WO2005105919A1 - 封止用樹脂組成物及び樹脂封止された半導体装置 - Google Patents
封止用樹脂組成物及び樹脂封止された半導体装置 Download PDFInfo
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- WO2005105919A1 WO2005105919A1 PCT/JP2005/008324 JP2005008324W WO2005105919A1 WO 2005105919 A1 WO2005105919 A1 WO 2005105919A1 JP 2005008324 W JP2005008324 W JP 2005008324W WO 2005105919 A1 WO2005105919 A1 WO 2005105919A1
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- epoxy resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
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- 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
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
Definitions
- the present invention relates to a sealing resin composition suitable for resin-sealing a semiconductor element and an electrode wiring around the semiconductor element. More specifically, the present invention is not only excellent in electrical insulation, mechanical properties, heat resistance, chemical resistance, dimensional stability, etc., but also has a sealing molded product (solidified or cured resin composition).
- the present invention relates to a sealing resin composition capable of strictly and stably controlling the surface resistivity of a semiconductive region. Further, the present invention relates to a semiconductor device such as a semiconductor device in which a semiconductor element is resin-sealed with the sealing resin composition.
- resin encapsulation is performed by pouring resin around these elements.
- Resin encapsulation is performed to protect semiconductor elements such as IC and LSI, wiring such as bonding wires and inner leads from the external environment, and to improve handling during mounting.
- an epoxy type encapsulant is mainly used.
- Epoxy-based encapsulants generally use an epoxy compound (epoxy resin) that has two or more epoxy groups in the molecule. When a curing agent is added to the epoxy compound and heated, it has chemical resistance and mechanical strength. Excellent cured product is obtained.
- Epoxy-based encapsulating materials include an epoxy resin as the main component, a curing agent, a curing accelerator, a flexible agent, a filler, a coupling agent, a flame retardant aid, a coloring agent, a release agent, and an ion.
- An epoxy resin composition to which an auxiliary agent selected from a scavenger or the like is appropriately added is used.
- Resin sealing includes transfer molding, dipping, potting, and powder flowing immersion. Among these However, because of its suitability for mass production, most of the packages are sealed with resin using the transfer molding method.
- an epoxy-based encapsulating material is molded into an epoxy tablet (B-stage solid), and the epoxy tablet is heated to a high temperature.
- a method is adopted in which the semiconductor chip or module previously loaded in the mold is sealed by inserting the mold into the mold and applying pressure.
- the epoxy resin material forms a resin sealing portion cured by heating.
- a method has been proposed in which an epoxy-based sealing material is used to perform resin molding by an injection molding method (injection molding method).
- the sealing resin material has excellent electrical insulation, mechanical properties, heat resistance, chemical resistance, dimensional stability, moisture resistance, stress relaxation, circuit concealment, light shielding, heat dissipation, etc. It is also required to have characteristics. For example, a semiconductor element such as an IC is itself a fine circuit, and therefore, must be sealed with a resin while maintaining insulation between terminals. Therefore, the sealing resin material needs to have electrical insulation properties. In addition, since the circuit of the semiconductor element is easily broken by moisture and ionic impurities, the sealing resin material is required to have a low moisture absorption (water absorption).
- the epoxy resin has a vitrification rate of 10 to 9
- Epoxy resin composition for semiconductor encapsulation blended with 5% by weight of partially spheroidized silicon (JP-A-2000-066366), excellent in heat resistance, moisture resistance, and flexural modulus Spherical silica with an average particle size of 2 to 10 ⁇ m and an extremely small specific surface area is Yarn composition containing 40 to 85% by mass (Japanese Patent Laid-Open No. 2001-226652), and one after-curing step is omitted.
- the electronic device surface resistivity has a resin sealing portion less than 1 0 5 Omega slag is too fast moving speed of charges in the resin sealing portion in, Ya strong current generated during the electrostatic discharge High voltages can damage electronic devices.
- the surface resistivity of the resin sealing portion is too low, electrical insulation cannot be ensured.
- resin-sealed with a sealing resin material those skilled in the art have not sufficiently recognized the problem of ESD failure due to the resin-sealed portion. No proposal has been made to solve the problem of ESD damage of the sealing resin material.
- seals used in these technical fields have been developed to ensure that electronic devices are sufficiently protected from electrostatic interference and that they maintain a high degree of cleanliness without attracting dust. Responding to ESD obstacles has become an important issue for stopping resin materials.
- a method of volume resistivity, such as conductive carbon black and carbon fiber in the resin material for sealing is blended conductive filler of less than 1 0 2 ⁇ ⁇ cm, the electric resistance of the resin component and the conductive charge Hamazai Since the ratios are so far apart, slight differences in the compounding ratio of the conductive filler and slight fluctuations in the molding conditions greatly change the surface resistivity of the resin-sealed portion. Therefore, simply the method of blending the conductive filler, the surface resistivity of the resin sealing portion 1 0 5 ⁇ 1 0 1 3 ⁇ / desired value become so strictly and stably control the range of the mouth It is extremely difficult to control.
- An object of the present invention is to provide a sealing resin composition that can be strictly controlled in a sealing region.
- Another object of the present invention is to provide a semiconductor device in which a semiconductor element is resin-sealed with a sealing resin composition having such excellent characteristics.
- Rate is solely carbon precursor 1 0 2 ⁇ 1 0 ⁇ ⁇ ⁇ cm, or the carbon precursor and the body volume resistivity was formulated by combining the 1 0 2 ⁇ . Cm below the conductive filler resin I arrived at the composition.
- a thermosetting resin is preferable.
- an epoxy resin widely used as a sealing resin material is preferable.
- the encapsulating resin composition of the present invention strictly and stably controls the surface resistivity of a molded product (solidified or cured product) to a desired value in a semiconductive region while ensuring electrical insulation. It can be controlled, and the variation in the surface resistivity depending on the location is small.
- the encapsulating resin composition of the present invention also has excellent properties such as mechanical properties, heat resistance, chemical resistance, and dimensional stability. Therefore, the encapsulating resin composition of the present invention can exhibit a high degree of performance suitable as an encapsulating resin material. The present invention has been completed based on these findings.
- the synthetic resin (A) 1 0 0 part by weight, the carbon precursor having a volume resistivity of 1 0 2 ⁇ 1 0 1 0 ⁇ ⁇ cm (B) 1 0 ⁇ 5 0 0 parts by weight, the volume resistivity rate is 1 0 2 Omega ⁇ cm less than the conductive filler (C) 0 to 6 0 parts by weight, and other inorganic fillers (D) for sealing containing 1 0 0-1 5 0 0 parts by weight
- a resin composition is provided.
- thermosetting resin an epoxy resin component containing an epoxy compound having two or more epoxy groups in one molecule and a curing agent. Is done.
- the synthetic resin used in the present invention is not particularly limited, and examples thereof include polyamide, polyacetanol, polybutylene terephthalate, polyethylene terephthalate, polyethylene, polypropylene, polyisobutylene, polyisoprene, polybutene, poly p-xylene, polychlorinated vinyl, Polyvinylidene chloride, polycarbonate, modified polyphenylene ether, polyurethane, polydimethylsiloxane, polyvinegar Acid biels, polystyrene, polymethyl acrylate, polymethyl methacrylate, ABS resin, polyphenylene / refide, polyether A tenoroketone, polyetherenoketone, polyphenylene / refide ketone, polyphenylene / refidenolephone, polyether ether Tolyl, wholly aromatic polyester, fluororesin, polyarylate, polysulfone, polyethersulfone, polyetherimide, polyamideimide, polyaminobis
- fluororesin examples include tetrafluoroethylene Z hexafluoropropylene copolymer, tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, polyclonal trifluoroethylene, polyvinylidene fluoride, and fluoride.
- Vinylidene / hexafluoropropylene / tetrafluoroethylene copolymer polyfluorinated vinyl, ethylene / tetrafluoroethylene copolymer, ethylene / chlorotrifluoroethylene copolymer, propylene / tetrafluoroethylene copolymer Polymer, tetrafluoroethylene / perfluoroalkyl perfluorobutyl ether copolymer, vinylidene fluoride z-hexafluoropropylene copolymer, vinylidene fluoride
- Trifluoroethylene copolymer Trifluoroethylene copolymer, tetrafluoroethylene / ethylene z-isobutylene copolymer, ethylene / hexafluoropropylene copolymer, tetrafluoroethylene / ethyl vinyl ether copolymer, and the like.
- These synthetic resins can be used alone or in combination of two or more.
- thermosetting resin is preferable.
- the thermosetting resin used in the present invention include an epoxy resin, a phenol resin, a melamine resin, and a urea resin, and any of known resins can be used.
- Epoxy resin has excellent dimensional stability.
- Phenol resins and melamine resins have excellent impact resistance, heat resistance, chemical resistance, water resistance, and flame resistance.
- Urea resin has a high surface hardness and is characterized by an ivory-like appearance.
- the phenol resin include a general-purpose phenol resin obtained by a reaction between phenol and formalin, a nopolak-type phenol resin, and a resole-type phenol resin.
- phenols that are raw materials for phenolic resins include phenol, bisphenoleno A, cresonole, anolequinolephenol, resonolecin, and naphthol-based compounds (eg, hydroxynaphthalene, dihydroquinaphthalene).
- the phenols can be used alone or in combination of two or more.
- the formaldehyde supply material which is a raw material of the phenol resin, include an aqueous formaldehyde solution, paraformaldehyde, an aqueous solution of hexamethylenetetramine, and 1,3-dioxolan.
- the melamine resin examples include general-purpose melamine resins obtained by reacting melamine and formalin, and alkyl etherified melamine resins (for example, butoxymethylmelamine resin and methoxymethylmelamine resin).
- the urea resin examples include a general-purpose urea resin obtained by reacting urea and formaldehyde. Further, a melamine / urea resin obtained by co-condensation of melamine, urea and formalin, and a phenol / uria resin obtained by co-condensation of phenol, urea and formalin can also be used as the thermosetting resin.
- epoxy resins which are widely used as sealing resins, are preferred.
- the epoxy resin is generally a mixture containing an epoxy compound and a curing agent. Epoxy compounds by themselves are often referred to as epoxy resins. Therefore, in the present invention, the mixture containing the epoxy resin compound and the curing agent is referred to as “epoxy resin component”.
- the epoxy compound used in the present invention is a compound having two or more epoxy groups in one molecule.
- the epoxy compound either a solid or liquid epoxy compound can be used.
- examples of such epoxy compounds include bisphenol-type epoxy resins such as bisphenol A-type epoxy resin and bisphenol F-type epoxy resin; phenol nopolak epoxy resin, cresol nopolak epoxy resin, and alkylphenol nopolak.
- Epoxy resin, xylene resin-modified Novola Novolak epoxy resins such as epoxy resin, ⁇ -naphthol novolak epoxy resin; Triphenol alkane epoxy resin such as trifenolmethane methane epoxy resin, trifenolpropane epoxy resin; Biphenyl epoxy resin Biphenyl skeleton epoxy resin such as biphenyl-aralkyl epoxy resin; phenol aralkyl epoxy resin; heterocyclic epoxy resin; naphthalene skeleton epoxy resin; stilbene epoxy resin; dicyclopentadiene epoxy Resins; brominated epoxy resins such as tetrabromobisphenol-type epoxy resin and brominated phenol nopolak-type epoxy resin; and the like. These epoxy resins can be used alone or in combination of two or more.
- a biphenyl skeleton type epoxy resin represented by the following chemical formulas 1 to 15 ( Chemical formulas 1-2), dicyclopentadiene type epoxy resin (chemical formula 3), cresol nopolak type epoxy resin (chemical formula 4), naphthalene skeleton type epoxy resin (chemical formulas 5-10), trifluorophenol propane Type epoxy resins (chemical formulas 11 to 12) and brominated epoxy resins (chemical formulas 13 to 15) are preferred.
- G represents a glycidyl group.
- R in Chemical Formula 1 represents ⁇ or CH 3 (preferably CH 3 ).
- a bromine atom (B r) is usually bonded to each aromatic ring in an amount of usually 1 to 3, and in many cases, 1 or 2.
- a self-extinguishing epoxy resin such as a brominated epoxy resin.
- a flame retardant auxiliary such as antimony trioxide.
- bromine compounds are generally pointed out as problems with regard to environmental impact, so when brominated epoxy resins are used as epoxy compounds, they are used in combination with other epoxy resins that do not contain halogen atoms. It is desirable to do.
- a brominated epoxy resin When a brominated epoxy resin is used, it is usually used in a proportion of 1 to 50% by weight, preferably 3 to 30% by weight, more preferably 5 to 20% by weight, based on the total amount of the epoxy compound. It is desirable.
- the curing agent used in the present invention is not particularly limited as long as it is used as a curing agent for an epoxy resin.
- Examples of the hardening agent for the epoxy resin include a phenolic compound having two or more phenolic hydroxyl groups, an amine compound, an organic acid anhydride, an imidazole compound, and a nitrogen-containing compound such as diazabicycloundecene.
- Examples include a heterocyclic compound, an organic phosphine, an organic boron complex, a quaternary ammonium compound, and a quaternary phosphonium compound.
- Each of these curing agents can be used alone, but two or more curing agents may be used in combination in order to control the curing speed and the physical properties of the cured product.
- these curing agents phenol compounds, amine compounds, organic acid anhydrides, and the like are preferable, and phenol compounds are more preferable because the cured product has no water resistance or reactivity with moisture.
- the phenol compound used as a curing agent is a compound containing two or more phenolic hydroxyl groups in one molecule.
- a nopolak-type phenol resin such as a phenol nopolak resin and a cresol nopolak resin; a phenol having a naphthalene ring Resin; phenol aralkyl phenolic resin; biphenyl phenolic resin; biphenyl aralkyl phenolic resin; triphenol methane phenolic resin, triphenol alkane phenolic resin such as triphenol propane phenolic resin Resin; alicyclic phenol resin; heterocyclic phenol resin; Bisphenol-type phenolic resins such as bisphenol A-type phenolic resin and bisphenol F-type phenolic resin;
- phenol nopolak resin cresol novolak resin, phenolaralkyl resin, naphthalene-type phenol resin, biphenyl-type phenol resin, and dicyclopentagen-type phenol resin are preferable, and phenol nopolak resin is more preferable.
- Specific examples of preferred phenol compounds are shown in the following chemical formulas 16 to 20.
- n represents 0 or an integer of 1 or more (preferably 1 to 10).
- Chemical Formula 18 n is an integer of 1 or more.
- R represents H or an alkyl group (preferably, CH 3 ).
- the curing agent is used at a ratio of usually 0.5 to 1.6 equivalents, preferably 0.6 to 1.4 equivalents, more preferably 0.7 to 1.2 equivalents to the epoxy group of the epoxy compound. Is done.
- the curing agent is incorporated into the skeleton of the cured product, so it is desirable to select the type and use ratio of the curing agent according to the characteristics required for the cured product.
- the phenolic compound preferably used as a curing agent in the present invention is such that the phenolic hydroxyl group in the phenolic compound is usually 0.5 to 1.6 mol per mol of the epoxy group in the epoxy compound (epoxy resin). Preferably, it is used in a ratio of 0.6 to 1.4 mol, more preferably 0.7 to 1.2 mol. If the phenolic hydroxyl group content is less than 0.5 mol, the phenolic hydroxyl group involved in the curing reaction becomes insufficient and the homopolymerization ratio of the epoxy group increases, resulting in a low glass transition temperature of the cured product. Easy to become.
- a curing accelerator can be used as needed to accelerate the curing reaction between the epoxy compound and the curing agent.
- the type of the curing accelerator is not particularly limited, and is known to have a property that the reaction is started by heating and hardly progresses at room temperature so that even if mixed with an epoxy resin or other components, there is practically no difficulty in curing. Can be used.
- the curing accelerator may be a shift between a so-called one-pack type latent type that can be stored in a mixed state as a composition and a two-pack type that starts curing immediately upon mixing.
- the curing accelerator examples include derivatives of 1,8-diazabicyclo [5.4.0] pendene-17, such as phenolic salts, phenolic novolak salts, and carbonates; 2-methylimidazole, 2-phenylimidazole, (2) Imidazonoles, such as heptadecyl imidazole, 2-ethynoleic 4-methylimidazole, 2-phenylenoid 4-methinoreimidazoi; ethi ⁇ phosphine, propyne phosphine, fenizure phosphine, triphenylinole phosphine A / legano phosphine compounds, such as trianolex / lephosphine; Ar— ⁇ —CO— ⁇ (where Ar is a substituted or unsubstituted And a compound having an imidazole skeleton.
- the curing accelerators can be used alone or in combination of two or more. When a curing accelerator is used, it is usually added in an amount of 0.2 to 20 parts by weight, preferably 0.5 to 10 parts by weight, based on 100 parts by weight of the epoxy compound (epoxy resin).
- the volume resistivity used in the present invention is 10 2 to 10 1 .
- the carbon precursor of ⁇ ⁇ cm can be obtained by firing an organic substance in an inert atmosphere at a temperature of 400 ° C to 900 ° C. More specifically, the carbon precursor used in the present invention includes, for example, (i) heating tar or pitch such as petroleum tar, petroleum pitch, coal tar, coal pitch, etc. to perform aromatization and polycondensation.
- oxidation and infusibilization in an oxidizing atmosphere, and heating and baking in an inert atmosphere and (ii) infusibilizing a thermoplastic resin such as polyataryl nitrile and polysalt in an oxidizing atmosphere, Further, it can be produced by a method of heating and baking in an inert atmosphere, (iii) a method of heating and curing a thermosetting resin such as a phenol resin or a furan resin, and then heating and baking in an inert atmosphere. .
- the carbon precursor means a substance which is not completely carbonized and has a carbon content of 97% by mass or less obtained by these treatments. Heating an organic substance in an inert atmosphere * When firing, as the firing temperature increases, the carbon content of the obtained fired body increases.
- the carbon content of the carbon precursor can be easily controlled by properly setting the firing temperature.
- the carbon precursor having a volume resistivity of 10 2 to 10 cm used in the present invention can be obtained as a completely non-carbonized carbon precursor having a carbon content of preferably 80 to 97% by mass.
- the volume resistivity of the carbon precursor is preferably 10 2 to 10 10 ⁇ ⁇ cm, more preferably 10 3 to 10 9 Q'cm.
- Carbon precursors are typically used in the form of particles or fibers.
- the average particle diameter of the carbon precursor particles used in the present invention is preferably 1 mm or less. If the average particle size of the carbon precursor is too large, it becomes difficult to obtain a solid or cured product having a good appearance when the synthetic resin composition is molded.
- the carbon precursor When the carbon precursor is fibrous, its average particle size is usually from 0.1 mm to: L mm, preferably from 0.5 to 500 ⁇ ⁇ , and more preferably from 1 to 100 / m. It is. In many cases, good results can be obtained by using a carbon precursor having an average particle size of about 5 to 50 m.
- the average diameter of the fibrous carbon precursor used in the present invention is preferably 0.1 mm or less. When the average diameter of the fibrous carbon precursor exceeds 0.1 mm, it becomes difficult to obtain a cured product having a good appearance.
- the fibrous carbon precursor is preferably a short fiber from the viewpoint of dispersibility in a synthetic resin such as an epoxy resin.
- the ratio of the carbon precursor is 100 parts by weight based on 100 parts by weight of a synthetic resin (for example, an epoxy resin component containing an epoxy compound and a curing agent). 0 to 500 parts by weight, preferably 15 to 450 parts by weight, more preferably 20 to 400 parts by weight.
- a synthetic resin for example, an epoxy resin component containing an epoxy compound and a curing agent.
- the surface resistivity can be in the semiconductive region even if the mixing ratio is as low as 10 to 50 parts by weight. it can.
- the carbon precursor is not used in combination with the conductive filler, it is preferable that the mixing ratio be in the range of more than 50 parts by weight and not more than 400 parts by weight in order to control the surface resistivity within a desired range. .
- the compounding ratio of the carbon precursor is too large, the withstand voltage of the solidified or cured product may be too low. If the compounding ratio of the carbon precursor is too small, it is difficult to sufficiently lower the surface resistivity of the solidified product or the cured product, and it is difficult to control the surface resistivity in the semiconductive region. If the proportion of the carbon precursor is too small, the variation in the surface resistivity depending on the location of the solidified or cured product tends to increase.
- the conductive filler having a volume resistivity of less than 1 0 2 ⁇ ⁇ cm to be used in the present invention is not particularly limited, for example, carbon fibers, black tin, conductive carbon black, and metal powder. Among them, the viewpoint of controllability and reproducibility of surface resistivity Thus, conductive carbon materials such as carbon fiber, graphite, conductive carbon black, and mixtures thereof are preferred.
- the surface resistivity of the cured product when used in combination with a carbon precursor, can be strictly controlled to a semiconductive region, and the variation in the surface resistivity depending on the location is sufficiently ensured.
- Carbon fiber is preferred because it can be smaller.
- the use of carbon fibers can also improve the mechanical properties of the cured product.
- the carbon fibers used in the present invention include cellulose-based carbon fibers, polyacrylonitrile-based carbon fibers (PAN-based carbon fibers), lignin-based carbon fibers, and pitch-based carbon fibers.
- PAN-based carbon fibers and pitch-based carbon fibers are preferred, and PAN-based carbon fibers are more preferred.
- the average diameter of the carbon fibers is preferably 50 ⁇ m or less. If the average diameter of the carbon fibers is too large, it becomes difficult to obtain a cured product having a good appearance.
- the average fiber length of the carbon fibers is preferably 10 ⁇ m or more and short fibers. If the average fiber length is too short, the effect of improving the mechanical properties is reduced.
- the conductive carbon black is not particularly limited as long as it has conductivity. Examples thereof include acetylene black, oil furnace black, thermal black, and channel black. Among these, conductive carbon blacks such as oil furnace black and acetylene black are preferred.
- the graphite is not particularly limited, and examples thereof include natural graphite such as artificial graphite, flaky graphite, flaky graphite, and ground graphite in which coke, tar, pitch, and the like are graphitized at a high temperature.
- the volume resistivity of the conductive filler used in the present invention is less than 1 0 2 ⁇ ⁇ cm, the lower limit of which is typically a volume resistivity of the metal material such as a metal powder or metal fibers.
- the conductive filler does not always need to be blended, and the surface resistivity of the cured product can be controlled within the semiconductive region by using the carbon precursor alone.
- the mixing ratio of the conductive filler is Synthetic resin (for example, an epoxy resin component containing an epoxy compound having two or more epoxy groups in one molecule and a hardening agent) 0 to 60 parts by weight, preferably 0 to 100 parts by weight based on 100 parts by weight To 50 parts by weight, more preferably 0 to 40 parts by weight, particularly preferably 0 to 30 parts by weight.
- Synthetic resin for example, an epoxy resin component containing an epoxy compound having two or more epoxy groups in one molecule and a hardening agent
- 0 to 60 parts by weight preferably 0 to 100 parts by weight based on 100 parts by weight To 50 parts by weight, more preferably 0 to 40 parts by weight, particularly preferably 0 to 30 parts by weight.
- a conductive filler such as carbon fiber
- its mixing ratio is usually 1 to 60 parts by weight, preferably 2 to 50 parts by weight, based on 100 parts by weight of the synthetic resin. It is preferably 3 to 40 parts by weight, particularly preferably 5 to 30 parts by weight. If the proportion
- other inorganic fillers are used in addition to the carbon precursor and the conductive filler.
- the other inorganic filler is preferably a non-conductive inorganic filler that does not substantially affect the volume resistivity or surface resistivity of the cured product.
- fillers occupy the largest proportion in the resin material for encapsulation and have a significant effect on the moldability and the properties of the cured product. Therefore, it is preferable to use, as the inorganic filler, those used in the technical field of the sealing resin material.
- the inorganic filler examples include crystalline silica, amorphous (amorphous) silica, spherical silica, fused silica, partially spherical silica having a vitrification ratio of 10 to 95% by weight, alumina, and nitrided silica. Element, talc, clay, glass fiber, glass beads, calcium sulfate, and the like.
- the inorganic filler may be surface-treated or coated. Silica is preferred for suppressing burrs, improving moisture resistance and improving low stress properties. In order to improve the thermal conductivity of the cured product, spherical alumina, silicon nitride and the like are preferable.
- silica such as silica
- amorphous silica spherical silica
- fused silica partially spheroidized with a vitrification ratio of 10 to 95% by weight
- Silica such as silica
- the average particle size of the silica is about 0.1 to 6 ⁇ , preferably 30 xm or less, more preferably 10 ⁇ m or less.
- These silicas may be used alone or in combination of two or more.
- the compounding ratio of the other inorganic filler is a synthetic resin (for example, an epoxy resin containing an epoxy compound having two or more epoxy groups in one molecule and a curing agent).
- (Resin component) 100 to 150 parts by weight, preferably 200 to 1200 parts by weight, more preferably 300 to 100 parts by weight, based on 100 parts by weight, Particularly preferably, it is from 350 to 900 parts by weight. If the mixing ratio of the inorganic filler is too large, the fluidity of the sealing resin composition becomes poor, and the sealing moldability decreases. If the blending ratio of the inorganic filler is too small, the water resistance becomes poor, and other characteristics tend to be unsatisfactory. 7.
- Coupling agent 100 to 150 parts by weight, preferably 200 to 1200 parts by weight, more preferably 300 to 100 parts by weight, based on 100 parts by weight, Particularly preferably, it is from 350 to 900 parts by weight. If the mixing ratio of the inorganic filler is too large, the fluidity of the sealing resin composition
- a force coupling agent such as a silane coupling agent, a titanate coupling agent, or an anorem-pum coupling agent can be used.
- the silane coupling agent is a silicone compound such as an alkoxysilane or a halosilane having one or more functional groups such as an amino group, a perylene group, an epoxy group, an isocyanate group, and a mercapto group in a molecule.
- silane coupling agent examples include ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -aminopropylmethoxysilane, ⁇ -phenyl / reaminopropyltrimethoxysilane, ⁇ - ureidopropyltriethoxysilane, .gamma. ureidopropionic built Increment Tokishishiran, .gamma. ureido propyl methyl trimethinecyanine Tokishishiran, .gamma.
- titanate coupling agent examples include isopropyl triisostearate peroxy titanate, isopropyl tri (N-aminoethyl 'aminoethyl) titanate, diisopropyl bis (dioctyl phosphate) titanate, and tetraisopropyl bis (dioctyl phosphite) ) Titanate, tetraoctylbis (ditridecyl phosphite) titanate, tetra (2,2-diallyloxymethyl-1 1-butyl) bis (ditridecyl) phosphite titanate, bis (dioctylpyrophosphate) oxyacetate Titanate, bis (dioctyl pyrophosphate) ethylene titanate and the like can be used.
- These coupling agents are used in a proportion of usually 0.01 to 5 parts by weight, preferably 0.05 to 3 parts by weight, based on 100 parts by weight of the other inorganic filler.
- thermoplastic resin can be contained in the thermosetting resin composition for improving the toughness of the thermosetting resin composition for sealing such as the epoxy resin composition for sealing.
- thermoplastic resin is not particularly limited, and examples thereof include polyamide, polyacetal, polybutyrene terephthalate, polyethylene terephthalate, polyethylene, polypropylene, polyisobutylene, polyisoprene, polybutene, poly (p-xylene), polychloride butyl, Polyvinylidene chloride, polycarbonate, modified polyphenylene ether, polyurethane, polydimethylsiloxane, polyvinyl acetate, polystyrene, polymethyl acrylate, polymethyl methacrylate, ABS resin, polyphenylene sulfide, polyetherenoate Zoleketone, polyester Polyphenylene / refined ketone, Polyphenylene sulfide sulfone, Polyethylene ternitrile, wholly aromatic polyester, Fluororesin, Polyarylate, Polysulfone, Polyether sulfone, Polyetherimide, Polyamide imide, Polyimide, Polyaminobismaleide, Examples include
- fluororesin examples include tetrafluoroethylene / hexafluoropropylene copolymer, tetrafluoroethylene / perfluoroalkylbier ether copolymer, polyclonal trifluoroethylene, polyvinylidene fluoride, and fluoroethylene.
- Vinylidene hexafluoropropylene / tetrafluoroethylene copolymer polyfluorinated vinyl, ethylene-no-tetraf / rho-ethylene copolymer, ethylene / chlorotrifluoroethylene copolymer, propylene / tetrafluoroethylene copolymer Polymer, Tet Fluoroalkyl perfluorovinyl ether copolymer, vinylidene fluoride / hexafluoropropylene copolymer, vinylidene fluoride Z-mouth trifluoroethylene copolymer, tetrafluoroethylene / ethylene / Examples include an isobutylene copolymer, an ethylene / hexafluoropropylene copolymer, and a tetrafluoroethylene / ethyl vinyl ether copolymer.
- thermoplastic resins can be used alone or in combination of two or more.
- the mixing ratio of the thermoplastic resin is usually 100 parts by weight of the thermosetting resin (for example, an epoxy resin component containing an epoxy compound having two or more epoxy groups in one molecule and a curing agent). It is 50 parts by weight or less, preferably 30 parts by weight or less, more preferably 20 parts by weight or less.
- the sealing resin composition of the present invention can contain other various additives as necessary.
- Other additives include, for example, a release agent such as a natural wax; an impact modifier such as an epoxy group-containing ⁇ -olefin copolymer; a resin modifier such as ethylene dalicydyl methacrylate; zinc carbonate; Mold corrosion inhibitor such as pentaerythritol tetrastearate; thermosetting Resin; antioxidant; ultraviolet absorber; nucleating agent such as boron nitride; flame retardant such as bromide; flame retardant auxiliary such as antimony trioxide; coloring agent such as dye and pigment; Activator; wetting enhancer such as silicone oil; and the like.
- a release agent such as a natural wax
- an impact modifier such as an epoxy group-containing ⁇ -olefin copolymer
- a resin modifier such as ethylene dalicydyl methacrylate
- zinc carbonate zinc carbonate
- Mold corrosion inhibitor such as pentaery
- the sealing resin and composition of the present invention When the sealing resin and composition of the present invention are in a liquid state, they can be produced by sufficiently mixing the respective raw materials with a stirring and mixing device such as a Henschel mixer.
- the mixing temperature is usually in the range of 20 to 60 ° C.
- the encapsulating resin composition is a powder (compound), it is prepared by uniformly mixing the components with a high-speed mixer or the like and then sufficiently kneading with a two-roll or continuous kneading device. be able to.
- the kneading temperature is usually about 30 to: L 20 ° C.
- the sealing resin composition of the present invention can increase the filling rate of the filler.
- the total proportion of the filler composed of the carbon precursor, the conductive filler, and the other inorganic filler is preferably 60 to 93% by weight, more preferably 70 to 90% by weight, based on the total amount of the resin composition. % By weight.
- properties such as surface resistivity, heat resistance, mechanical strength, dimensional stability, and chemical resistance can be highly balanced.
- the surface resistivity of a sample represents the resistance per unit surface area, and its unit is ⁇ , but in order to distinguish it from mere resistance, it is expressed as ⁇ port or ⁇ / sq. Express.
- the surface resistivity is a value measured by the method described in Examples.
- the solidified or cured product of the encapsulating resin composition of the present invention has a small variation in surface resistivity depending on the location.
- the resin composition for sealing of the present invention can be used for resin sealing of electronic parts and electric parts.
- the sealing resin composition of the present invention is particularly preferably used for resin sealing of a semiconductor element.
- a transfer molding method, a dive method, Hardening molding can be performed by a known molding method such as a potting method, a powder flowing immersion method, an underfill method for mounting a clip chip, a compression molding method, and an injection molding method.
- a resin-sealed semiconductor device can be obtained.
- the encapsulating resin composition of the present invention has a high filling factor of a filler and is solid at room temperature, it is preferable to manufacture a resin-sealed semiconductor device by a transfer molding method or an injection molding method.
- the sealing epoxy resin composition is molded into an epoxy tablet (B-stage solid), and the epoxy tablet is formed.
- the sealing epoxy resin composition is molded into an epoxy tablet (B-stage solid), and the epoxy tablet is formed.
- curing is performed at 150 to 180 ° C, preferably at 160 to 180 ° C, for 30 to 180 seconds, and then at 150 to 180 ° C, preferably.
- post cure post-curing
- the sealing is performed. It is possible to adopt a method of coating, printing, or flowing the resin composition for use at least to cover the semiconductor element and the wiring portion of the wiring donating member, and solidify or cure this. it can.
- the use of the encapsulating resin composition of the present invention can increase the adhesion to the metal surface of a semiconductor element or a wiring-providing member on which a wiring such as an electrode or a circuit is formed and improve the moisture resistance.
- Semiconductor devices manufactured using the encapsulating resin composition of the present invention have high reliability such as moisture resistance and heat cycle resistance, and are also excellent in bending resistance, impact resistance, vibration resistance, and the like. ing. Therefore, the resin sealing of the present invention Extremely high reliability can be obtained even when the semiconductor device thus manufactured is used in electronic devices in the form of cards, portable information devices, and the like.
- the surface resistivity was measured at an applied voltage of 100 V using a Hiresta UP (UR-SS probe) manufactured by Mitsubishi Chemical Corporation.
- a plate-shaped molded product (3 OmmX 3 OmmX 1 mm thick) obtained by injection-molding a resin composition by a transfer molding machine was used as a measurement sample.
- the surface resistivity was measured at five points of the plate-like molded body.
- the surface resistivity was represented by the average value.
- the oxidized pitch was pulverized and further sieved with a mesh having an opening of about 50 / zm to remove particles having a size of 50 ⁇ or more.
- 13 g of the crushed oxidized pitch powder was filled in a cylindrical mold having a cross section of 80 cm 2 and molded at a pressure of 196 MPa to obtain a molded body.
- This molded body was heat-treated in a nitrogen stream at 580 ° C. for 1 hour, which is the same temperature as the heat treatment temperature in the above-described method for producing carbon precursor particles, to obtain a carbon precursor volume resistivity sample (molding). Body).
- the volume resistivity of this sample was measured according to JISK 7194. As a result, the volume resistivity of the carbon precursor was 3 X 1 0 7 ⁇ ⁇ cm .
- a softening point of 210 ° C, a quinoline insoluble content of 1% by weight, an H / C atomic ratio of 0.63, 68 kg of petroleum-based pitch and 32 kg of naphthalene were added to an inner volume of 300 kg with stirring blades.
- the mixture was charged in a pressure vessel of a liter, heated to 190 ° C., melted and mixed, then cooled to 80 to 90 ° C. and extruded to obtain a string-shaped molded body having a diameter of about 500 m.
- this cord-like molded body was powder-framed so that the ratio of the diameter to the length was about 1.5, and the obtained pulverized material was heated to 93 ° C. with 0.53% of polybutyl alcohol ( (Saponification degree: 88%) It was dropped into an aqueous solution, stirred and dispersed, and cooled to obtain a spherical pitch molded body.
- n_hexane as that of the spherical pitch compact.
- the spherical pitch formed body thus obtained was oxidized while being kept at 260 ° C. for 1 hour while passing heated air to obtain an oxidized pitch.
- the oxide pitch was heat-treated for 1 hour in a nitrogen gas stream 5 5 0 ° C, milled, average particle diameter of a carbon precursor particles of about 1 0 ⁇ ⁇ . Before this carbon The carbon content of the precursor particles was 91.0% by weight.
- the oxidized pitch was pulverized and sieved with a mesh having an opening of about 50 ⁇ to remove particles of 50 Aim or more.
- 13 g of the crushed oxidized pitch powder was filled in a cylindrical mold having a cross-sectional area of 80 cm 2 and molded at a pressure of 196 MPa to obtain a molded body.
- This molded body was heat-treated in a nitrogen stream at 580 ° C for 1 hour, which is the same temperature as the heat treatment temperature in the above-described method for producing carbon precursor particles. ) Got.
- the volume resistivity of this sample was measured according to JIS K7194. As a result, the volume resistivity of the carbon precursor was 8 ⁇ 10 8 ⁇ ⁇ cm.
- Epoxy resin (A) (Biphenyl type epoxy resin; manufactured by Yuka Shell Co., Ltd., trade name “Epicoat YX4000HK:”] 47 parts by weight, epoxy resin (A 2 ) [brominated cresol nopolak type epoxy resin; Nippon Kayaku Co., Ltd.
- epoxy resin component 100 parts by weight of epoxy resin component, including 48 parts by weight of a hardener [Phenol nopolak resin; product name of “DL-92” manufactured by Meiwa Kasei Co., Ltd.] 0.8 parts by weight, 5 parts by weight of antimony trioxide, 2 parts by weight of carnauba wax (release agent) , Trifluorenylphosphine (curing accelerator) 1 part by weight, 70 parts by weight of the carbon precursor (B1) obtained in Production Example 1, and spherical amorphous silica (manufactured by Mitsubishi Rayon Co., Ltd., trade name "QS-4") 700 parts by weight to a twin screw extruder Continuously extruded at over temperature 170 ° C, and pellet of.
- the pellet of the epoxy resin composition thus obtained was injected into a mold having a length of 3 Omm, a width of 30 mm, and a thickness of 1 mm using a transfer molding machine, and was thermally cured at 175 ° C for 150 seconds. .
- the obtained plate-shaped molded body was taken out of the mold, and post-cured at 180 ° C. for 5 hours. Thus, a measurement sample was prepared. Table 1 shows the results. Examples 2 to 5
- a measurement sample was prepared in the same manner as in Example 1, except that the components and the mixing ratio were changed as shown in Table 1.
- Table 1 shows the results. '
- Epoxy resin Vib-peel type epoxy resin; manufactured by Yuka Shell Co., Ltd., trade name "Epicoat YX4000HK:",
- Epoxy resin (A 2 ) brominated cresol nopolak type epoxy resin; manufactured by Nippon Kayaku Co., Ltd., trade name “BREN-105”,
- Curing agent phenol nopolak resin; manufactured by Meiwa Kasei Co., Ltd., trade name "DL_92",
- Silane coupling agent manufactured by Toray Dako Co., Ltd., trade name “SZ—608 3”,
- Carbon precursor (B 1) volume resistivity 3 ⁇ 10 7 ⁇ ⁇ cm, carbon content 91.0% by weight,
- Carbon precursor (B 2) volume resistivity 8 ⁇ 10 8 ⁇ ⁇ cm, carbon content 91.0% by weight,
- carbon fiber manufactured by Toray Industries, Inc., trade name "Tre force MLD30", volume resistivity less than 10 2 Omega ⁇ cm, average diameter 7 mu m, average fiber length 30 / xm,
- conductive carbon black manufactured by Mitsubishi Chemical Corporation, trade name "MA- 100", the volume resistivity of less than 10 2 ⁇ ⁇ cm.
- the surface resistivity of the encapsulated molded product (cured product) can be controlled by ESD by incorporating a carbon precursor into the epoxy resin component (Examples 1 to 5). It can be controlled within the range of 10 5 to 10 13 ⁇ / mouth of the semiconductive region, and the static decay time can be extremely short.
- the surface resistivity of the cured product was changed within the semiconductive region by changing the mixing ratio of the carbon precursor. It can be controlled to a desired value. From the results of Example 5, it can be seen that the combined use of the carbon precursor and the carbon fiber makes it possible to cure even if the total blending ratio of these is reduced. It can be seen that the surface resistivity of the object can be controlled to a desired value within the semi-conductive region.
- the surface resistivity of a sealed molded product is semiconductive while ensuring electrical insulation.
- the present invention provides a sealing resin composition that can be strictly controlled in a sealing region.
- a semiconductor device such as an electronic device sealed with the sealing resin composition of the present invention is sufficiently protected not only from an external environment such as moisture and light but also from an ESD failure. Therefore, the encapsulating resin composition of the present invention can be used as an encapsulating resin material for electronic components and electric components, and can be particularly suitably applied to resin encapsulation of semiconductor elements.
- a semiconductor device such as an electronic device sealed with the sealing resin composition of the present invention can be used in the technical field of semiconductor.
Abstract
Description
Claims
Priority Applications (5)
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KR1020127008823A KR101238509B1 (ko) | 2004-04-30 | 2005-04-25 | 밀봉용 수지 조성물 및 수지 밀봉된 반도체 장치 |
JP2006512866A JP5165891B2 (ja) | 2004-04-30 | 2005-04-25 | 封止用樹脂組成物及び樹脂封止された半導体装置 |
US11/587,479 US8642682B2 (en) | 2004-04-30 | 2005-04-25 | Resin composition for encapsulation and semiconductor unit encapsulated with resin |
KR1020067025126A KR101191541B1 (ko) | 2004-04-30 | 2005-04-25 | 밀봉용 수지 조성물 및 수지 밀봉된 반도체 장치 |
US13/396,989 US8860233B2 (en) | 2004-02-16 | 2012-02-15 | Resin composition for encapsulation and semiconductor unit encapsulated with resin |
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JP2004135324 | 2004-04-30 | ||
JP2004-135324 | 2004-04-30 |
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US10/587,479 A-371-Of-International US20070149437A1 (en) | 2004-01-30 | 2005-01-28 | Production processes and systems, compositions, surfactants, monomer units, metal complexes, phosphate esters, glycols, aqueous film forming foams, and foams stabilizers |
US13/396,989 Continuation US8860233B2 (en) | 2004-02-16 | 2012-02-15 | Resin composition for encapsulation and semiconductor unit encapsulated with resin |
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WO2005105919A1 true WO2005105919A1 (ja) | 2005-11-10 |
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US (2) | US8642682B2 (ja) |
JP (2) | JP5165891B2 (ja) |
KR (1) | KR101238509B1 (ja) |
CN (1) | CN100441619C (ja) |
TW (1) | TWI388617B (ja) |
WO (1) | WO2005105919A1 (ja) |
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2012
- 2012-02-08 JP JP2012024870A patent/JP5341218B2/ja not_active Expired - Fee Related
- 2012-02-15 US US13/396,989 patent/US8860233B2/en not_active Expired - Fee Related
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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JPWO2007055338A1 (ja) * | 2005-11-11 | 2009-04-30 | 日立化成工業株式会社 | 樹脂成形材料 |
JP4957554B2 (ja) * | 2005-11-11 | 2012-06-20 | 日立化成工業株式会社 | 樹脂成形材料 |
EP1970953A1 (de) * | 2007-03-10 | 2008-09-17 | Klaus-Peter Bergmann | Vergossene Elektroanordnung und Verfahren zum Vergießen einer wenigstens ein Elektrobauteil aufweisenden Elektroanordnung |
WO2015025661A1 (ja) * | 2013-08-21 | 2015-02-26 | 日東電工株式会社 | 封止用シート、及び、半導体装置の製造方法 |
JP2017512361A (ja) * | 2014-02-18 | 2017-05-18 | エルジー・ケム・リミテッド | 封止フィルム及びこれを含む有機電子装置 |
US10096797B2 (en) | 2014-02-18 | 2018-10-09 | Lg Chem, Ltd. | Encapsulation film and organic electronic device comprising the same |
US10181577B1 (en) | 2014-02-18 | 2019-01-15 | Lg Chem, Ltd. | Encapsulation film and organic electronic device comprising the same |
US10720600B2 (en) | 2014-02-18 | 2020-07-21 | Lg Chem, Ltd. | Encapsulation film and organic electronic device including the same |
Also Published As
Publication number | Publication date |
---|---|
JP2012097282A (ja) | 2012-05-24 |
JPWO2005105919A1 (ja) | 2008-03-13 |
KR101238509B1 (ko) | 2013-03-04 |
US8642682B2 (en) | 2014-02-04 |
TW200540221A (en) | 2005-12-16 |
US20120146248A1 (en) | 2012-06-14 |
US8860233B2 (en) | 2014-10-14 |
CN1950447A (zh) | 2007-04-18 |
KR20120051088A (ko) | 2012-05-21 |
CN100441619C (zh) | 2008-12-10 |
JP5341218B2 (ja) | 2013-11-13 |
TWI388617B (zh) | 2013-03-11 |
JP5165891B2 (ja) | 2013-03-21 |
US20080242768A1 (en) | 2008-10-02 |
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