CN114883050A - Low-temperature sintering copper paste based on multi-conductive network structure filler and preparation method thereof - Google Patents
Low-temperature sintering copper paste based on multi-conductive network structure filler and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of low-temperature sintering copper paste based on multi-conductive network structure filler, which comprises the following steps: preparing MXene nanosheet dispersion; adding a dopamine solution into the MXene nanosheet dispersion liquid, stirring, centrifuging, and dispersing the prepared precipitate into deionized water to obtain a polydopamine-modified MXene nanosheet dispersion liquid; adding nano copper powder into the carbon nano tube dispersion liquid, continuing stirring, then adding the prepared poly dopamine modified MXene nanosheet dispersion liquid, performing ultrasonic treatment, and filtering to obtain a composite conductive filler; mixing and dissolving matrix resin and toughening resin in a diluent to obtain a resin solution, adding a dispersing agent, a surfactant, ethylene glycol, isopropanolamine, a curing agent and a composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry. The prepared copper paste has the advantages of low sintering temperature, good conductivity and excellent combination property with a matrix.
Description
The technical field is as follows:
the invention relates to the technical field of conductive materials, in particular to low-temperature sintered copper paste based on a multi-conductive network structure filler and a preparation method thereof.
Background art:
printed electronics is a new technology process that uses traditional printing techniques in the fabrication and production of electronic devices and systems. The printing technology simplifies the manufacturing process of electronic products, reliably connects electronic circuits and components, has small volume and light weight, meets the requirements of various shapes, and is low in cost and environment-friendly. One key technology in printed electronics manufacturing technology is the study of conductive inks. This is a material that may have certain conductive properties. With the rapid development of electronic products toward being thinner, more elaborate, more reliable and finer in recent years, higher requirements are put forward for manufacturing the electronic products.
Conductive ink is a composite material formed by mixing filler particles having conductive properties such as gold and silver with a binder, and is widely used in the production of printed wiring boards. As a functional printing material with special application, the conductive ink has different technological characteristics from other common inks. The biggest difference is that the conductive filler accounts for a high proportion of the components and plays a role in conducting electricity. The gold powder printing material, the silver paste printing material and the copper paste printing material are mainly used for printing a printed circuit, a plug, an electroplating bottom layer, a keyboard contact, a resistor and the like in the production of the printed board. The conductive ink mainly comprises a composite functional material consisting of conductive filler, a bonding agent, a coupling agent and other auxiliary agents, and has the function of transmitting current, wherein the conductive filler is a key part in the conductive ink, and the conductivity of the conductive ink depends on the conductive filler in a system. In the preparation of the conductive ink, the conductivity and the preparation cost are considered at the same time, copper powder is a conductive filler commonly used in the conductive ink, but the copper powder has poor oxidation resistance and is easy to oxidize in the air, and the copper oxide generated by oxidation is an insulating substance and can reduce the conductivity of the material, so that certain pretreatment needs to be carried out on the copper powder to improve the oxidation resistance. The existing copper powder pretreatment method is complex in operation and high in preparation cost, and the conductivity of the ink cannot be well improved.
The invention content is as follows:
the invention aims to solve the technical problem of providing low-temperature sintered copper slurry of a multi-conductive network structure filler and a preparation method thereof, aiming at the defects of the prior art, the invention adopts poly-dopamine modified MXene nanosheets and carbon nanotubes to form a double-conductive network, and then the nano copper powder is coated in the double-conductive network to obtain the filler with the multi-conductive network structure, and the prepared copper slurry has the advantages of low sintering temperature, good conductive performance and excellent combination property with a matrix.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of low-temperature sintering copper paste based on multi-conductive network structure filler comprises the following steps:
(1) mixing lithium fluoride and hydrochloric acid solution, adding into a reaction kettle, and adding Ti 3 AlC 2 Stirring and etching MAX phase materials, then repeatedly washing the powder by using deionized water until the pH value of the supernatant reaches 6, then mixing the washed powder and the deionized water, performing ultrasonic treatment, centrifuging, and collecting the supernatant to obtain MXene nanosheet dispersion liquid;
(2) adding a dopamine solution into the MXene nanosheet dispersion liquid, stirring, centrifuging, and dispersing the prepared precipitate into deionized water to obtain a polydopamine-modified MXene nanosheet dispersion liquid;
(3) ultrasonically dispersing a carbon nano tube in deionized water to prepare a carbon nano tube dispersion liquid, then adding nano copper powder, continuing stirring, then adding the prepared polydopamine-modified MXene nanosheet dispersion liquid, ultrasonically treating, and filtering to prepare a composite conductive filler;
(4) mixing and dissolving matrix resin and toughening resin in a diluent to obtain a resin solution, adding a dispersing agent, a surfactant, ethylene glycol, isopropanolamine, a curing agent and a composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
Preferably, in the step (1), the concentration of the hydrochloric acid solution is 9mol/L, and the lithium fluoride, the hydrochloric acid solution and the Ti are added 3 AlC 2 The dosage ratio of MAX phase materials is 2 g: (30-40) ml: 1 g.
Preferably, in the step (1), the time of the stirring etching treatment is 24 hours, the time of the ultrasonic treatment is 1-2 hours, the centrifugal rotation speed is 3500rpm, and the centrifugal time is 30 min.
Preferably, in the step (2), the concentration of the MXene nanosheet dispersion is 3-5mg/ml, and the concentration of the dopamine solution is 1 mg/ml; the volume ratio of the two is (12-14): 1.
in the above technical means, in the step (2), the stirring time is preferably 1 hour, the rotation speed of the centrifugal treatment is 3500rpm, and the centrifugal treatment time is preferably 10 to 20 min.
Preferably, in the step (3), the concentration of the carbon nanotube dispersion liquid is 1mg/ml, the concentration of the poly-dopamine-modified MXene nanosheet dispersion liquid is 1-2mg/ml, and the usage ratio of the carbon nanotube dispersion liquid, the nano-copper powder and the poly-dopamine-modified MXene dispersion liquid is 20 ml: 1 g: (30-50) ml.
In the above technical solution, the matrix resin is preferably an epoxy resin, and more preferably a dicyclopentadiene phenol epoxy resin DNE260 or an organosilicon modified epoxy resin.
Preferably, in the above technical solution, the toughening resin is at least one of hydroxyl-terminated polybutadiene toughening epoxy resin, polyether polyol, polyurethane modified epoxy resin, and reactive liquid nitrile rubber.
Preferably, the amount of each component is 8-10 parts by weight of matrix resin, 3-6 parts by weight of toughening resin, 5-10 parts by weight of diluent, 0.05-1 part by weight of dispersant, 0.05-1 part by weight of surfactant, 2-3 parts by weight of glycol, 2-5 parts by weight of isopropanolamine, 1-4 parts by weight of curing agent and 70-80 parts by weight of composite conductive filler.
The dispersant and the surfactant can effectively improve the compatibility of the composite conductive filler and the matrix resin to a certain extent, and further the conductive slurry with excellent stability is prepared. Further, the dispersing agent is at least one of BYK-W985, BYK-W903, BYK-W996, BYK-W980, BYK-9076, BYK-9077 and BYK-W940; the surfactant is at least one of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 3-aminopropyl triethoxy silane, titanium coupling agent and aluminum coupling agent.
The thinner is used for dissolving resin, so that the composite conductive filler can be fully dispersed in the resin solution, and the viscosity and the drying speed of the slurry can be effectively adjusted. Therefore, the diluent needs to have a too low boiling point to prevent too rapid volatilization of the diluent, which results in too great a change in the viscosity of the slurry. The selective diluent is at least one of 3,3' - (oxybis methylene) bis (3-ethyl) oxetane, 2- (oxetan-2-yl) ethyl acetate, 1, 4-butanediol diglycidyl ether, phenyl glycidyl ether, p-tert-butylphenyl glycidyl ether, neopentyl glycol diglycidyl ether and propylene glycol methyl ether acetate.
In order to ensure that the slurry can be quickly cured at low temperature, the curing agent disclosed by the invention is at least one of dicyandiamide, 4 diaminodiphenyl sulfone, 4 diaminodiphenylmethane, 4 diaminodiphenyl ether and dodecenyl succinic anhydride.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the low-temperature sintering copper paste provided by the invention comprises epoxy resin, toughening resin, a diluent, a dispersing agent, a surfactant, ethylene glycol, isopropanolamine, a curing agent and a composite conductive filler, the dosage of each component is effectively adjusted, and the prepared copper paste can realize low-temperature curing and has good stability. The composite conductive filler added in the invention is composed of poly-dopamine modified MXene nanosheets, carbon nanotubes and nano copper powder, and after the low-temperature sintered copper slurry is formed into a film and sintered, the composite conductive filler can form an effective multi-conductive network, so that the high conductivity of the material is ensured.
MXene has a two-dimensional layered structure and higher conductivity, and the MXene is subjected to in-situ modification by using polydopamine, and MXene nanosheets modified by the polydopamine are mixed with carbon nanotubes and nano-copper powder, so that the MXene nanosheets with the layered structure and the carbon nanotubes with the one-dimensional structure form a one-dimensional/two-dimensional double-conductive network, and the nano-copper powder is uniformly dispersed in the double-conductive network to form a more stable conductive bridge. The low-temperature sintered copper paste prepared by the invention has the advantages of good stability, simple preparation method and excellent conductivity.
The specific implementation mode is as follows:
in order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Example 1
S1: 2g of lithium fluoride and 30ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 MAX phase materials are stirred and etched for 24 hours, then deionized water is adopted to repeatedly wash the powder until the pH value of the supernatant reaches 6, then the washed powder and the deionized water are mixed and ultrasonically treated for 1 hour, centrifugation is carried out for 30min at 3500rpm, and the supernatant is collected to prepare MXene nanosheet dispersion liquid with the concentration of 3.5 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 25ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 10min, dispersing the prepared precipitate into deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1 mg/ml;
s3: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, then adding 30ml of the prepared polydopamine modified MXene nanosheet dispersion liquid, ultrasonically treating, and filtering to prepare the composite conductive filler;
s4: mixing 8 parts by weight of organosilicon modified epoxy resin and 5 parts by weight of hydroxyl-terminated polybutadiene toughened epoxy resin, dissolving the mixture in 6 parts by weight of 3,3' - (oxybis-methylene) bis (3-ethyl) oxetane to obtain a resin solution, adding 0.1 part by weight of BYK-W985, 0.1 part by weight of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 2 parts by weight of ethylene glycol, 3 parts by weight of isopropanolamine, 3 parts by weight of dicyandiamide and 80 parts by weight of composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper paste.
Example 2
S1: 2g of lithium fluoride and 35ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 MAX phase materials are stirred and etched for 24 hours, then deionized water is adopted to repeatedly wash the powder until the pH value of the supernatant reaches 6, then the washed powder and the deionized water are mixed and ultrasonically treated for 1 hour, centrifugation is carried out for 30min at 3500rpm, and the supernatant is collected to prepare MXene nanosheet dispersion liquid with the concentration of 3.5 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 25ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 15min, dispersing the prepared precipitate into deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1.5 mg/ml;
s3: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, then adding 35ml of the prepared polydopamine modified MXene nano sheet dispersion liquid, ultrasonically treating, and filtering to prepare the composite conductive filler;
s4: mixing and dissolving 10 parts by weight of organic silicon modified epoxy resin and 4 parts by weight of polyurethane modified epoxy resin in 10 parts by weight of 1, 4-butanediol diglycidyl ether to obtain a resin solution, adding 0.12 part by weight of BYK-W903, 0.15 part by weight of 3-aminopropyltriethoxysilane, 2 parts by weight of ethylene glycol, 3 parts by weight of isopropanolamine, 3 parts by weight of 4, 4-diaminodiphenyl sulfone and 75 parts by weight of composite conductive filler into the resin solution, stirring, grinding and filtering to obtain the low-temperature sintered copper slurry.
Example 3
S1: 2g of lithium fluoride and 35ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 MAX phase materials are stirred and etched for 24 hours, then deionized water is adopted to repeatedly wash the powder until the pH value of the supernatant reaches 6, then the washed powder and the deionized water are mixed and subjected to ultrasonic treatment for 1 hour, centrifugation is carried out for 30min at 3500rpm, and the supernatant is collected to prepare MXene nanosheet dispersion liquid with the concentration of 4 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 24ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 10min, dispersing the prepared precipitate in deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1.5 mg/ml;
s3: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, then adding 35ml of the prepared polydopamine modified MXene nano sheet dispersion liquid, ultrasonically treating, and filtering to prepare the composite conductive filler;
s4: mixing 8 parts by weight of organic silicon modified epoxy resin and 4 parts by weight of reactive liquid nitrile rubber, dissolving the mixture in 8 parts by weight of phenyl glycidyl ether to obtain a resin solution, adding 0.08 part of BYK-W996, 0.08 part of titanium coupling agent, 2 parts of ethylene glycol, 3 parts of isopropanolamine, 2 parts of 4,4 diaminodiphenylmethane and 78 parts of composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
Example 4
S1: 2g of lithium fluoride and 30ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 Stirring and etching MAX phase materials for 24 hours, then repeatedly washing the powder by using deionized water until the pH value of the supernatant reaches 6, then mixing the washed powder and the deionized water, performing ultrasonic treatment for 1 hour, centrifuging at 3500rpm for 30min, and collecting the supernatant to prepare MXene nanosheet dispersion liquid with the concentration of 3 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 28ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 10min, dispersing the prepared precipitate into deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1 mg/ml;
s3: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, then adding 40ml of the prepared polydopamine modified MXene nano sheet dispersion liquid, ultrasonically treating, and filtering to prepare the composite conductive filler;
s4: mixing and dissolving 9 parts by weight of organic silicon modified epoxy resin and 4 parts by weight of polyurethane modified epoxy resin in 8 parts by weight of p-tert-butylphenyl glycidyl ether to obtain a resin solution, adding 0.15 part by weight of BYK-W980, 0.15 part by weight of an aluminum coupling agent, 3 parts by weight of ethylene glycol, 5 parts by weight of isopropanolamine, 3 parts by weight of 4, 4-diaminodiphenyl ether and 80 parts by weight of a composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
Example 5
S1: 2g of lithium fluoride and 35ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 Stirring and etching MAX phase materials for 24 hours, then repeatedly washing the powder by using deionized water until the pH value of the supernatant reaches 6, then mixing the washed powder and the deionized water, performing ultrasonic treatment for 1 hour, centrifuging at 3500rpm for 30min, and collecting the supernatant to prepare MXene nanosheet dispersion liquid with the concentration of 4 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 25ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 10min, dispersing the prepared precipitate into deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1 mg/ml;
s3: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, then adding 40ml of the prepared polydopamine modified MXene nano sheet dispersion liquid, ultrasonically treating, and filtering to prepare the composite conductive filler;
s4: mixing and dissolving 10 parts by weight of organic silicon modified epoxy resin and 5 parts by weight of polyurethane modified epoxy resin in 6 parts by weight of neopentyl glycol diglycidyl ether to obtain a resin solution, adding 0.1 part of BYK-W980, 0.1 part of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 2 parts of ethylene glycol, 3 parts of isopropanolamine, 1 part of dodecenyl succinic anhydride and 80 parts of composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
Comparative example 1
Mixing and dissolving 10 parts by weight of organic silicon modified epoxy resin and 5 parts by weight of polyurethane modified epoxy resin in 6 parts by weight of neopentyl glycol diglycidyl ether to obtain a resin solution, adding 0.1 part of BYK-W980, 0.1 part of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 2 parts of ethylene glycol, 3 parts of isopropanolamine, 1 part of dodecenyl succinic anhydride and 80 parts of nano copper powder into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
Comparative example 2
S1: 2g of lithium fluoride and 35ml of 9mol/L hydrochloric acid solution are mixed and added into a reaction kettle, and then 1g of Ti is added 3 AlC 2 Stirring and etching MAX phase materials for 24 hours, then repeatedly washing the powder by using deionized water until the pH value of the supernatant reaches 6, then mixing the washed powder and the deionized water, performing ultrasonic treatment for 1 hour, centrifuging at 3500rpm for 30min, and collecting the supernatant to prepare MXene nanosheet dispersion liquid with the concentration of 4 mg/ml;
s2: adding 2ml of dopamine solution with the concentration of 1mg/ml into 25ml of MXene nanosheet dispersion liquid, stirring for 1h, then centrifuging at the rotating speed of 3500rpm for 10min, dispersing the prepared precipitate into deionized water, and preparing the MXene nanosheet dispersion liquid modified by polydopamine with the concentration of 1 mg/ml;
s3: carrying out ultrasonic treatment on 1g of nano copper powder and 40ml of the prepared polydopamine modified MXene nanosheet dispersion liquid, and filtering to obtain a composite conductive filler;
s4: mixing and dissolving 10 parts by weight of organic silicon modified epoxy resin and 5 parts by weight of polyurethane modified epoxy resin in 6 parts by weight of neopentyl glycol diglycidyl ether to obtain a resin solution, adding 0.1 part of BYK-W980, 0.1 part of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 2 parts of ethylene glycol, 3 parts of isopropanolamine, 1 part of dodecenyl succinic anhydride and 80 parts of composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
The copper pastes prepared in the above examples and comparative examples were printed on the surface of a polyimide film substrate having a thickness of 12 μm in the form of lines having a width of 2mm and a thickness of 12 μm by a gravure press, and then subjected to a sintering process at 200 c, and the sintered materials were subjected to performance tests, the results of which are shown in table 1.
Comparative example 3
S1: ultrasonically dispersing 20mg of carbon nano tube in 20ml of deionized water to prepare 1mg/ml carbon nano tube dispersion liquid, then adding 1g of nano copper powder, continuing stirring, and filtering to prepare the composite conductive filler;
s2: mixing and dissolving 10 parts by weight of organic silicon modified epoxy resin and 5 parts by weight of polyurethane modified epoxy resin in 6 parts by weight of neopentyl glycol diglycidyl ether to obtain a resin solution, adding 0.1 part of BYK-W980, 0.1 part of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 2 parts of ethylene glycol, 3 parts of isopropanolamine, 1 part of dodecenyl succinic anhydride and 80 parts of composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
TABLE 1
The test results show that the prepared copper paste has excellent conductivity, compared with comparative examples 1-3, the composite conductive filler is prepared by compounding the MXene nanosheets modified by polydopamine, the carbon nanotubes and copper powder, the MXene nanosheets and the carbon nanotubes can form a one-dimensional/two-dimensional double-conductive network under the adhesion of the polydopamine, the copper nanoparticles enter the conductive network, and a stable conductive bridge is formed after sintering, so that the electrical resistivity is small, and the bonding performance with a matrix is good.
Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Claims (10)
1. A preparation method of low-temperature sintering copper paste based on multi-conductive network structure filler is characterized by comprising the following steps:
(1) mixing lithium fluoride and hydrochloric acid solution, adding into a reaction kettle, and adding Ti 3 AlC 2 MAX phase materials are stirred and etched, then deionized water is used for repeatedly washing the powder until the pH value of the supernatant reaches 6, then the washed powder and the deionized water are mixed and subjected to ultrasonic treatment, centrifugation is carried out, and the supernatant is collected, so that MXene nanosheet dispersion liquid is prepared;
(2) adding a dopamine solution into the MXene nanosheet dispersion liquid, stirring, centrifuging, and dispersing the prepared precipitate into deionized water to obtain a polydopamine-modified MXene nanosheet dispersion liquid;
(3) ultrasonically dispersing a carbon nano tube in deionized water to prepare a carbon nano tube dispersion liquid, then adding nano copper powder, continuing stirring, then adding the prepared polydopamine-modified MXene nanosheet dispersion liquid, ultrasonically treating, and filtering to prepare a composite conductive filler;
(4) mixing and dissolving matrix resin and toughening resin in a diluent to obtain a resin solution, adding a dispersing agent, a surfactant, ethylene glycol, isopropanolamine, a curing agent and a composite conductive filler into the resin solution, stirring, grinding, and filtering to obtain the low-temperature sintered copper slurry.
2. The method for preparing the low-temperature sintering copper paste based on the multi-conductive-network-structure filler according to claim 1, wherein in the step (1), the concentration of the hydrochloric acid solution is 9mol/L, and the lithium fluoride, the hydrochloric acid solution and the Ti are mixed together 3 AlC 2 The dosage ratio of MAX phase materials is 2 g: (30-40) ml: 1g of the total weight of the composition.
3. The method for preparing the low-temperature sintered copper paste based on the multi-conductive-network-structure filler according to claim 1, wherein in the step (1), the stirring etching treatment time is 24 hours, the ultrasonic treatment time is 1-2 hours, the centrifugal rotation speed is 3500rpm, and the centrifugal time is 30 min.
4. The method for preparing the low-temperature sintered copper paste based on the multi-conductive-network-structure filler, according to claim 1, is characterized in that in the step (2), the concentration of the MXene nanosheet dispersion is 3-5mg/ml, and the concentration of the dopamine solution is 1 mg/ml; the volume ratio of the two is (12-14): 1.
5. the method for preparing the low-temperature sintered copper paste based on the multi-conductive-network-structure filler according to claim 1, wherein in the step (2), the stirring treatment time is 1h, the centrifugal treatment rotating speed is 3500rpm, and the centrifugal treatment time is 10-20 min.
6. The method for preparing the low-temperature sintered copper paste based on the multi-conductive-network-structure filler, according to claim 1, wherein in the step (3), the concentration of the carbon nanotube dispersion liquid is 1mg/ml, the concentration of the poly-dopamine-modified MXene nanosheet dispersion liquid is 1-2mg/ml, and the usage ratio of the carbon nanotube dispersion liquid, the nano-copper powder and the poly-dopamine-modified MXene dispersion liquid is 20 ml: 1 g: (30-50) ml.
7. The method for preparing the low-temperature sintering copper paste based on the multi-conductive-network-structure filler, according to claim 1, wherein in the step (4), the matrix resin is epoxy resin.
8. The method for preparing the low-temperature sintered copper paste based on the multi-conductive-network-structure filler according to claim 1, wherein in the step (4), the toughening resin is at least one of hydroxyl-terminated polybutadiene toughening epoxy resin, polyether polyol, polyurethane modified epoxy resin and reactive liquid nitrile rubber.
9. The method for preparing the low-temperature sintering copper paste based on the multi-conductive-network-structure filler according to claim 1, wherein in the step (4), the amounts of the components are, by weight, 8-10 parts of the matrix resin, 3-6 parts of the toughening resin, 5-10 parts of the diluent, 0.05-1 part of the dispersant, 0.05-1 part of the surfactant, 2-3 parts of the ethylene glycol, 2-5 parts of the isopropanolamine, 1-4 parts of the curing agent and 70-80 parts of the composite conductive filler.
10. A low temperature sintered copper paste based on a multi-conductive network structured filler, characterized by being prepared by the method of any one of claims 1 to 9.
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| CN117964993A (en) * | 2024-03-28 | 2024-05-03 | 会通新材料股份有限公司 | ABS resin reinforcing additive, ABS resin material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117964993A (en) * | 2024-03-28 | 2024-05-03 | 会通新材料股份有限公司 | ABS resin reinforcing additive, ABS resin material and preparation method thereof |
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