WO2017199987A1 - 導電性粒子、導電材料及び接続構造体 - Google Patents

導電性粒子、導電材料及び接続構造体 Download PDF

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Publication number
WO2017199987A1
WO2017199987A1 PCT/JP2017/018462 JP2017018462W WO2017199987A1 WO 2017199987 A1 WO2017199987 A1 WO 2017199987A1 JP 2017018462 W JP2017018462 W JP 2017018462W WO 2017199987 A1 WO2017199987 A1 WO 2017199987A1
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WO
WIPO (PCT)
Prior art keywords
conductive
particles
particle
insulating
compression
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PCT/JP2017/018462
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English (en)
French (fr)
Japanese (ja)
Inventor
仁志 山際
茂雄 真原
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積水化学工業株式会社
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Filing date
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Application filed by 積水化学工業株式会社 filed Critical 積水化学工業株式会社
Priority to JP2017531411A priority Critical patent/JP7028641B2/ja
Priority to CN201780017468.3A priority patent/CN108780677B/zh
Priority to KR1020187014628A priority patent/KR102398998B1/ko
Publication of WO2017199987A1 publication Critical patent/WO2017199987A1/ja
Priority to JP2021192833A priority patent/JP7381547B2/ja

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R11/00—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts
    • H01R11/01—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts characterised by the form or arrangement of the conductive interconnection between the connecting locations
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R43/00—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors

Definitions

  • an anisotropic conductive material containing conductive particles is disposed on the glass substrate.
  • the semiconductor chips are stacked, and heated and pressurized.
  • the anisotropic conductive material is cured, and the electrodes are electrically connected via the conductive particles to obtain a connection structure.
  • thermocompression bonding at a low temperature is increasing in the production of this connection structure.
  • the connection resistance may increase and the conduction reliability may decrease.
  • An object of the present invention is to provide conductive particles that can be conductively connected at a relatively low temperature and that can improve conduction reliability even when the conductive connection is made at a relatively low temperature.
  • a conductive particle main body having a conductive part and insulating particles disposed on a surface of the conductive particle main body, the conductive particle main body being outside the conductive part.
  • a plurality of protrusions on the surface, the glass transition temperature of the insulating particles is less than 100 ° C.
  • the insulating particles satisfy at least one compression condition of a temperature of 100 ° C. to 160 ° C. and a pressure of 60 MPa to 80 MPa.
  • the maximum particle diameter in the compression direction of the insulating particles after compression is relative to the maximum value of the particle diameter in the direction orthogonal to the compression direction of the insulating particles after compression.
  • Conductive particles are provided that are deformable such that the ratio is 0.7 or less.
  • a plurality of the insulating particles are arranged on the surface of the conductive particle main body.
  • the ratio of the average particle diameter of the insulating particles to the average height of the protrusions exceeds 0.5.
  • the insulating particles are compressed when compressed under at least one compression condition that satisfies a compression condition of a temperature of 100 ° C. to 160 ° C. and a pressure of 60 MPa to 80 MPa.
  • the maximum value of the particle diameter in the compression direction of the subsequent insulating particles can be deformed so as to be equal to or less than the average height of the protrusions before compression.
  • the viscosity of the conductive material at 100 ° C. is 1000 Pa ⁇ s or more and 5000 Pa ⁇ s or less.
  • a first connection target member having a first electrode on the surface
  • a second connection target member having a second electrode on the surface
  • the first connection target member A connection part connecting the second connection target member, the material of the connection part is the conductive particles described above, or a conductive material containing the conductive particles and a binder resin
  • a connection structure is provided in which the first electrode and the second electrode are electrically connected by the conductive particle body in the conductive particle.
  • the conductive particles described above are provided between the first connection target member having the first electrode on the surface and the second connection target member having the second electrode on the surface. Or a step of arranging a conductive material including the conductive particles and a binder resin, and a step of conducting a conductive connection by thermocompression bonding at a glass transition temperature of the insulating particles to 160 ° C. or lower. A method for manufacturing a connection structure is provided.
  • thermocompression bonding is performed at a temperature not lower than the glass transition temperature of the insulating particles and not higher than 120 ° C.
  • FIG. 1 is a cross-sectional view showing conductive particles according to the first embodiment of the present invention.
  • FIG. 2 is a cross-sectional view showing conductive particles according to the second embodiment of the present invention.
  • FIG. 3 is a cross-sectional view showing conductive particles according to the third embodiment of the present invention.
  • FIG. 4 is a cross-sectional view showing conductive particles when the insulating portion is an insulating layer.
  • FIG. 5 is a cross-sectional view schematically showing a connection structure using the conductive particles shown in FIG.
  • the electroconductive particle which concerns on this invention is equipped with an electroconductive particle main body and an insulation part.
  • the conductive particle body has a conductive portion.
  • the insulating part is disposed on the surface of the conductive particle body.
  • the conductive particle body has a plurality of protrusions on the outer surface of the conductive part.
  • the glass transition temperature of the said insulating part is less than 100 degreeC.
  • the insulating portion is an insulating particle. In the conductive particles according to the present invention, when the insulating particles are compressed under at least one compression condition that satisfies a compression condition of a temperature of 100 ° C.
  • the conductive particle body has a plurality of protrusions on the outer surface of the conductive part.
  • the glass transition temperature of the insulating part is less than 100 ° C.
  • the reason for this is considered to be that when the temperature during thermocompression bonding is equal to or lower than the glass transition temperature of the insulating portion, the insulating portion is not easily softened, and thus the insulating portion is difficult to come off from the conductive particle body.
  • the insulating part may be a single layer or a multilayer, and other than the insulating particles disposed on the surface of the insulating particle body, Insulating particles may be arranged.
  • the average height of the protrusions is preferably 0.001 ⁇ m or more, more preferably 0.05 ⁇ m or more, preferably 0.9 ⁇ m or less, more preferably 0.2 ⁇ m or less.
  • the connection resistance is effectively reduced.
  • the insulating particles have at least one compression condition that satisfies a compression condition of a temperature of 100 ° C. to 160 ° C. and a pressure of 60 MPa to 80 MPa (preferably a temperature of 100 ° C. to 120 ° C.
  • the maximum value (L1) of the particle diameter in the compression direction (for example, the vertical direction) of the insulating particles after compression The insulating particle can be deformed such that the ratio (L1 / L2) to the maximum value (L2) of the particle diameter in a direction (eg, horizontal direction) orthogonal to the compression direction of the insulating particles is 0.7 or less.
  • the insulating particles satisfy at least one compression condition (preferably a temperature of 100 ° C. to 120 ° C. and a pressure of 100 ° C. to 160 ° C. and a pressure of 60 MPa to 80 MPa).
  • the temperature at which the insulating particles are compressed is preferably 100 ° C or higher, preferably 160 ° C or lower, more preferably 150 ° C or lower, still more preferably 140 ° C or lower, and particularly preferably 120 ° C or lower.
  • the pressure when compressing the insulating particles is preferably 60 MPa or more, preferably 80 MPa or less, more preferably 70 MPa or less.
  • the conductive portion 12 and the conductive portion 12A are different.
  • the conductive part 12A as a whole has a first conductive part 12AA on the base particle 11 side and a second conductive part 12AB on the opposite side to the base particle 11 side.
  • the conductive part 12 having a single layer structure is formed, whereas in the conductive particle 1 ⁇ / b> A, the conductive part 12 ⁇ / b> A having a two-layer structure having the first conductive part 12 ⁇ / b> AA and the second conductive part 12 ⁇ / b> AB. Is formed.
  • the first conductive portion 12AA and the second conductive portion 12AB are formed as separate conductive portions.
  • the conductive particles 1C tend to have lower conduction reliability than the conductive particles 1, 1A, 1B.
  • the material for the organic core includes the material for the resin particles described above.
  • the inorganic materials mentioned as the material for the base material particles described above can be used.
  • the material of the inorganic shell is preferably silica.
  • the inorganic shell is preferably formed on the surface of the core by forming a metal alkoxide into a shell-like material by a sol-gel method and then firing the shell-like material.
  • the metal alkoxide is preferably a silane alkoxide.
  • the inorganic shell is preferably formed of a silane alkoxide.
  • hydroxyl groups are present on the surface of the conductive part due to oxidation.
  • a hydroxyl group exists on the surface of a conductive portion formed of nickel by oxidation.
  • An insulating part can be arrange
  • the core material include barium titanate (Mohs hardness 4.5), nickel (Mohs hardness 5), silica (silicon dioxide, Mohs hardness 6-7), titanium oxide (Mohs hardness 7), zirconia. (Mohs hardness 8-9), alumina (Mohs hardness 9), tungsten carbide (Mohs hardness 9), diamond (Mohs hardness 10), and the like.
  • the inorganic particles are preferably nickel, silica, titanium oxide, zirconia, alumina, tungsten carbide or diamond, more preferably silica, titanium oxide, zirconia, alumina, tungsten carbide or diamond, titanium oxide, zirconia.
  • Alumina, tungsten carbide or diamond is more preferable, and zirconia, alumina, tungsten carbide or diamond is particularly preferable.
  • the Mohs hardness of the material of the core substance is preferably 4 or more, more preferably 5 or more, still more preferably 6 or more, still more preferably 7 or more, and particularly preferably 7.5 or more.
  • the shape of the core substance is not particularly limited.
  • the shape of the core substance is preferably a lump.
  • Examples of the core substance include a particulate lump, an agglomerate in which a plurality of fine particles are aggregated, and an irregular lump.
  • the insulating portion is an insulating particle.
  • the material for the insulating part include polyolefin compounds, (meth) acrylate polymers, (meth) acrylate copolymers, block polymers, thermoplastic resins, cross-linked thermoplastic resins, thermosetting resins, and water-soluble resins. Can be mentioned. Only 1 type may be used for the material of the said insulation part, and 2 or more types may be used together.
  • thermosetting resin an epoxy resin, a phenol resin, a melamine resin, etc.
  • crosslinking of the thermoplastic resin include introduction of polyethylene glycol methacrylate, alkoxylated trimethylolpropane methacrylate, alkoxylated pentaerythritol methacrylate and the like.
  • water-soluble resin include polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyvinyl pyrrolidone, polyethylene oxide, and methyl cellulose.
  • chain transfer agent for adjustment of a polymerization degree. Examples of the chain transfer agent include thiol and carbon tetrachloride.
  • the material of the insulating part is appropriately selected so that the glass transition temperature of the insulating part is less than 100 ° C.
  • the surface of the conductive part and the surface of the insulating part may each be coated with a compound having a reactive functional group.
  • the surface of the conductive portion and the surface of the insulating portion may not be directly chemically bonded, but may be indirectly chemically bonded by a compound having a reactive functional group.
  • the carboxyl group may be chemically bonded to a functional group on the surface of the insulating part via a polymer electrolyte such as polyethyleneimine.
  • the binder resin is not particularly limited.
  • the binder resin a known insulating resin is used.
  • the binder resin preferably includes a thermoplastic component (thermoplastic compound) or a curable component, and more preferably includes a curable component.
  • the curable component include a photocurable component and a thermosetting component. It is preferable that the said photocurable component contains a photocurable compound and a photoinitiator.
  • the thermosetting component preferably contains a thermosetting compound and a thermosetting agent.
  • binder resin examples include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers.
  • vinyl resins examples include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers.
  • the said binder resin only 1 type may be used and 2 or more types may be used together.
  • Examples of the vinyl resin include vinyl acetate resin, acrylic resin, and styrene resin.
  • examples of the thermoplastic resin include polyolefin resin, ethylene-vinyl acetate copolymer, and polyamide resin.
  • examples of the curable resin include an epoxy resin, a urethane resin, a polyimide resin, and an unsaturated polyester resin.
  • the curable resin may be a room temperature curable resin, a thermosetting resin, a photocurable resin, or a moisture curable resin.
  • the curable resin may be used in combination with a curing agent.
  • the viscosity of the conductive material at 100 ° C. is preferably 1000 Pa ⁇ s or more, more preferably 2000 Pa ⁇ s or more. From the viewpoint of further increasing the insulation reliability, the viscosity of the conductive material at 100 ° C. is preferably 5000 Pa ⁇ s or less, more preferably 4000 Pa ⁇ s or less.
  • the viscosity can be measured using, for example, an E-type viscometer (“TVE22L” manufactured by Toki Sangyo Co., Ltd.) and the like at 100 ° C. and 5 rpm.
  • E-type viscometer (“TVE22L” manufactured by Toki Sangyo Co., Ltd.) and the like at 100 ° C. and 5 rpm.
  • connection structure includes a first connection object member, a second connection object member, and a connection part connecting the first and second connection object members, and the material of the connection part is the above-described material.
  • the conductive material is preferably a conductive material containing the conductive particles and the binder resin described above. It is preferable that the connection part is formed of the above-described conductive particles or a conductive material containing the above-described conductive particles and a binder resin. In the case where conductive particles are used, the connection portion itself is conductive particles.
  • the first connection object member preferably has a first electrode on the surface.
  • the second connection target member preferably has a second electrode on the surface. It is preferable that the first electrode and the second electrode are electrically connected by the conductive particle body in the conductive particle.
  • connection structure is formed by thermocompression bonding with the step of arranging the conductive particles or the conductive material between the first connection target member and the second connection target member. It can be obtained through a conductive connection step. It is preferable to heat to the glass transition temperature or higher of the insulating portion at the thermocompression bonding.
  • FIG. 5 is a cross-sectional view schematically showing a connection structure using the conductive particles shown in FIG.
  • connection structure 51 shown in FIG. 5 includes a first connection target member 52, a second connection target member 53, and a connection portion 54 connecting the first and second connection target members 52 and 53.
  • the connection part 54 is formed of a conductive material including the conductive particles 1. It is preferable that the conductive material has thermosetting properties and the connection portion 54 is formed by thermosetting the conductive material.
  • the conductive particles 1 are schematically shown for convenience of illustration. Instead of the conductive particles 1, conductive particles 1A and 1B may be used.
  • the manufacturing method of the connection structure is not particularly limited.
  • the conductive material is disposed between the first connection target member and the second connection target member to obtain a laminate, and then the laminate is heated and pressurized. Methods and the like.
  • the pressure for the thermocompression bonding is preferably 40 MPa or more, more preferably 60 MPa or more, preferably 90 MPa or less, more preferably 70 MPa or less.
  • the heating temperature of the thermocompression bonding is preferably 80 ° C. or higher, more preferably 100 ° C. or higher, preferably 140 ° C. or lower, more preferably 120 ° C. or lower.
  • connection target member examples include electronic components such as semiconductor chips, capacitors, and diodes, and electronic components such as printed boards, flexible printed boards, glass epoxy boards, and glass boards.
  • the connection target member is preferably an electronic component.
  • the conductive particles are preferably used for electrical connection of electrodes in an electronic component.
  • a nickel plating solution (pH 8.5) containing 0.35 mol / L of nickel sulfate, 1.38 mol / L of dimethylamine borane and 0.5 mol / L of sodium citrate was prepared.
  • the nickel plating solution was gradually dropped into the suspension to perform electroless nickel plating. Thereafter, the suspension is filtered to remove the particles, washed with water, and dried to dispose a nickel-boron conductive layer (thickness 0.15 ⁇ m) on the surface of the base particle A, and the surface is a conductive layer. Conductive particles A were obtained. Of the total surface area of 100% of the outer surface of the conductive part, the surface area of the portion with protrusions was 70%.
  • the obtained anisotropic conductive paste was applied on the transparent glass substrate so as to have a thickness of 30 ⁇ m to form an anisotropic conductive paste layer.
  • the semiconductor chip was stacked on the anisotropic conductive paste layer so that the electrodes face each other.
  • a pressure heating head is placed on the upper surface of the semiconductor chip, and a pressure of 60 MPa is applied to form the anisotropic conductive paste layer. It hardened
  • the connection structure was obtained by changing the temperature and pressure during the production of the connection structure as shown in Table 1 below.
  • Example 3 Except that tridecyl methacrylate used in the production of the insulating particles was changed to dodecyl methacrylate and that the average particle size of the insulating particles was set as shown in Table 1 below, the same as in Example 1. Then, conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and connection structure were obtained.
  • Example 5 Except that the tridecyl methacrylate used in the production of the insulating particles was changed to amyl methacrylate and that the average particle size of the insulating particles was set as shown in Table 1 below, the same as in Example 1. Then, conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and connection structure were obtained.
  • Example 6 Conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and anisotropic conductive paste were used in the same manner as in Example 1 except that the average particle size of the alumina particle slurry used for preparing the conductive particles was changed to 102 nm. A connection structure was obtained.
  • Example 9 Conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and connection structure were obtained in the same manner as in Example 1 except that the average particle size of the insulating particles was changed to 156 nm.
  • Example 10 Conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and connection structure were obtained in the same manner as in Example 1 except that the average particle size of the insulating particles was changed to 511 nm.
  • Example 11 Conductive particles in the same manner as in Example 1 except that the average particle diameter of the base particle A was changed to 10 ⁇ m and the average particle diameter of the insulating particles was set as shown in Table 2 below. (Conductive particles with insulating particles), anisotropic conductive paste and connection structure were obtained.
  • Example 14 The average particle size of the base particle A was changed to 20 ⁇ m, the alumina particle slurry used for producing the conductive particles was changed to the average particle size of the nickel particle slurry, 461 nm, and the average particle size of the insulating particles was changed to Except having set as shown in following Table 2, it carried out similarly to Example 1, and obtained electroconductive particle (electroconductive particle with an insulating particle), anisotropic conductive paste, and the connection structure.
  • Example 1 The same as in Example 1 except that all the methacrylic acid esters used in the production of the insulating particles were changed to methyl methacrylate and the average particle size of the insulating particles was set as shown in Table 2 below. Thus, conductive particles (conductive particles with insulating particles), anisotropic conductive paste, and connection structure were obtained.
  • Example 4 The average particle diameter of the base particle A was changed to 10 ⁇ m, the alumina particle slurry was not used when producing the conductive particles, and the average particle diameter of the insulating particles was set as shown in Table 2 below. Except that, conductive particles (conductive particles with insulating particles), an anisotropic conductive paste, and a connection structure were obtained in the same manner as Example 1.
  • Viscosity of conductive material anisotropic conductive paste
  • E-type viscometer (“TVE22L” manufactured by Toki Sangyo Co., Ltd.)
  • the viscosity of the anisotropic conductive paste was measured under the conditions of 100 ° C. and 5 rpm. .
  • ⁇ The ratio of the number of connection structures having a resistance value of 10 8 ⁇ or more is 80% or more.
  • ⁇ The ratio of the number of connection structures having a resistance value of 10 8 ⁇ or more is 70% or more and less than 80%.
  • the ratio of the number of connection structures having a value of 10 8 ⁇ or more is 60% or more and less than 70% ⁇ : The ratio of the number of connection structures having a resistance value of 10 8 ⁇ or more is less than 60%

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Thermal Sciences (AREA)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)
  • Multi-Conductor Connections (AREA)
  • Connections Effected By Soldering, Adhesion, Or Permanent Deformation (AREA)
PCT/JP2017/018462 2016-05-19 2017-05-17 導電性粒子、導電材料及び接続構造体 WO2017199987A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2017531411A JP7028641B2 (ja) 2016-05-19 2017-05-17 導電材料及び接続構造体
CN201780017468.3A CN108780677B (zh) 2016-05-19 2017-05-17 导电性粒子、导电材料以及连接结构体
KR1020187014628A KR102398998B1 (ko) 2016-05-19 2017-05-17 도전성 입자, 도전 재료 및 접속 구조체
JP2021192833A JP7381547B2 (ja) 2016-05-19 2021-11-29 導電性粒子、導電材料及び接続構造体

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JP2016-100595 2016-05-19
JP2016100595 2016-05-19

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JP (2) JP7028641B2 (zh)
KR (1) KR102398998B1 (zh)
CN (1) CN108780677B (zh)
TW (1) TWI774675B (zh)
WO (1) WO2017199987A1 (zh)

Cited By (1)

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CN111902884A (zh) * 2018-04-04 2020-11-06 积水化学工业株式会社 带有绝缘性粒子的导电性粒子、带有绝缘性粒子的导电性粒子的制造方法、导电材料以及连接结构体

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