CN111057485B - Hollow conductive particles for anisotropic conductive adhesive film and preparation method thereof - Google Patents

Hollow conductive particles for anisotropic conductive adhesive film and preparation method thereof Download PDF

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CN111057485B
CN111057485B CN201911415869.1A CN201911415869A CN111057485B CN 111057485 B CN111057485 B CN 111057485B CN 201911415869 A CN201911415869 A CN 201911415869A CN 111057485 B CN111057485 B CN 111057485B
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adhesive film
anisotropic conductive
conductive adhesive
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conductive particles
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CN111057485A (en
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王继宝
周翠苹
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Shenzhen Sapience Technology Co ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C08J3/122—Pulverisation by spraying
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/28—Treatment by wave energy or particle radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
    • C08J2333/12—Homopolymers or copolymers of methyl methacrylate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to the technical field of conductive gold balls, in particular to hollow conductive particles for an anisotropic conductive adhesive film and a preparation method thereof. The preparation method of the hollow conductive particles for the anisotropic conductive adhesive film comprises the following steps: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at the temperature of 300-500 ℃ to obtain the conductive metal-plated microspheres. The hollow conductive particles for the anisotropic conductive adhesive film prepared by the invention have good uniformity, are controlled to be 1-10 mu m in size, and have an error within the range of plus or minus 0.3 mu m. The anisotropic conductive adhesive film can reduce the probability of transverse conduction of the anisotropic conductive adhesive film when being used in the anisotropic conductive adhesive film, and has wide application prospect.

Description

Hollow conductive particles for anisotropic conductive adhesive film and preparation method thereof
Technical Field
The invention belongs to the technical field of conductive gold balls, and particularly relates to hollow conductive particles for an anisotropic conductive adhesive film and a preparation method thereof.
Background
The anisotropic conductive adhesive film is a green packaging material and is mainly used for replacing tin soldering to conduct interconnection between electrodes. The anisotropic conductive material is mainly formed by blending resin adhesive and conductive particles, and the conductive particles are the core part of the anisotropic conductive material. The mainstream technology for preparing the conductive particles at present is to use micron-sized polymer microspheres with uniform particle sizes as core materials and then deposit a metal conductive layer on the surface of the core materials.
Patent CN 100441613C and patent US 2008/0078977a1 both report a method for preparing conductive gold balls for anisotropic conductive adhesive films, i.e. electroless nickel plating is performed on the surface of polymer microspheres, and then electroless gold plating is performed. This method is also the most common preparation method currently in industrialization. However, both the solid metal ball and the resin ball are coated with metal by precise screening, the error of precise control to plus or minus 0.3 μm is difficult to realize, in addition, the solid metal ball is also difficult to control coating arrangement precisely due to specific gravity, the resin ball is coated with metal by crushing process, so that the small-particle-size high-density distribution cannot be realized, the requirement on the electrode pin is not realized within 10 μm, and the particle size uniformity of the conductive particles is difficult to control.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a method for preparing hollow conductive particles for an anisotropic conductive film, comprising the steps of: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at the temperature of 300-500 ℃ to obtain the conductive metal-plated microspheres.
As a preferred technical scheme, the acrylic microspheres comprise the following preparation raw materials in parts by weight: 10-20 parts of alkoxylated bisphenol A dimethacrylate, 30-50 parts of acrylic ester monomer, 1-5 parts of photoinitiator, 1-5 parts of combustion improver and 1-3 parts of additive.
As a preferred technical scheme, the alkoxylation number in the alkoxylated bisphenol A dimethacrylate is more than or equal to 4.
As a preferable technical scheme, the preparation raw material of the acrylic microsphere further comprises 30-50 parts by weight of fatty acid wax.
As a preferred technical scheme, the photoinitiator is selected from one or more of diaryl iodonium salt, triaryl sulfonium salt, alkyl sulfonium salt, iron arene salt and polyalkyl iodonium salt.
As a preferred technical scheme, the photoinitiator is polyalkyl iodonium salt.
As a preferred technical solution, the conductive metal is selected from one or more of silver, nickel and gold.
As a preferred technical scheme, the preparation method of the acrylic microsphere comprises the following steps: mixing the above raw materials at 50-60 deg.C, filtering, pressurizing, atomizing into spherical shape in a spray atomizing cavity with a nozzle at uniform speed, curing by EB electron beam radiation, dropping into 1,1,2, 2-tetrabromoethane, collecting, and oven drying.
The second aspect of the present invention provides hollow conductive particles for an anisotropic conductive adhesive film, which are prepared by the above method for preparing hollow conductive particles for an anisotropic conductive adhesive film.
As a preferable technical scheme, the particle diameter of the hollow conductive particles for the anisotropic conductive adhesive film is 1-10 μm.
Has the advantages that: the acrylic microspheres in the preparation method of the hollow conductive particles for the anisotropic conductive adhesive film have the characteristics of low specific gravity, low melting point and EB (Epstein-Barr) instant curing, and the finally prepared hollow conductive particles have good uniformity, are controlled to be 1-10 mu m and adjustable, and have an error within the range of plus or minus 0.3 mu m. The conductive film can reduce the probability of transverse conduction of the anisotropic conductive adhesive film when being used in the anisotropic conductive adhesive film, solves the problem of uniformity control of the hollow metal conductive microspheres, solves the reliability of connection of precise electrodes with the pin pitch of less than 10 mu m, and has wide application prospect.
Drawings
FIG. 1: transmission Electron Microscopy (TEM) images of the hollows.
FIG. 2: scanning Electron Microscope (SEM) image of spherical plane.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "including". As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase will render the claim closed except for the materials described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein in the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received by modifying or otherwise modifying such quantity without substantially changing the basic function to which it is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
The first aspect of the present invention provides a method for preparing hollow conductive particles for an anisotropic conductive adhesive film, comprising the steps of: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at the temperature of 300-500 ℃ to obtain the conductive metal-plated microspheres.
In a preferred embodiment, the method for preparing the hollow conductive particles for the anisotropic conductive adhesive film comprises the following steps: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at 400 ℃ to obtain the conductive metal-plated microspheres.
In a preferred embodiment, the acrylic microspheres comprise the following preparation raw materials in parts by weight: 10-20 parts of alkoxylated bisphenol A dimethacrylate, 30-50 parts of acrylic ester monomer, 1-5 parts of photoinitiator, 1-5 parts of combustion improver and 1-3 parts of additive.
In a preferred embodiment, the raw material for preparing the acrylic microspheres further comprises 30-50 parts by weight of fatty acid wax.
In one embodiment, the conductive metal is selected from one or more of silver, nickel, gold.
In one embodiment, the conductive metal is selected from one or more of pure silver, pure nickel, and pure gold.
In a preferred embodiment, the conductive metal is pure gold.
The purity of the pure gold is 99.00%.
In a preferred embodiment, the preparation method of the acrylic microspheres comprises the following steps: mixing the above raw materials at 50-60 deg.C, filtering, pressurizing, atomizing into spherical shape by uniform velocity passing through spray cavity with nozzle, curing by EB electron beam radiation, dropping into 1,1,2, 2-tetrabromoethane, collecting, and oven drying.
The specific gravity of the 1,1,2, 2-tetrabromoethane is 3.0.
Alkoxylated bisphenol A di (meth) acrylates
The alkoxylated bisphenol A di (meth) acrylate, abbreviated as BPA monomer, of the present invention is a monomer containing bisphenol A and having different degrees of ethoxylation or propoxylation.
In one embodiment, the alkoxylated bisphenol a dimethacrylate has a number of alkoxylation greater than or equal to 4.
In a preferred embodiment, the alkoxylated bisphenol a dimethacrylate has an alkoxylation number of 30.
In a most preferred embodiment, the alkoxylated bisphenol a dimethacrylate is ethoxylated bisphenol a dimethacrylate.
The ethoxylated bisphenol A dimethacrylate was purchased from Saedoma chemical Co., Ltd under the brand number SR 9036.
Fatty acid wax
The fatty acid wax of the present invention was purchased from Japan wax Korea under the trade name EP-1400.
Acrylic ester monomer
The chemical name of the acrylic is polymethyl methacrylate, and the monomer of the acrylic is methyl methacrylate.
The specific gravity of the acrylic ester monomer is 0.9.
Photoinitiator
The photoinitiator is also called photosensitizer or photocuring agent, and can generate free radicals and cations so as to initiate the polymerization of monomers, crosslinking and curing.
In one embodiment, the photoinitiator is selected from one or more of diaryliodonium salts, triarylsulfonium salts, alkylsulfonium salts, iron arene salts, and polyalkyliodonium salts.
In a preferred embodiment, the photoinitiator is a polyalkyliodonium salt.
In a most preferred embodiment, the polyalkyliodonium salt is 4, 4-didodecylbenziodonium hexafluoroantimonate.
The 4, 4-didodecylbenziodonium hexafluoroantimonate was purchased from San-Apro corporation, japan under the designation CPI-300K.
Combustion improver
The combustion improver refers to a substance which cannot be combusted per se but can generate oxygen required for combustion. The combustion improver is not strictly limited.
In a preferred embodiment, the combustion improver is a amyl nitrate.
The amyl nitrate was purchased from Shandong valley chemical Co., Ltd.
Additive agent
The additive is a substance capable of regulating and controlling interfacial tension, and the interfacial tension is required to be regulated and controlled to be 25-40 dynes/cm. The additives are not strictly limited in the present invention.
In a preferred embodiment, the additives are BYK-DYNFET 800N from BYK and ELEC ME-2 from King of Japan.
In a most preferred embodiment, the mass ratio of BYK-DYNFET 800N of BYK to ELEC ME-2 of King of Japan is 15: 1.
the second aspect of the present invention provides hollow conductive particles for an anisotropic conductive adhesive film, which are prepared by the above method for preparing hollow conductive particles for an anisotropic conductive adhesive film.
In one embodiment, the hollow conductive particles for the anisotropic conductive film have a particle size of 1 to 10 μm.
The inventor of the invention has found through long-term research that acrylic ester monomer with the melting point lower than 400 ℃ and the specific gravity of 0.9 is mixed with fatty acid wax, a certain pressure is applied to form spherical liquid drops through precision net drying spraying, then EB electron beam radiation curing is carried out in an atomizing cavity, cured microspheres fall into 1,1,2, 2-tetrabromoethane with the specific gravity of 3.0, the cured microspheres float on the surface of the 1,1,2, 2-tetrabromoethane due to small specific gravity, and then the acrylic microspheres with uniform pore diameters and errors of 0.3 mu m can be obtained after collection and blow drying.
Examples
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available, unless otherwise specified.
Example 1
Embodiment 1 provides a method for preparing hollow conductive particles for an anisotropic conductive adhesive film, including the steps of: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at 400 ℃ to obtain the conductive metal-plated microspheres.
The acrylic microsphere comprises the following preparation raw materials in parts by weight: 15 parts of alkoxylated bisphenol A dimethacrylate, 40 parts of acrylic ester monomer, 40 parts of fatty acid wax, 3 parts of photoinitiator, 3 parts of combustion improver and 2 parts of additive.
The preparation method of the acrylic microsphere comprises the following steps: mixing the above raw materials uniformly at 55 deg.C, filtering, pressurizing, passing through spray atomization cavity with nozzle at uniform speed, curing by EB electron beam radiation, dropping into 1,1,2, 2-tetrabromoethane, collecting, and oven drying.
The conductive metal is pure gold.
The alkoxylated bisphenol A dimethacrylate is ethoxylated bisphenol A dimethacrylate.
The ethoxylated bisphenol A dimethacrylate has the mark of SR 9036.
The fatty acid wax is EP-1400 from Japan wax Kogyo.
The photoinitiator is 4, 4-didodecyl phenyl iodonium hexafluoroantimonate.
The 4, 4-didodecylbenziodonium hexafluoroantimonate was purchased from San-Apro corporation under the designation CPI-300K.
The combustion improver is amyl nitrate.
The additive is BYK-DYNFET 800N and ELEC ME-2 from Japan flower king.
The mass ratio of BYK-DYNFET 800N to ELEC ME-2 of King of Japan is 15: 1.
the particle size of the hollow conductive particles for the anisotropic conductive adhesive film is 3 mu m.
Example 2
The embodiment 2 is basically the same as the embodiment 1, except that the acrylic microspheres comprise the following preparation raw materials in parts by weight: 10 parts of alkoxylated bisphenol A dimethacrylate, 30 parts of acrylic ester monomer, 30 parts of fatty acid wax, 1 part of photoinitiator, 1 part of combustion improver and 1 part of additive.
Example 3
Example 3 is substantially the same as example 1 except that the acrylic microspheres comprise the following preparation raw materials in parts by weight: 20 parts of alkoxylated bisphenol A dimethacrylate, 50 parts of acrylic ester monomer, 50 parts of fatty acid wax, 5 parts of photoinitiator, 5 parts of combustion improver and 3 parts of additive.
Comparative example 1
The comparative example 1 is basically the same as the example 1, except that the acrylic microspheres comprise the following preparation raw materials in parts by weight: 15 parts of alkoxylated bisphenol A dimethacrylate, 40 parts of acrylic acrylate monomer, 3 parts of photoinitiator, 3 parts of combustion improver and 2 parts of additive.
Comparative example 2
Comparative example 2 is essentially the same as example 1 except that: the additive is BYK-DYNFET 800N.
Evaluation of Performance
The specific gravity test method of the hollow conductive ball comprises the following steps: the liquid displacement test is generally carried out using a standard pycnometer, using a glass pycnometer having a volume of about 50mL, placing 3g of the dried hollow conductive particles obtained in the examples and comparative examples into the pycnometer, adding the displacement liquid into the bottle to a level of 10mm above the sample, placing the pycnometer in a vacuum desiccator, evacuating until no air bubbles escape from the solid, returning the pycnometer to normal pressure, filling the pycnometer with the liquid, placing the flask in a thermostatic bath, covering the flask after 1 hour, allowing the liquid to fill the capillaries in the flask, wiping the pycnometer dry, and weighing.
TABLE 1 results of the Performance test of the hollow conductive particles obtained in examples 1 to 3
Figure BDA0002351184950000081
TABLE 2 specific gravities of hollow conductive spheres of the hollow conductive particles prepared in examples and comparative examples
Figure BDA0002351184950000082

Claims (8)

1. The preparation method of the hollow conductive particles for the anisotropic conductive adhesive film is characterized by comprising the following steps of: (1) preparing acrylic microspheres; (2) coating treatment: carrying out metal coating micropore processing treatment on the surface of the acrylic microsphere to obtain a microsphere plated with conductive metal; (3) hollowing treatment: hollowing the microspheres plated with the conductive metal at the temperature of 300-500 ℃ to obtain the conductive metal-plated microspheres;
the acrylic microsphere comprises the following preparation raw materials in parts by weight: 10-20 parts of alkoxylated bisphenol A dimethacrylate, 30-50 parts of acrylic ester monomer, 1-5 parts of photoinitiator, 1-5 parts of combustion improver and 1-3 parts of additive;
the preparation method of the acrylic microsphere comprises the following steps: mixing the above raw materials at 50-60 deg.C, filtering, pressurizing, passing through spray atomization cavity with nozzle at uniform speed, curing by EB electron beam radiation, falling into 1,1,2, 2-tetrabromoethane, collecting, and oven drying.
2. The method as claimed in claim 1, wherein the number of alkoxylation in the alkoxylated bisphenol A dimethacrylate is 4 or more.
3. The method for preparing hollow conductive particles for an anisotropic conductive adhesive film according to claim 1, wherein the raw material for preparing the acryl microspheres further comprises 30 to 50 parts by weight of a fatty acid wax.
4. The method for preparing hollow conductive particles for an anisotropic conductive adhesive film according to claim 1, wherein the photoinitiator is one or more selected from diaryliodonium salts, triarylsulfonium salts, alkylsulfonium salts, iron arene salts, and polyalkyliodonium salts.
5. The method for preparing hollow conductive particles for an anisotropic conductive adhesive film according to claim 4, wherein the photoinitiator is a polyalkyliodonium salt.
6. The method for preparing hollow conductive particles for an anisotropic conductive adhesive film according to claim 1, wherein the conductive metal is selected from one or more of silver, nickel, and gold.
7. The hollow conductive particles for an anisotropic conductive adhesive film, which are prepared by the method for preparing the hollow conductive particles for an anisotropic conductive adhesive film according to any one of claims 1 to 6.
8. The hollow conductive particle for the anisotropic conductive adhesive film according to claim 7, wherein the particle diameter is 1 to 10 μm.
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