CN110964460A - Ultraviolet-cured anisotropic conductive adhesive and preparation method thereof - Google Patents
Ultraviolet-cured anisotropic 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
- 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
- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
Abstract
The invention provides an ultraviolet curing anisotropic conductive adhesive and a preparation method thereof, and relates to the technical field of materials. The ultraviolet light curing anisotropic conductive adhesive provided by the invention comprises, by weight, 10% -50% of low-melting-point metal conductive filler, 20% -88% of ultraviolet light curing resin and 1% -30% of an auxiliary agent, wherein the auxiliary agent comprises an ultraviolet light curing agent, and the melting point of the low-melting-point metal conductive filler is below 300 ℃. The technical scheme of the invention can provide the anisotropic conductive adhesive with better conductive performance and lower price.
Description
Technical Field
The invention relates to the technical field of materials, in particular to ultraviolet curing anisotropic conductive adhesive and a preparation method thereof.
Background
The anisotropic conductive adhesive is a polymer-based microelectronic interconnection material which is conductive only in the vertical direction and is non-conductive in the horizontal direction. Anisotropic conductive adhesives are widely used in electronic products such as flexible printed circuit boards and RFID tags, and have the function of electrically and mechanically fixing semiconductor elements and components to keep the opposite electrodes in conduction and the adjacent electrodes in insulation.
Anisotropic conductive adhesives are generally composed of conductive fillers, curable resins, curing agents, diluents and the like, wherein the conductive fillers are uniformly dispersed in the curable resins, and the resins are cured to form anisotropic conductive adhesives which are conductive only in the vertical direction and have high or almost no electrical resistance in the horizontal direction. At present, the conductive particles commonly used in the anisotropic conductive adhesive include metal particles such as gold, silver, copper, and nickel, inorganic particles such as graphite and carbon black, and mixed particles of metal and inorganic filler such as silver-plated glass beads, silver silicide, and silicon carbide.
However, when the conductive particles are metal particles such as gold, silver, copper, platinum, etc., the anisotropic conductive adhesive has good conductivity, but is expensive; when the conductive particles are inorganic particles such as graphite and carbon black, and mixed particles of metal such as silver-plated glass beads, silver silicide and silicon carbide and inorganic filler, the prepared anisotropic conductive adhesive has poor conductivity and limited application range, although the price is low.
Disclosure of Invention
The invention provides an ultraviolet curing anisotropic conductive adhesive and a preparation method thereof, and can provide an anisotropic conductive adhesive with better conductivity and lower price.
In a first aspect, the present invention provides an ultraviolet light cured anisotropic conductive adhesive, which adopts the following technical scheme:
the ultraviolet curing anisotropic conductive adhesive is composed of, by weight, 10% -50% of low-melting-point metal conductive filler, 20% -88% of ultraviolet curing resin and 1% -30% of an auxiliary agent, wherein the auxiliary agent comprises an ultraviolet curing agent, and the melting point of the low-melting-point metal conductive filler is below 300 ℃.
Optionally, the low-melting-point metal conductive filler includes one or more of elemental mercury, elemental gallium, elemental indium, elemental tin, elemental gallium-indium alloy, gallium-indium-tin alloy, gallium-zinc alloy, gallium-indium-zinc alloy, gallium-tin-zinc alloy, gallium-indium-tin-zinc alloy, gallium-tin-cadmium alloy, gallium-zinc-cadmium alloy, bismuth-indium alloy, bismuth-tin alloy, bismuth-indium-tin-zinc alloy, bismuth-indium-tin-lead alloy, bismuth-tin-cadmium alloy, bismuth-lead-tin alloy, bismuth-tin-cadmium alloy, tin-lead alloy, tin-copper alloy, tin-zinc-copper alloy, and tin-silver-copper alloy.
Optionally, the particle size of the low-melting-point metal conductive filler is 0.5-100 microns.
Optionally, the ultraviolet light curable resin includes one or more of epoxy resin, phenol resin, urea resin, acrylate resin, polyester acrylate resin, poly (vinyl chloride) acrylate resin, methoxy acrylate resin, epoxy acrylate resin, poly (vinyl chloride) acrylate resin, and melamine acrylate resin.
Optionally, in the ultraviolet light cured anisotropic conductive adhesive, the weight percentage of the ultraviolet light curing agent is 1% to 5%.
Optionally, the uv curing agent comprises one or more of Irgacure 127, Irgacure 184, Irgacure 250, Irgacure 320, Irgacure 369, Irgacure379, Irgacure 754, Irgacure819, Irgacure907, Irgacure1173, Irgacure 2022, Irgacure 2959, Irgacure MBF, Irgacure TPO, Irgacure819DW, uycure 160, and uycure 261.
Optionally, the auxiliary agent further comprises one or more of a solvent, a diluent, a dispersing agent, a thickening agent, a toughening agent, a filler, a drying agent, a defoaming agent, an antistatic agent, a leveling agent and an antioxidant.
In a second aspect, the invention provides a method for preparing an ultraviolet curing anisotropic conductive adhesive, which adopts the following technical scheme:
the preparation method of the ultraviolet curing anisotropic conductive adhesive comprises the following steps:
step S1, preparing low-melting-point metal conductive filler;
step S2, mixing the ultraviolet light curing resin and the auxiliary agent uniformly according to a certain proportion;
and step S3, mixing the low-melting-point metal conductive filler with the mixture of the ultraviolet curing resin and the auxiliary agent according to a certain proportion to form uniformly dispersed mixed liquid, so as to obtain the ultraviolet curing anisotropic conductive adhesive.
Alternatively, in the step S1, the low melting point metal conductive filler is prepared by one of a liquid phase stirring method, an ultrasonic dispersion method, a spraying method, and a high pressure extrusion method at a temperature higher than the melting point of the low melting point metal conductive filler.
Optionally, in the step S2, the ultraviolet curing resin and the auxiliary agent are uniformly mixed by stirring, the stirring speed is 500-3000 r/min, and the stirring time is 0.1-10 hours; in the step S3, the low-melting-point metal conductive filler is mixed with the mixture of the ultraviolet curing resin and the auxiliary agent in a stirring manner, the stirring speed is 500-3000 r/min, and the stirring time is 0.1-10 h.
The invention provides an ultraviolet light curing anisotropic conductive adhesive and a preparation method thereof, wherein the ultraviolet light curing anisotropic conductive adhesive comprises, by weight, 10% -50% of low-melting-point metal conductive filler, 20% -88% of ultraviolet light curing resin and 1% -30% of auxiliary agent, wherein the auxiliary agent comprises an ultraviolet light curing agent, the melting point of the low-melting-point metal conductive filler is below 300 ℃, because the cost of the low-melting-point metal conductive filler is far lower than that of noble metal particles such as gold particles, silver particles, copper particles, platinum particles and the like, and the conductivity far exceeds inorganic particles such as graphite particles, carbon black particles and the like, and the mixed particles of silver-plated glass beads, silver silicide, silicon carbide and other metals and inorganic fillers, therefore, the ultraviolet curing anisotropic conductive adhesive provided by the invention has the advantages of good conductive performance, low price and wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a flowchart of a method for preparing an ultraviolet light cured anisotropic conductive adhesive according to an embodiment of the present invention.
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 will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. 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.
It should be noted that the technical features in the embodiments of the present invention may be combined with each other without conflict.
The embodiment of the invention provides an ultraviolet curing anisotropic conductive adhesive, which specifically comprises, by weight, 10% -50% of a low-melting-point metal conductive filler, 20% -88% of an ultraviolet curing resin and 1% -30% of an auxiliary agent, wherein the auxiliary agent comprises an ultraviolet curing agent, and the melting point of the low-melting-point metal conductive filler is below 300 ℃.
It should be noted that, in the embodiment of the present invention, when the melting point of the low-melting-point metal conductive filler is less than or equal to room temperature, the low-melting-point metal conductive filler is low-melting-point metal conductive liquid droplets, and when the melting point of the low-melting-point metal conductive filler is higher than room temperature, the low-melting-point metal conductive filler is low-melting-point metal conductive particles.
The cost of the low-melting-point metal conductive filler is far lower than that of noble metal particles such as gold particles, silver particles, copper particles and platinum particles, and the conductivity of the low-melting-point metal conductive filler is far higher than that of inorganic particles such as super-graphite particles and carbon black particles and mixed particles of metal such as silver-plated glass beads, silver silicide and silicon carbide and the inorganic filler, so that the ultraviolet curing anisotropic conductive adhesive provided by the invention has the advantages of good conductivity, low price and wide application prospect.
The low-melting-point metal conductive filler is used for enabling the ultraviolet curing anisotropic conductive adhesive to be conductive in the vertical direction (namely the thickness direction of the conductive adhesive) and not conductive in the horizontal direction; the ultraviolet curing resin is used for curing the ultraviolet curing anisotropic conductive adhesive after ultraviolet irradiation; the specific use of the auxiliary agent varies according to the specific kind of the auxiliary agent, and the specific kind of the auxiliary agent will be exemplified in the following contents in the examples of the present invention.
If the weight percentage of one or more of the low-melting-point metal conductive filler, the ultraviolet curable resin and the auxiliary agent in the ultraviolet curable anisotropic conductive adhesive exceeds the aforementioned range, the ultraviolet curable anisotropic conductive adhesive has poor performance, such as horizontal conductivity, vertical non-conductivity, non-curing, too slow curing, non-uniformity, and the like.
For example, the ultraviolet light curable anisotropic conductive adhesive may include 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50% by weight of the low melting point metal conductive filler, 20%, 30%, 40%, 50% by weight of the ultraviolet light curable resin, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 88% by weight of the ultraviolet light curable resin, and 1%, 5%, 10%, 15%, 20%, 25%, 30% by weight of the auxiliary.
The following examples of the present invention describe the components of the ultraviolet curable anisotropic conductive adhesive in detail.
Optionally, the specific implementation manner of the low-melting-point metal in the low-melting-point metal conductive filler may be various, and in the first example, the low-melting-point metal is a simple substance with a melting point below 300 ℃; in a second example, the low melting point metal is an alloy having a melting point of 300 degrees celsius or less; in a third example, the low-melting-point metal is a conductive mixture including an element having a melting point of 300 degrees celsius or less and/or an alloy having a melting point of 300 degrees celsius or less, for example, a conductive nanofluid formed by mixing the element having a melting point of 300 degrees celsius or less with metal nanoparticles and a fluid dispersant, and when the conductive nanofluid is selected, the fluid dispersant is preferably one of ethanol, propylene glycol, glycerol, polyvinylpyrrolidone, polydimethylsiloxane, polyethylene glycol, and polymethyl methacrylate.
Further, the low-melting-point metal conductive filler comprises one or more of elemental mercury, elemental gallium, elemental indium, elemental tin, elemental gallium-indium alloy, gallium-indium-tin alloy, gallium-zinc alloy, gallium-indium-zinc alloy, gallium-tin-zinc alloy, gallium-indium-tin-zinc alloy, gallium-tin-cadmium alloy, gallium-zinc-cadmium alloy, bismuth-indium alloy, bismuth-tin alloy, bismuth-indium-tin-zinc alloy, bismuth-indium-tin-lead alloy, bismuth-tin-cadmium alloy, bismuth-lead-tin alloy, bismuth-tin-cadmium alloy, tin-lead alloy, tin-copper alloy, tin-zinc-copper alloy and tin-silver-copper alloy.
The inventors found that the particle size of the low-melting point metal conductive filler has an influence on the performance of the ultraviolet light cured anisotropic conductive adhesive, specifically, if the particle size of the low-melting point metal conductive filler is too small, the ultraviolet light cured anisotropic conductive adhesive is not conductive in the vertical direction, and if the particle size of the low-melting point metal conductive filler is too large, the ultraviolet light cured anisotropic conductive adhesive is also conductive in the horizontal direction. Therefore, the particle size of the low melting point metal conductive filler needs to be reasonably selected. Optionally, the low melting point metallic conductive filler has a particle size of 0.5 to 100 microns.
Optionally, the ultraviolet light curable resin includes one or more of epoxy resin, phenol resin, urea resin, acrylate resin, polyester acrylate resin, poly (vinyl chloride) acrylate resin, methoxy acrylate resin, epoxy acrylate resin, poly (vinyl chloride) acrylate resin, and melamine acrylate resin.
Optionally, in the ultraviolet light cured anisotropic conductive adhesive, the weight percentage of the ultraviolet light curing agent is 1% to 5%, so that the curing effect of the ultraviolet light cured resin is better.
Optionally, the uv curing agent comprises one or more of Irgacure 127, Irgacure 184, Irgacure 250, Irgacure 320, Irgacure 369, Irgacure379, Irgacure 754, Irgacure819, Irgacure907, Irgacure1173, Irgacure 2022, Irgacure 2959, Irgacure MBF, Irgacure TPO, Irgacure819DW, Uyracure160, Uyracure 261.
Optionally, the auxiliary agent further comprises one or more of a solvent, a diluent, a dispersant, a thickener, a toughening agent, a filler, a drying agent, a defoaming agent, an antistatic agent, a leveling agent and an antioxidant.
Wherein the solvent comprises one or more of water, ethanol, N-butanol, isopropanol, acetone, butanone, cyclohexanone, diethyl ether, ethyl acetate, isoamyl acetate, toluene, xylene, dichloromethane, chloroform, tetrahydrofuran, carbon tetrachloride, N-dimethylformamide, N-dimethylacetamide and dimethyl sulfoxide.
Preferably, the specific solvent is selected according to the uv curable resin. For example, the ultraviolet light curing resin is epoxy resin, and the solvent comprises one or more of acetone, xylene, n-butanol, ethyl acetate, toluene, butanone and cyclohexanone; the ultraviolet light curing resin is phenolic resin, and the solvent comprises one or more of tetrahydrofuran and ethanol; the ultraviolet light curing resin is acrylate resin, and the solvent comprises one or more of ethyl acetate, dimethylbenzene, methylbenzene, acetone and isopropanol; the ultraviolet light curing resin is acrylic resin, and the solvent comprises one or more of water, dimethylbenzene, methylbenzene and acetone; the ultraviolet light curing resin is polyvinyl chloride resin, and the solvent comprises one or more of dichloromethane, dimethylacetamide and dichloroethane; the ultraviolet light curing resin is melamine acrylate resin, and the solvent comprises N, N-dimethylacetamide; the ultraviolet light curing resin is polyester acrylate resin or polyvinyl chloride acrylate resin, and the solvent comprises one or more of toluene, xylene and dimethyl sulfoxide.
Optionally, the diluent comprises one or more of acetone, methyl ethyl ketone, cyclohexanone, benzene, toluene, xylene, n-butanol, styrene, diallyl phthalate, dioctyl phthalate, dibutyl phthalate, 616-slow dry diluent, UV-SG diluent, UV-SL diluent, UV-SB diluent, UV-SW diluent.
Optionally, the dispersant comprises one or more of water glass, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methylpentanol, cellulose derivatives, polyacrylamide, guar gum, fatty acid polyglycol ester, and vinyl bis stearamide.
Optionally, the thickener comprises one or more of bentonite, diatomaceous earth, attapulgite, molecular sieve, silica gel, methylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, sodium carboxymethylcellulose, starch, gelatin, sodium alginate, agar, polyacrylamide, polyvinyl alcohol, and polyvinylpyrrolidone.
Optionally, the toughening agent comprises one or more of liquid nitrile rubber, liquid polysulfide rubber, liquid acrylate rubber, liquid polybutadiene rubber, ethylene propylene rubber, styrene butadiene rubber, polyvinyl chloride, styrene, polyolefin, polyester, syndiotactic 1, 2-polybutadiene, chlorinated polyethylene, dimethyl diethyl ester, dibutyl dipentyl ester, triethyl phosphate, tributyl phosphate, and triphenyl phosphate.
Optionally, the filler comprises one or more of titanium dioxide, calcium carbonate, carbon black, wood flour, pottery clay, mica, silica, talcum powder, barium sulfate, boron nitride, silicon carbide, zirconia, ferroferric oxide, copper oxide and alumina.
Optionally, the desiccant comprises one or more of calcium sulfate, calcium chloride, silica gel, calcium oxide, montmorillonite, molecular sieve, attapulgite, magnesium sulfate, and potassium carbonate.
Optionally, the defoaming agent comprises one or more of polydimethylsiloxane, acrylate BZ420A, XH236, XPS-200, higher alcohol fatty acid ester SXP-110 and organic silicon x-50-60.
Optionally, the antistatic agent comprises one or more of Cyastab SP, Cyastat LS, antistatic agent SN, HZ-1, KJ-210, HKD-510.
Optionally, the leveling agent comprises one or more of dimethyl siloxane, polyether polyester modified organic siloxane, alkyl modified organic siloxane, molar chemical 1073, molar chemical 1074, molar chemical 1154, BYK-306, BYK-307, BYK-333, BYK-337 and BYK-341.
Optionally, the antioxidant comprises one or more of antioxidant 264, antioxidant 1076, antioxidant 2264, antioxidant 1010, antioxidant 4010, antioxidant H, antioxidant D and antioxidant DNP.
In addition, an embodiment of the present invention provides a method for preparing an ultraviolet light cured anisotropic conductive adhesive, specifically, as shown in fig. 1, fig. 1 is a flowchart of a method for preparing an ultraviolet light cured anisotropic conductive adhesive, which is provided by an embodiment of the present invention, and the method for preparing an ultraviolet light cured anisotropic conductive adhesive includes:
step S1, preparing low-melting-point metal conductive filler;
alternatively, in step S1, the low melting point metal conductive filler is prepared by one of a liquid phase stirring method, an ultrasonic dispersion method, a spraying method, and a high pressure extrusion method at a temperature higher than the melting point of the low melting point metal conductive filler.
In one example, Ga79In21 (melting point 16 ℃) was stirred In anhydrous ethanol for 2 hours at 1000r/min by a liquid phase stirring method to obtain conductive droplets of low melting point metal with an average particle size of about 80 microns.
In yet another example, Ga82In12Zn6 (melting point 19 ℃ C.) was stirred In petroleum ether at 1200r/min for 1 hour using a liquid phase stirring method to obtain low melting point metallic conductive droplets having an average particle size of about 50 μm.
In yet another example, Bi49In21Sn12Pb18 (melting point 60 ℃) was stirred In silicone oil at 100 ℃ for 2 hours at 1000r/min by a liquid phase stirring method to obtain low melting point metal conductive droplets having an average particle size of about 100 μm, and the low melting point metal conductive particles were obtained after cooling.
In yet another example, Ga67In20Zn13 (melting point 11 ℃ C.) was sonicated In isopropanol for 0.5h using an ultrasonic dispersion method to give low melting point metal conductive droplets having an average particle size of about 2 microns.
In yet another example, the simple substance Ga (melting point 30 ℃) is treated by ultrasonic dispersion method in absolute ethyl alcohol for 1h under the condition of 50 ℃ to obtain low-melting point metal conductive liquid drops with the average particle size of about 5 microns, and low-melting point metal conductive particles are obtained after cooling.
In yet another example, Bi54Sn26Cd20 (melting point 103 ℃) was extruded at 150 ℃ through a filter membrane having a pore size of 10 microns using a high pressure extrusion process to give low melting metal conductive particles having an average particle size of about 10 microns.
Step S2, mixing the ultraviolet light curing resin and the auxiliary agent uniformly according to a certain proportion;
optionally, in step S2, the uv curable resin and the auxiliary agent are uniformly mixed by stirring. Wherein, the faster the stirring speed, the smaller the particle size of the prepared low-melting-point metal conductive filler, and the longer the stirring time, the smaller the particle size of the prepared low-melting-point metal conductive filler, and those skilled in the art can select the stirring speed and the stirring time according to actual needs. Optionally, the stirring speed is 500-3000 r/min (e.g. 800r/min), and the stirring time is 0.1-10 h (e.g. 0.2 h). The ultrasonic mode can be assisted in the stirring process to shorten the time.
And step S3, mixing the low-melting-point metal conductive filler with a mixture of the ultraviolet curing resin and the auxiliary agent according to a certain proportion to form uniformly dispersed mixed liquid, and obtaining the ultraviolet curing anisotropic conductive adhesive.
Optionally, in step S3, the low-melting-point metal conductive filler is mixed with the mixture of the ultraviolet curable resin and the auxiliary agent by stirring, the stirring rate is 500 to 3000r/min (e.g. 800r/min), and the stirring time is 0.1 to 10 hours (e.g. 0.5 hours).
The embodiment of the invention provides an ultraviolet curing anisotropic conductive adhesive and a preparation method thereof, wherein the ultraviolet curing anisotropic conductive adhesive comprises, by weight, 10% -50% of low-melting-point metal conductive filler, 20% -88% of ultraviolet curing resin and 1% -30% of auxiliary agent, the melting point of the low-melting-point metal conductive filler is below 300 ℃, and the cost of the low-melting-point metal conductive filler is far lower than that of precious metal particles such as gold particles, silver particles, copper particles and platinum particles, and the conductivity of the low-melting-point metal conductive filler is far lower than that of inorganic particles such as super graphite particles, carbon black particles and the like, and the conductivity of silver-plated glass beads, silver silicide, silicon carbide and the like and mixed particles of the inorganic filler, so that the ultraviolet curing anisotropic conductive adhesive provided by the invention has good conductivity, low price and wide application prospect.
In addition, the ultraviolet curing anisotropic conductive adhesive also has the following advantages:
on one hand, the ultraviolet curing resin and the ultraviolet curing agent are selected, so that the ultraviolet curing anisotropic conductive adhesive can be rapidly cured at room temperature and can be used on various base materials with poor temperature resistance, the application range of the anisotropic conductive adhesive is improved, and the mounting production efficiency of electronic product components can be obviously improved;
on the other hand, the ultraviolet curing anisotropic conductive adhesive has lower contact resistance, stronger bonding strength and excellent humidity and heat resistance stability with various base materials;
on the other hand, when the melting point of the selected low-melting-point metal is lower than the room temperature, the ultraviolet curing anisotropic conductive adhesive has good fluidity at the room temperature, is applied to a flexible base material, and also has excellent properties such as bending resistance, distortion resistance, stretching resistance and the like.
The following embodiments of the present invention take a plurality of specific embodiments as examples to illustrate the ultraviolet light curing anisotropic conductive adhesive provided in the embodiments of the present invention.
Example 1
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
15 parts of low-melting-point metal conductive liquid drop
The preparation process of the ultraviolet curing anisotropic conductive adhesive comprises the following steps:
a. ultrasonically treating Ga67In20Zn13 (melting point 11 ℃) In isopropanol for 0.5h by using an ultrasonic dispersion method to obtain low-melting-point metal conductive liquid drops with the average particle size of about 2 micrometers;
b. mixing all materials except the low-melting-point metal conductive liquid drops according to a formula, and stirring at the speed of 800r/min for 1 h;
c. and (c) mixing the low-melting-point metal conductive liquid drops obtained in the step (a) with the mixture obtained in the step (b) in proportion, and stirring at the rotating speed of 800r/min for 0.5h to obtain the ultraviolet curing anisotropic conductive adhesive.
The prepared ultraviolet curing anisotropic conductive adhesive is used as an interconnection material, and a flip chip (0.6 multiplied by 0.6 mm) is packaged by a flip chip packaging technology2RFID UHF Chip) is attached to Al/coated paper (i.e. an Al antenna is printed on the coated paper), wherein the thickness of Al is 30 micrometers and the thickness of coated paper is 100 micrometers. Curing conditions are as follows: ultraviolet curing at room temperature for 5s under the pressure of 1.5 MPa. After curing, the RFID can be successfully identified. Under the conditions that the temperature is 85 ℃ and the relative humidity is 85%, the RFID can still be identified after high-temperature high-humidity aging treatment is carried out for 1000h, the contact resistance change rate before and after the ultraviolet curing anisotropic conductive adhesive aging test is 11%, and the bonding strength between the ultraviolet curing anisotropic conductive adhesive and art paper is more than 20N/cm.
Example 2
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
10 parts of low-melting-point metal conductive liquid drop
The composition of the low-melting-point metal conductive droplet is Ga79In21 (melting point 16 ℃).
Example 3
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
wherein the low-melting-point metal conductive particles contain Ga (melting point 30 ℃).
Example 4
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
the composition of the low-melting-point metal conductive particles is Bi49In21Sn12Pb18 (melting point 60 ℃).
Example 5
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
the low-melting-point metal conductive particles comprise Bi54Sn26Cd20 (melting point of 103 ℃).
Example 6
The ultraviolet curing anisotropic conductive adhesive comprises the following components in parts by mass:
the composition of the low-melting-point metal conductive droplet is Ga82In12Zn6 (melting point is 19 ℃).
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The ultraviolet curing anisotropic conductive adhesive is characterized by comprising, by weight, 10% -50% of low-melting-point metal conductive filler, 20% -88% of ultraviolet curing resin and 1% -30% of an auxiliary agent, wherein the auxiliary agent comprises an ultraviolet curing agent, and the melting point of the low-melting-point metal conductive filler is below 300 ℃.
2. The ultraviolet-curable anisotropic conductive adhesive according to claim 1, wherein the low-melting-point metal conductive filler comprises one or more of elemental mercury, elemental gallium, elemental indium, elemental tin, gallium-indium alloy, gallium-indium-tin alloy, gallium-zinc alloy, gallium-indium-zinc alloy, gallium-tin-zinc alloy, gallium-indium-tin-zinc alloy, gallium-tin-cadmium alloy, gallium-zinc-cadmium alloy, bismuth-indium alloy, bismuth-tin alloy, bismuth-indium-zinc alloy, bismuth-tin-zinc alloy, bismuth-indium-tin-lead alloy, bismuth-tin-cadmium alloy, bismuth-lead-tin alloy, tin-lead alloy, tin-copper alloy, tin-zinc alloy, tin-copper alloy, and tin-silver-copper alloy.
3. The ultraviolet curable anisotropic conductive adhesive of claim 1, wherein the particle size of the low melting point metal conductive filler is 0.5 to 100 μm.
4. The ultraviolet light curable anisotropic conductive adhesive of claim 1, wherein the ultraviolet light curable resin comprises one or more of epoxy resin, phenolic resin, urea resin, acrylate resin, acrylic resin, polyester acrylate resin, poly (vinyl chloride) acrylate resin, methoxy acrylate resin, epoxy acrylate resin, poly (vinyl chloride) acrylate resin, and melamine acrylate resin.
5. The ultraviolet light curable anisotropic conductive adhesive according to claim 1, wherein the ultraviolet light curing agent is present in an amount of 1 to 5% by weight.
6. The ultraviolet curable anisotropic conductive adhesive of claim 5, wherein the ultraviolet curing agent comprises one or more of Irgacure 127, Irgacure 184, Irgacure 250, Irgacure 320, Irgacure 369, Irgacure379, Irgacure 754, Irgacure819, Irgacure907, Irgacure1173, Irgacure 2022, Irgacure 2959, Irgacure MBF, Irgacure TPO, Irgacure819DW, Uyracure160, and Uyracure 261.
7. The ultraviolet light curable anisotropic conductive adhesive according to claim 1, wherein the auxiliary agent further comprises one or more of a solvent, a diluent, a dispersant, a thickener, a toughening agent, a filler, a drying agent, a defoaming agent, an antistatic agent, a leveling agent and an antioxidant.
8. A preparation method of ultraviolet curing anisotropic conductive adhesive is characterized by comprising the following steps:
step S1, preparing low-melting-point metal conductive filler;
step S2, mixing the ultraviolet light curing resin and the auxiliary agent uniformly according to a certain proportion;
and step S3, mixing the low-melting-point metal conductive filler with the mixture of the ultraviolet curing resin and the auxiliary agent according to a certain proportion to form uniformly dispersed mixed liquid, so as to obtain the ultraviolet curing anisotropic conductive adhesive.
9. The method of claim 8, wherein the step S1 is performed by one of liquid phase stirring, ultrasonic dispersion, spraying, and high pressure extrusion at a temperature higher than the melting point of the low melting point metal conductive filler.
10. The method for preparing the ultraviolet curing anisotropic conductive adhesive according to claim 8, wherein in the step S2, the ultraviolet curing resin and the auxiliary agent are uniformly mixed by stirring, the stirring speed is 500 to 3000r/min, and the stirring time is 0.1 to 10 hours; in the step S3, the low-melting-point metal conductive filler is mixed with the mixture of the ultraviolet curing resin and the auxiliary agent in a stirring manner, the stirring speed is 500-3000 r/min, and the stirring time is 0.1-10 h.
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| JPH05109914A (en) * | 1992-04-10 | 1993-04-30 | Nec Corp | Ultraviolet light erasing semiconductor device |
| CN104576779A (en) * | 2015-01-21 | 2015-04-29 | 黄华松 | Screen mesh array conducting film, solar cell and preparation method thereof |
| CN104910844A (en) * | 2014-03-10 | 2015-09-16 | 日立化成株式会社 | Electrically conductive adhesive composition, connection structure, solar battery module, and method for producing same |
| CN107342354A (en) * | 2017-06-28 | 2017-11-10 | 深圳市环基实业有限公司 | A kind of IC package technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05109914A (en) * | 1992-04-10 | 1993-04-30 | Nec Corp | Ultraviolet light erasing semiconductor device |
| CN104910844A (en) * | 2014-03-10 | 2015-09-16 | 日立化成株式会社 | Electrically conductive adhesive composition, connection structure, solar battery module, and method for producing same |
| CN104576779A (en) * | 2015-01-21 | 2015-04-29 | 黄华松 | Screen mesh array conducting film, solar cell and preparation method thereof |
| CN107342354A (en) * | 2017-06-28 | 2017-11-10 | 深圳市环基实业有限公司 | A kind of IC package technique |
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Application publication date: 20200407 |