24 | 山东凯恩新材料科技有限公司 | Organic silicon composite ultraviolet curing adhesive and preparation method thereof |
| CN117106402B (en) * | 2023-10-19 | 2024-01-02 | 山东凯恩新材料科技有限公司 | Organic silicon composite ultraviolet curing adhesive and preparation method thereof |
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| CN112852379B (en) | 2022-05-13 |
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