WO2007083673A1 - Composition à base de résine époxy liquide et adhésif faisant appel à ladite composition - Google Patents

Composition à base de résine époxy liquide et adhésif faisant appel à ladite composition Download PDF

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Publication number
WO2007083673A1
WO2007083673A1 PCT/JP2007/050614 JP2007050614W WO2007083673A1 WO 2007083673 A1 WO2007083673 A1 WO 2007083673A1 JP 2007050614 W JP2007050614 W JP 2007050614W WO 2007083673 A1 WO2007083673 A1 WO 2007083673A1
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WIPO (PCT)
Prior art keywords
epoxy resin
resin composition
liquid epoxy
seconds
adhesive
Prior art date
Application number
PCT/JP2007/050614
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English (en)
Japanese (ja)
Inventor
Masa Taniguchi
Yuichi Watanabe
Hideki Kikuchi
Yasuo Matsumura
Original Assignee
Somar Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Priority claimed from PCT/JP2006/301894 external-priority patent/WO2007083397A1/fr
Application filed by Somar Corporation filed Critical Somar Corporation
Priority to CN200780008387.3A priority Critical patent/CN101400715B/zh
Priority to JP2007554928A priority patent/JPWO2007083673A1/ja
Publication of WO2007083673A1 publication Critical patent/WO2007083673A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H01L2224/29001—Core members of the layer connector
    • H01L2224/29099—Material
    • H01L2224/2919—Material with a principal constituent of the material being a polymer, e.g. polyester, phenolic based polymer, epoxy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/01—Chemical elements
    • H01L2924/01005—Boron [B]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/013—Alloys
    • H01L2924/014—Solder alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/06—Polymers
    • H01L2924/0665—Epoxy resin
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/19—Details of hybrid assemblies other than the semiconductor or other solid state devices to be connected
    • H01L2924/1901—Structure
    • H01L2924/1904—Component type
    • H01L2924/19041—Component type being a capacitor
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/303—Surface mounted components, e.g. affixing before soldering, aligning means, spacing means
    • H05K3/305—Affixing by adhesive

Definitions

  • the present invention relates to a liquid epoxy resin composition suitable for surface mounting and an adhesive using the same, and particularly, when a component such as a semiconductor or an electronic component is fixed on various printed circuit boards, it is cured in a short time.
  • a liquid epoxy resin composition that can hold electronic components placed on various printed circuit boards over time without causing misalignment, and can be securely bonded and fixed even in electronic components that are downsized. It relates to the adhesive.
  • an adhesive containing an epoxy resin composition has been used as an adhesive for adhering and fixing a surface mounting component onto a printed circuit board.
  • a resin include epoxy resin, amine-based curing agent, and hydrophilic silica particles as a thixotropic agent (see Patent Document 1), liquid epoxy resin and amine-based latent curing.
  • Patent Document 2 A material containing an agent, a calcined talc, and an organic rheological additive has been proposed (see Patent Document 2).
  • JIS K 6850 has been adopted as a method for measuring this type of adhesive force, but it includes chip capacitors that use materials other than aluminum as surface mounting components.
  • a measurement method using a push-pull gauge has been adopted. This way Needless to say, a material that exhibits an adhesive strength of a certain level or more when evaluated in (1) is desired.
  • Patent Document 1 Japanese Patent Laid-Open No. 04-33916
  • Patent Document 2 Japanese Patent Laid-Open No. 07-316400
  • Patent Document 3 Japanese Patent Laid-Open No. 03-39378
  • Patent Document 4 Japanese Patent Laid-Open No. 10-27956
  • the present invention is capable of reliably bonding and fixing these problems, that is, an electronic component that has a high adhesive force and a small size with a short curing time, and the force does not depend on the type of the electronic component. It is an object of the present invention to provide a liquid epoxy resin composition with sufficient adhesive strength and an adhesive using the same.
  • the present invention provides the following liquid epoxy resin composition and an adhesive using the same. To do.
  • a liquid epoxy resin composition containing at least (a) an epoxy resin and (b) a curing agent, wherein the liquid epoxy resin composition is coated with a solder resist and a preflux.
  • a dispenser on the substrate after applying two points with a coating diameter of 0.7 ⁇ 0.15 mm, attach a 2012 type square ceramic capacitor as an adherend on the coated part.
  • Respective reaction rates of the liquid epoxy resin composition when cured at a temperature of 130 ° C for 0 seconds, 30 seconds, 60 seconds, and 90 seconds are j8 (0) and ⁇ ( 30), ⁇ (60), ⁇ (90), these relationships are represented by the following formulas, and the liquid epoxy resin according to any one of (1) to (3) above Fat composition.
  • the reaction rate in the present invention refers to a differential scanning calorimeter (DSC) manufactured by MacScience Co., Ltd. (currently Bruker 'A-Tex Co., Ltd. (Japan)), which will be described later! This refers to the reaction rate at a specific time calculated based on the formula derived from the reaction prediction formula according to the DSC Ozawa Software manual.
  • DSC differential scanning calorimeter
  • the new version of thermal analysis Takeo Ozawa, Hirotaro Kobe, edited by Kodansha Scientific
  • the liquid epoxy resin composition of the present invention and the adhesive using the liquid epoxy resin have high adhesive strength in spite of being fast-curing and prevent the occurrence of cracks and the like due to an increase in internal stress. As a result, both yield and product reliability can be improved. in this way
  • the liquid epoxy resin composition of the present invention can provide an extremely useful adhesive particularly when surface mounting electronic parts (including semiconductors) or the like on a printed circuit board.
  • the epoxy resin used in the present invention has two or more epoxy groups in one molecule.
  • epoxy resin that is liquid at normal temperature is preferable, but even if it is solid at normal temperature, it can be used by dissolving it in liquid epoxy resin at normal temperature.
  • epoxy resins may be used alone or in combination of two or more.
  • the balance of adhesiveness, electrical insulation, and mechanical properties of cured products Bisphenol A type epoxy resin and bisphenol F type epoxy resin are preferred.
  • a mixture of bisphenol A type epoxy resin and bisphenol F type epoxy resin is preferred.
  • the latent curing agent is, for example, a modified amine compound that is solid at room temperature, which is activated by heat, or a microcapsule that is dissolved or destroyed at a desired temperature, for example, acid anhydrides, imidazoles, phenols.
  • a mic mouth capsule type latent hardener containing a curing agent such as a compound or amide. These may be used alone Two or more types may be used in combination from the viewpoint of adjusting the curing time (reactivity) and the physical properties of the cured product.
  • amine latent curing agent for adjusting the curing time (reactivity) and adjusting the viscosity when used as an adhesive.
  • amine-based latent curing agents include 2-heptadecyl imidazole, 2-ferro-4-methyl-5-hydroxymethyl imidazole, 2-ferro-4-benzyl-5-hydroxymethyl imidazole, 2, 4 diamino 6- ⁇ 2-Methylimidazolyl- (1) ⁇ -ethyl-5-triazine and its 2,4 diamine-6- ⁇ 2-methylimidazolyl- (1) ⁇ -ethyl-5-triazine isocyanuric acid compound such as isocyanuric acid adduct Etc.
  • Examples of the amine adduct compound include Amicure PN-23, Amicure PN-40J, Amicure MY-24 (all manufactured by Ajinomoto Fine Techno Co., Ltd., Amicure is a registered trademark), Novakia HX-3721, Novakia HX — 3741 (all manufactured by Asahi Kasei Chemicals Corporation, Novakia is a registered trademark) can be used.
  • Examples of spirocetal compounds include CTU, ATU, and CTU guanamine (all manufactured by Ajinomoto Fine Techno Co., Ltd.).
  • an amine adduct compound is preferable because it has good adhesion to the cured product and has a balance between curability at low temperatures and storage stability.
  • latent curing agents are commercially available in the form of a powder or a paste mixed in an epoxy resin at room temperature, and the mass average particle size is preferably 15 m or less, preferably 10 m or less. . If the particle size exceeds 15 m, it is difficult to increase the reactivity and adhesive strength in a short time, which is not preferable. It is preferable to use a latent curing agent of 5 m or less from the viewpoint of fast curing and adhesion.
  • the use ratio of the curing agent is preferably in the range of 20 to 60 parts by mass, more preferably 36 to 50 parts by mass with respect to 100 parts by mass of the epoxy resin. If it is less than 20 parts by mass, the curability will be remarkably reduced, and if it exceeds 60 parts by mass, the moisture resistance and electrical properties of the cured product will be lowered and the viscosity will be remarkably increased.
  • These latent curing agents may be used alone or in combination of two or more.
  • the adhesive strength when the holding time at a temperature of 150 ° C is 60 seconds when tested by an adhesion test measured with a push-pull gauge in consideration of the low-temperature curing rate.
  • a compound having a reaction rate of 50% or more at 150 ° C for 30 seconds is preferably at least 50% by mass of the total amount of the curing agent. Preferably, it should be selected in such a proportion that it occupies 60% by mass.
  • dicyandiamide-based curing agents generally have a slow curing rate at 150 ° C., and therefore are not preferably used as the main curing agent raw material in the composition of the present invention.
  • a dicyandiamide-based curing agent may be added for the purpose of improving storage stability and enhancing adhesive strength, as long as it satisfies the requirements as a composition according to the present invention.
  • the liquid epoxy resin composition of the present invention can contain other additives as required.
  • additives include fused silica, crystalline silica, low ⁇ -ray silica, glass flakes, glass beads, glass balloons, talc, alumina, calcium silicate, aluminum hydroxide, calcium carbonate, barium sulfate, magnesia, and nitride.
  • Inorganic fillers such as silicon and boron nitride, fillers with particle size such as acrylic resin, polyester resin and silicone resin, and at least one epoxy group in the molecule.
  • Compounds with low viscosity under normal pressure such as phenol glycidyl ether, polyethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, methyl glycidyl ether, propyl glycidyl ether, pentaerythritol polyglycidyl ether, sorbitol poly Glycidyl ether, Reactive diluents such as ⁇ -butyldaricol glycidyl ether, 2-ethylhexyl glycidyl ether, phosphorus compounds such as triphenylphosphine, such as triethylamine, tetraethanolamine, 1,8 diazabicyclo [ 5.
  • Reactive diluents such as ⁇ -butyldaricol glycidyl ether, 2-ethylhexyl glycidyl ether, phosphorus compounds such as triphenylphosphine
  • DBU undecene
  • ⁇ N dimethylbenzylamine, 1, 1, 3, 3-tetramethyldazine, 2 ethyl-4-methylimidazole, N-methylpiperazine, etc.
  • Tertiary amine compounds for example, boron accelerators such as 1,8 diazabicyclo [5.4.0] -17 borondecatetraphenol, stress accelerators such as nitrile rubber and butadiene rubber, silane Coupling agents, titanate coupling agents, coupling agents such as aluminum coupling agents, coloring dyes and pigments Agents, oxidation stabilizers, moisture resistance improvers, thixotropy imparting agents, diluents, antifoaming agents, leveling agents, and other various types of resin.
  • boron accelerators such as 1,8 diazabicyclo [5.4.0] -17 borondecatetraphenol
  • stress accelerators such as nitrile rubber and butadiene rubber
  • silane Coupling agents titanate coupling agents
  • the reactive diluent is excellent in the viscosity controllability of the composition, and is particularly effective when the liquid epoxy resin composition of the present invention is applied as an adhesive using screen printing or a dispenser.
  • the silane coupling agent is preferably used in terms of the adhesion between the epoxy resin and the filler.
  • the mixing ratio of the reactive diluent may be appropriately selected depending on the viscosity of the adhesive to be obtained, but is usually in the range of 0 to 20 parts by mass with respect to 100 parts by mass of the epoxy resin.
  • the blending ratio of the coupling agent is usually in the range of 0.25 to 2.0 parts by mass with respect to 100 parts by mass of the filler.
  • the surface of the filler previously treated with a coupling agent may be used.
  • the liquid epoxy resin composition of the present invention can be obtained by mixing various additives such as an epoxy resin, a curing agent, and, if necessary, a filler.
  • the adhesive of the present invention includes these components.
  • a liquid epoxy resin composition comprising:
  • the liquid epoxy resin composition comprising the epoxy resin, the curing agent, and various additives such as a filler used as required, has an adhesive strength after 60 seconds (A ) And the adhesive strength (B) after 1 hour satisfy 0.6B ⁇ A.
  • the present invention provides a liquid epoxy resin composition as a raw material for adhesives used in the manufacture of various electronic components including chip capacitors, etc., as long as they have adhesive properties that satisfy such a relationship. As a product, it has been found that it is sufficiently practical, and has been completed based on this fact.
  • the adhesive strength is at least 50%.
  • the present invention has been completed by finding that a strength of at least%, preferably at least 60%, is necessary.
  • a liquid epoxy resin composition is applied onto a substrate coated with solder resist and preflux. After applying two points at an application diameter of 0.7 ⁇ 0.15 mm with an dispenser, 2012 type square ceramic capacitors are mounted on the composition as adherends. 30 seconds after mounting, raise the temperature so that the surface temperature of the substrate will be 150 ° C, hold for 60 seconds or 1 hour, cure, cool to 23 ° C, and push it in the direction perpendicular to the major axis of the part to peel Measure the strength with a push pull gauge.
  • the adhesive strength (A) after 60 seconds is preferably 30N or more. 40N or more is preferable.
  • the liquid epoxy resin composition of the present invention has various reaction rates of the liquid epoxy resin composition when cured at 150 ° C for 0 seconds, 30 seconds, 60 seconds, and 90 seconds.
  • ⁇ is (0), ((30), a (60), and a (90), respectively, it is preferable that these relationships (X) satisfy the following formula (I).
  • a liquid epoxy resin composition that satisfies this relationship is less affected by the surrounding environment during the curing operation and exhibits a certain level of adhesive strength within a short period of time. Is preferable.
  • the liquid epoxy resin composition of the present invention has the respective reaction rates of the liquid epoxy resin composition when cured for 0 seconds, 30 seconds, 60 seconds, and 90 seconds at a temperature of 130 ° C.
  • Respectively , J8 (0), j8 (30), ⁇ (60), and ⁇ (90) it is preferable that these relationships (Y) satisfy the following formula (II). This is because those satisfying such a relationship are preferably used in the case of a bonding operation of a special semiconductor package with a low operation guarantee temperature.
  • the wrinkle is less than 2, the moisture resistance and insulating properties of the cured product are lowered, and if it exceeds 10, the curing rate is too high and the cured product is likely to be distorted.
  • Surface strength of cured product in terms of moisture resistance, insulation properties and strain suppression property Preferably it is in the range of 2-7.
  • the liquid epoxy resin composition of the present invention may satisfy the relationship X of the reaction rate at each time at 150 ° C, but recently, from the viewpoint of environmental problems including global warming and resource saving. Therefore, by setting the reaction rate of the liquid epoxy resin composition at a lower temperature, especially 130 ° C, and satisfying the relationship Y of the reaction rate at each time, the curing temperature tends to be lowered. It is preferable because a liquid epoxy resin composition having excellent adhesion and curability can be obtained regardless of whether the temperature is high or low.
  • the liquid epoxy resin composition of the present invention has a reaction rate ⁇ (150) when cured at a temperature of 150 ° C for 30 seconds and a cure rate of 30 seconds at a temperature of 80 ° C. It is preferable that the ratio ⁇ [ ⁇ (150) / ⁇ (80)] to the reaction rate ⁇ (80) is 10 or more. If this ratio is less than 10, the reaction proceeds at 80 ° C and the storage stability decreases, and the reaction rate after 60 seconds at 150 ° C decreases, that is, during storage and during Z or use. This is not preferable because the stability is lowered.
  • the surface strength of long-term storage, adhesion, and fast curing is particularly preferably 12 or more.
  • X determined by the formula (I) is 3 or more and 15 or less
  • Y is calculated by the formula (II) is 2 or more and 10 or less
  • the liquid epoxy resin composition with a Z ratio of 10 or more has a high initial (0 to 30 seconds) reaction rate. Since the reaction rate at is low, it has excellent long-term storage stability. As a result, an adhesive containing such a liquid epoxy resin composition has a high storage stability, but when used, it can be attached to an adherend such as an electronic component in a short time. It is possible to achieve both a high degree of compatibility with the effects of storage and adhesion, which can be firmly bonded to each other.
  • the liquid epoxy resin composition of the present invention preferably has an elastic modulus in the following elastic modulus measurement test in the range of 5 ⁇ 10 8 to 5 ⁇ 10 1 Q Pa.
  • the flexural modulus was measured by a method based on JIS K 6911. The test piece was cured at 120 ° C. for 1 hour and further cured at 150 ° C. for 1 hour.
  • the adhesive of the present invention contains the above-mentioned epoxy resin, curing agent, and optionally used various additives such as fillers at a predetermined ratio. If the epoxy resin is liquid at room temperature, the epoxy resin is used at room temperature. In the case of a solid, it can be obtained by uniformly mixing epoxy resin or all components in a solvent, but it is preferable to prepare by the following method from the viewpoint of storage stability and curability in a short time. .
  • Liquid epoxy resin or epoxy resin previously dissolved in an organic solvent such as toluene, ethanol, cellosolve, tetrahydrofuran, N-methyl-2-pyrrolidone, dimethylformamide, a curing agent, a filler, etc.
  • organic solvent such as toluene, ethanol, cellosolve, tetrahydrofuran, N-methyl-2-pyrrolidone, dimethylformamide, a curing agent, a filler, etc.
  • a planetary mixer, a universal stirrer, etc. which is conventionally used when producing an adhesive.
  • the adhesive of the present invention can be suitably used in various coating methods such as a dispense method, a pin transfer method, and a screen printing method. As an example, a method for fixing an electronic component using the adhesive of the present invention by the dispense method will be described.
  • Adhesive is applied using a dispenser to the place where the electronic components on the circuit pattern are mounted.
  • the dispenser can be a screw type (a method in which adhesive is discharged by rotating the screw) or an air type (a method in which air is discharged by air pressure).
  • an electronic component is placed on the adhesive and cured at a temperature of 130 to 180 ° C. for about 30 to 60 seconds to fix the component.
  • the adhesive strength and Z or reaction rate in 60 seconds after heating are high, so it is possible to securely fix electronic components in a short curing time, so it has excellent yield, but it moves to the next process Since the time required to complete the process can be shortened, it is excellent in work efficiency and productivity. Furthermore, since there is no change in the shape of the adhesive in the next process, for example, the nodal dipping process, it is possible to suppress the tilting of electronic components and the occurrence of misalignment, etc. can do.
  • liquid epoxy resin composition of the present invention and the adhesive using the liquid epoxy resin composition will be specifically described with reference to examples.
  • the liquid epoxy resin composition of the present invention and the adhesive using the same Is not limited by these examples.
  • the adhesives of Examples and Comparative Examples were evaluated for three items: adhesive strength, reaction rate, and elastic modulus. These items were evaluated by the following methods.
  • the liquid epoxy resin composition (adhesive) of the present invention is applied to a solder resist and a substrate coated with preflux in advance with a dispenser at a single coating diameter of 0.7 ⁇ 0.15 mm. Apply spot. After mounting a 2012 type square ceramic capacitor on this adhesive, the temperature of the substrate surface was raised to 150 ° C in 30 seconds, then 60 seconds later (A) and 1 hour (B) Holding and curing (curing furnace: static reflow furnace SAR—401A ( Okuhara Electric))). The specimens (A) and (B) were allowed to cool to room temperature (23 ° C), and the peel strength when pressed in the direction perpendicular to the major axis of the part was measured with a push-pull gauge. The number of items was 10 and the average value was recorded.
  • the Oka plot is created by taking the common logarithmic value of the above temperature rise speed on the vertical axis and the inverse value of the peak temperature on the horizontal axis, and then determining the activity energy, frequency factor, and reaction order for each sample. It was.
  • a reaction prediction diagram is created from the activation energy, frequency factor and reaction order obtained in ⁇ 2> above, and 80 from this figure.
  • C 130. . And 150. .
  • the reaction rates at 0 seconds, 30 seconds, 60 seconds and 90 seconds at each temperature were calculated.
  • reaction rate powers at 0 seconds, 30 seconds, 60 seconds and 90 seconds were obtained as follows: Result X at 150 ° C. and Result Y at 130 ° C.
  • test piece was further cured after 1 hour at 120 ° C.
  • Example 1 Bisphenol A type epoxy resin (made by Japan Epoxy Resin Co., Ltd., trade name: Epicote 828) 50 parts by mass, Bisphenol F type epoxy resin 50 parts by mass, curing agent (imidazole amine amine curing agent; Ajinomoto Fine Techno Co., Ltd., trade name: Amicure PN-H, average particle size 10 ⁇ m) 35 parts by mass and silica powder (manufactured by Nippon Aerosil Co., Ltd., trade name: Aerosil # 300) Mixing was performed to prepare an epoxy resin solution.
  • curing agent imidazole amine amine curing agent
  • silica powder manufactured by Nippon Aerosil Co., Ltd., trade name: Aerosil # 300
  • Example 1 20 parts by mass of an imidazole-based amine adduct hardener (Ajinomoto Finetano Co., Ltd., trade name: Amicure PN-23J, average particle size 3 m) and an aliphatic amine-based amine adduct were used. (Ajinomoto Fine Techno Co., Ltd., trade name: Amicure MY-24, average particle size 8 to: LO / zm) Except for changing to 15 parts by mass, the same liquid epoxy resin as in Example 1 An adhesive consisting of a composition was prepared. The physical properties of this product are shown in Table 1.
  • Example 1 30 parts by mass of an imidazole-based amine adduct curing agent (Ajinomoto Fine Tetano Co., Ltd., trade name: Amicure PN-23, average particle size 10 m) and an aliphatic amine-based amine adduct were used.
  • Curing agent (Ajinomoto Fine Techno Co., Ltd., trade name: Amicure MY-24, average particle size 8 to: LO / zm) Liquid epoxy resin in the same manner as in Example 1 except for changing to 10 parts by mass
  • An adhesive consisting of a composition was prepared. The physical properties of this product are shown in Table 1.
  • Example 1 30 parts by mass of an imidazole amine adduct hardener (manufactured by Ajinomoto Fine Tetano Co., Ltd., trade name: Amicure PN-40J, average particle size 3 m) and an aliphatic amine amine adduct are used.
  • Curing agent (Ajinomoto Fine Techno Co., Ltd., trade name: Amicure MY-24, average particle size 8 to: LO / zm) Except for changing to 10 parts by mass, all in the same manner as in Example 1 An adhesive consisting of a fat composition was prepared. The physical properties of this product are shown in Table 1.
  • Example 5 In Example 1, all the steps were performed except that the curing agent was changed to 35 parts by mass of the microcapsule type curing agent (manufactured by Asahi Kasei Chemicals Corporation, trade name: Novakiyua HX-3722, average particle size 2 m).
  • the curing agent was changed to 35 parts by mass of the microcapsule type curing agent (manufactured by Asahi Kasei Chemicals Corporation, trade name: Novakiyua HX-3722, average particle size 2 m).
  • an adhesive comprising a liquid epoxy resin composition was prepared. The physical properties of this product are shown in Table 1.
  • Example 1 10 parts by mass of an imidazole amine adduct (Ajinomoto Fine Techno Co., Ltd., trade name: Amicure PN-40J, average particle size 3 m) and an aliphatic amine aminadduct (Ajinomoto Co., Inc.) were used. Fine Techno Co., Ltd., trade name: Amicure MY-24, average particle size 8-10 ⁇ m) Adhesion comprising a liquid epoxy resin composition in the same manner as in Example 1 except for changing to 30 parts by mass An agent was prepared. In this composition, the amount of low-curing Amicure PN-40J is less than the amount of Amicaure MY-24, a low-temperature-curing curing agent that exhibits curability at higher temperatures. Since it only accounts for 25% by mass of the amount of glaze agent, the relationship of the adhesive strength of this composition did not satisfy 0.6B ⁇ A. Table 1 shows the physical properties of this product.
  • Example 1 the curing agent was changed to 35 parts by mass of a dicyandiamide-based microcapsule type curing agent (manufactured by Asahi Kasei Chemicals Corporation, trade name: Novakia HX-3613, average particle size 5 m). Except for the above, an adhesive comprising a liquid epoxy resin composition was prepared in the same manner as in Example 1. The physical properties of this product are shown in Table 1.
  • the adhesive of the present invention has a higher adhesive force in a shorter time than Comparative Examples 1 and 2.
  • the reaction rate at 80 ° C. is kept lower than that in Comparative Examples 1 and 2.
  • the adhesive has high storage stability and instantly undergoes a curing reaction when used and can provide a strong adhesive force in a short time. Therefore, it can be seen that the yield is improved and a high-quality product can be obtained.
  • the liquid epoxy resin composition of the present invention and the adhesive used therefor can fix a semiconductor, an electronic component or the like on a circuit board in a short time, and therefore can shorten the time to the next process. As a result, work efficiency and productivity can be improved, and adhesion with high storage stability can be obtained. Producing with such an adhesive can improve yield and produce high quality products. Therefore, the liquid epoxy resin composition of the present invention and the adhesive using the same are extremely effective in the field of mounting semiconductors and electronic components.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

La présente invention se rapporte à une composition à base de résine époxy liquide, qui contient au moins une résine époxy et un agent durcisseur. La composition à base de résine époxy liquide selon l'invention est caractérisée en ce que la force d'adhérence (A) après un durcissement à 150 °C pendant 60 secondes et la force d'adhérence (B) après un durcissement à 150 °C pendant une heure satisfont de préférence à la relation suivante : 0,6B < A. L'invention concerne également un adhésif contenant une composition de résine époxy liquide qui est caractérisée de préférence en ce que la force d'adhérence (A) après un durcissement à 150 °C pendant 60 secondes et la force d'adhérence (B) après un durcissement à 150 °C pendant une heure satisfont de préférence à la relation suivante : 0,6B < A.
PCT/JP2007/050614 2006-01-17 2007-01-17 Composition à base de résine époxy liquide et adhésif faisant appel à ladite composition WO2007083673A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN200780008387.3A CN101400715B (zh) 2006-01-17 2007-01-17 液态环氧树脂组合物及使用该组合物的粘合剂
JP2007554928A JPWO2007083673A1 (ja) 2006-01-17 2007-01-17 液状エポキシ樹脂組成物及びこれを用いた接着剤

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JP2006-009303 2006-01-17
JP2006009303 2006-01-17
JPPCT/JP2006/301894 2006-02-03
PCT/JP2006/301894 WO2007083397A1 (fr) 2006-01-17 2006-02-03 Composition à base de résine époxy liquide et adhésif faisant appel à ladite composition

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012122008A (ja) * 2010-12-09 2012-06-28 Kyocera Chemical Corp 接着剤層の形成方法、および接着剤組成物
WO2013089062A1 (fr) * 2011-12-15 2013-06-20 デクセリアルズ株式会社 Agent adhésif et procédé de connexion d'un composant électronique
JP2018039889A (ja) * 2016-09-06 2018-03-15 株式会社スリーボンド エポキシ樹脂組成物
WO2021106330A1 (fr) * 2019-11-26 2021-06-03 昭和電工株式会社 Stratifié composite et corps assemblé

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07133474A (ja) * 1993-11-09 1995-05-23 Matsushita Electric Ind Co Ltd 電子回路形成用一液性接着剤及び接着剤塗布方法
JPH09208806A (ja) * 1996-02-07 1997-08-12 Toray Dow Corning Silicone Co Ltd 硬化性エポキシ樹脂組成物および電子部品
JP2003133672A (ja) * 2001-10-25 2003-05-09 Sanei Kagaku Kk 穴詰材料、並びに穴詰プリント配線（基）板の製造方法及び穴詰プリント配線（基）板

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07133474A (ja) * 1993-11-09 1995-05-23 Matsushita Electric Ind Co Ltd 電子回路形成用一液性接着剤及び接着剤塗布方法
JPH09208806A (ja) * 1996-02-07 1997-08-12 Toray Dow Corning Silicone Co Ltd 硬化性エポキシ樹脂組成物および電子部品
JP2003133672A (ja) * 2001-10-25 2003-05-09 Sanei Kagaku Kk 穴詰材料、並びに穴詰プリント配線（基）板の製造方法及び穴詰プリント配線（基）板

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012122008A (ja) * 2010-12-09 2012-06-28 Kyocera Chemical Corp 接着剤層の形成方法、および接着剤組成物
WO2013089062A1 (fr) * 2011-12-15 2013-06-20 デクセリアルズ株式会社 Agent adhésif et procédé de connexion d'un composant électronique
JP2013124329A (ja) * 2011-12-15 2013-06-24 Dexerials Corp 接着剤、及び電子部品の接続方法
JP2018039889A (ja) * 2016-09-06 2018-03-15 株式会社スリーボンド エポキシ樹脂組成物
WO2021106330A1 (fr) * 2019-11-26 2021-06-03 昭和電工株式会社 Stratifié composite et corps assemblé

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