CN1970673A - Material for connecting circuit - Google Patents

Material for connecting circuit Download PDF

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Publication number
CN1970673A
CN1970673A CNA2006101468870A CN200610146887A CN1970673A CN 1970673 A CN1970673 A CN 1970673A CN A2006101468870 A CNA2006101468870 A CN A2006101468870A CN 200610146887 A CN200610146887 A CN 200610146887A CN 1970673 A CN1970673 A CN 1970673A
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China
Prior art keywords
circuit
methyl
radical polymerization
polymerization initiator
compound
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CNA2006101468870A
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Chinese (zh)
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CN1970673B (en
Inventor
加藤木茂树
须藤朋子
伊泽弘行
汤佐正己
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Showa Denko Materials Co ltd
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Hitachi Chemical Co Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H3/00—Toothed gearings for conveying rotary motion with variable gear ratio or for reversing rotary motion
    • F16H3/44—Toothed gearings for conveying rotary motion with variable gear ratio or for reversing rotary motion using gears having orbital motion
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H55/00—Elements with teeth or friction surfaces for conveying motion; Worms, pulleys or sheaves for gearing mechanisms
    • F16H55/02—Toothed members; Worms
    • F16H55/08—Profiling
    • F16H55/0806—Involute profile
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H55/00—Elements with teeth or friction surfaces for conveying motion; Worms, pulleys or sheaves for gearing mechanisms
    • F16H55/02—Toothed members; Worms
    • F16H55/08—Profiling
    • F16H2055/0866—Profiles for improving radial engagement of gears, e.g. chamfers on the tips of the teeth
    • 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
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • 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
    • H01L2924/01079—Gold [Au]
    • 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
    • H01L2924/078—Adhesive characteristics other than chemical
    • H01L2924/0781—Adhesive characteristics other than chemical being an ohmic electrical conductor
    • H01L2924/07811—Extrinsic, i.e. with electrical conductive fillers
    • 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
    • H01L2924/095—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00 with a principal constituent of the material being a combination of two or more materials provided in the groups H01L2924/013 - H01L2924/0715
    • H01L2924/097—Glass-ceramics, e.g. devitrified glass
    • H01L2924/09701—Low temperature co-fired ceramic [LTCC]
    • 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
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/102—Material of the semiconductor or solid state bodies
    • H01L2924/1025—Semiconducting materials
    • H01L2924/10251—Elemental semiconductors, i.e. Group IV
    • H01L2924/10253—Silicon [Si]

Abstract

This invention provides an adhesive composition rapidly carrying out a radical polymerization reaction at a low temperature, having a wide process margin, excellent adhesive strength and connection resistance and further excellent storage stability and to provide a material for connecting circuits, a connecting structure of circuit members and a semiconductor device. The adhesive composition solving the problems comprises a thermoplastic resin, a radically polymerizable compound, a first radical polymerization initiator having 90-145 DEG C half-life temperature for 1 min and a second radical polymerization initiator having 150-175 DEG C half-life temperature for 1 min.

Description

Circuit connection material
The application is to be on May 9th, 2005 applying date of original application, and application number is 200510069479.5, and denomination of invention is divided an application for the Chinese patent application of " syndeton of adhesive compound, circuit connection material, circuit block and semiconductor device ".
Technical field
The present invention relates to the syndeton and the semiconductor device of adhesive compound, circuit connection material, circuit block.
Background technology
In the past, as the tackiness agent of semiconductor element and used for liquid crystal display element, even use excellent in adhesion, particularly under hot and humid condition, also show the thermosetting resins such as Resins, epoxy (for example opening flat 01-113480 communique) of excellent cementability with reference to the spy.Such tackiness agent obtains cementability by solidifying in 1～3 hour 170～250 ℃ temperature heating.
In recent years, along with the height highly integrated, liquid crystal cell of semiconductor element becomes more meticulous, narrow and smallization of the spacing of interelement and wiring closet develops.When such semiconductor element etc. is used above-mentioned tackiness agent, because Heating temperature height and curing speed when solidifying are also slow, so, tend to cause the influences such as damage of circumferential component not only at desirable connecting portion but also can be heated to circumferential component.In order further to reduce cost, be necessary to make productivity to improve, require low temperature (100～170 ℃), short period of time (1 hour or its in), in other words " low temperature fast setting " is bonding.
On the other hand, receive publicity in recent years and with acrylate derivative or methacrylate derivative and as the radical-curable tackiness agent of the superoxide of radical polymerization initiator.This tackiness agent, utilize with reactive excellent free radical as the reactive behavior kind carry out polyreaction solidify, bonding, therefore can solidify (for example opening the 2000-203427 communique) with the short time with reference to the spy.
But the radical-curable tackiness agent is reactive excellent, and therefore the technology amplitude that is cured when handling has the tendency that narrows down.For example, for being electrically connected semiconductor element or liquid crystal display device when using above-mentioned radical-curable tackiness agent, even the processing condition such as temperature and time when obtaining its cured article change a little, the tendency that can not stably obtain bonding strength, connect characteristics such as resistance is just arranged.
Summary of the invention
Therefore, the invention provides and can be very promptly be cured the technology amplitude broad of handling and being cured when handling, the syndeton and the semiconductor device that can access very stable bonding strength and the adhesive compound that is connected resistance, circuit connection material, circuit block with low temperature.
Solve the adhesive compound of the present invention of above-mentioned problem, it is characterized in that, contain thermoplastic resin, free-radical polymerised compound, 1 minute half life temperature and be second radical polymerization initiator that 90～145 ℃ first radical polymerization initiator and 1 minute half life temperature are 150～175 ℃.
Here, so-called " 1 minute half life temperature " is meant that the transformation period becomes 1 minute temperature, and so-called " transformation period " is meant that compound concentrations reduces to the time of a half of initial value.
Adhesive compound of the present invention is the so-called radical-curable adhesive compound that contains thermoplastic resin and free-radical polymerised compound and radical polymerization initiator.The adhesive compound that contains free-radical polymerised compound like this is reactive excellent, even therefore also can solidify with the very short time at low temperatures.And then, by using the different radical polymerization initiator of two kinds of 1 minute half life temperatures, can enlarge the technology amplitude that is cured when handling as radical polymerization initiator.Therefore, the cured article that obtains from such adhesive compound is even technological temperature or time change when obtaining this cured article also can make bonding strength and be connected stability of characteristics such as resistance.In addition, also can suppress the cured article characteristic decline of intersexuality at any time.
And 1 minute half life temperature is at the radical-curable tackiness agent of above-mentioned scope, and general activation energy is low, so the tendency of poor storage stability is arranged.But, from the cured article that adhesive compound of the present invention obtains, compare with material in the past, can also possess excellent more stability in storage.People of the present invention think that this is a cause of using two kinds of different radical polymerization initiators of 1 minute half life temperature in adhesive compound of the present invention.
In addition, if use adhesive compound of the present invention, then can be cured processing and can enlarge the technology amplitude with the short period of time, so, even narrow and smallization of spacing of the interelement of semiconductor element and liquid crystal cell etc. and wiring closet, also can prevent not only at desirable connecting portion but also be heated to circumferential component and, can boost productivity causing the phenomenon of influences such as circumferential component damage.
In addition, in the adhesive compound of the present invention, free-radical polymerised compound preferably has two or (methyl) acryl more than it at intramolecularly.If use such adhesive compound, then can be cured processing with shorter time.The inventor infer this be free-radical polymerised compound have two or its above be imbued with the i.e. cause of (methyl) acryl of reactive free radical reaction group.
Also have, such free-radical polymerised compound, because use (methyl) acryl as reactive group, so, can obtain and the firm cementability that is had nothing to do by the material of bonding object.Therefore, contain the adhesive compound of the present invention of such free-radical polymerised compound, the versatility excellence when for example being used for semiconductor element or liquid crystal display device, also can obtaining more stable bonding strength and be connected characteristics such as resistance.
And then, first radical polymerization initiator and second radical polymerization initiator, all preferably molecular weight is 180～1000 peroxy esters derivative.
If first radical polymerization initiator and second radical polymerization initiator all are congener peroxy esters derivatives and are the molecular weight in the above-mentioned numerical range, intermiscibility excellence each other then is so the cured article that obtains just shows the bonding strength that its integral body is more stable or connects characteristic such as resistance.
In addition, adhesive compound of the present invention to 100 mass parts thermoplastic resins, preferably contains 50～250 mass parts free-radical polymerised compounds, and contains 0.05～30 mass parts, first radical polymerization initiator and second radical polymerization initiator respectively.This adhesive compound of the present invention contains this structured material by the blending ratio with above-mentioned scope, can bring into play effect of the present invention more significantly.
Further, in this adhesive compound, preferably contain electroconductive particle.Such adhesive compound just can have electroconductibility.Like that, this adhesive compound can be used as electrically conductive adhesive in electrical industry such as circuit electrode and semi-conductor and electronics industry and uses.And then, at this moment, because adhesive compound is an electroconductibility, so can reduce connection resistance after the curing more.
In addition, to the blending ratio of this electroconductive particle, to 100 mass parts thermoplastic resins, preferably contain the electroconductive particle of 0.5～30 mass parts.Contain electroconductive particle by the blending ratio with above-mentioned scope, such adhesive compound can be brought into play the effect of electroconductive particle more.When for example being used for the connection of circuit electrode, can prevent the phenomenon of non-conductive or adjacent circuit inter-electrode short-circuit between opposed circuit electrode.Further, contain the adhesive compound of electroconductive particle, can also show the anisotropy of electrical connection, can be used as the anisotropic conductive adhesive compound with above-mentioned blending ratio.
Also have, circuit connection material of the present invention is in order to be electrically connected the circuit connection material between the opposed circuit electrode, to it is characterized by, and circuit connection material contains above-mentioned adhesive compound.
Such circuit connection material even also can carry out bonding between the opposed circuit electrode with the very short time at low temperature, also can enlarge the technology amplitude.Further, the cured article that obtains from such circuit connection material is even technological temperature or time change when obtaining its cured article also can make bonding strength or connect stability of characteristics such as resistance.And, also can suppress the cured article characteristic decline of intersexuality at any time.Further,, then can show the anisotropy of electrical connection, also can be used as circuit electrode anisotropic conductive circuit connection material if this circuit connection material contains electroconductive particle with above-mentioned blending ratio.
In addition, above-mentioned adhesive compound or circuit connection material are preferably formed to membranaceous.Because make membranaceous adhesive compound or circuit connection material operability excellence, so can further boost productivity.
Also have, the syndeton of circuit block of the present invention, its be possess first circuit block that forms first circuit electrode on the interarea of first circuit substrate, the second circuit parts that form the second circuit electrode on the interarea of second circuit substrate, be arranged at first circuit substrate the interarea of interarea and second circuit substrate between and the syndeton of the circuit block of circuit connecting section part that first circuit electrode and second circuit electrode are electrically connected with the state of arranged opposite, it is characterized in that the circuit connecting section part is the cured article that foregoing circuit connects material.
The syndeton of such circuit block can effectively utilize the circuit electrode of electrical connection.That is, can be electrically connected first circuit electrode and be connected material with the foregoing circuit of second circuit electrode because use, so, the circuit block with syndeton of the present invention, quality fluctuation is few, can show the ten minutes stable properties.And then, when the circuit connection material cured article contains electroconductive particle, can reduce connection resistance.By mixing this electroconductive particle, can prevent the phenomenon of non-conductive or adjacent circuit inter-electrode short-circuit between opposed circuit electrode.In addition,, then can show the anisotropy of electrical connection, also can connect material as the anisotropy circuit if contain electroconductive particle with above-mentioned blending ratio.
In addition, semiconductor device of the present invention, be the substrate that possesses semiconductor element, semiconductor element mounted thereon, be arranged between semiconductor element and the substrate and be electrically connected the semiconductor device of the semiconductor element interconnecting piece of semiconductor element and substrate, it is characterized in that the semiconductor element interconnecting piece is the cured article or the membranaceous tackiness agent of above-mentioned adhesive compound.
Such semiconductor device is the cured article of above-mentioned adhesive compound because be electrically connected the cured article of the adhesive compound of semiconductor element and substrate, so quality fluctuation is few, can show very stable properties.And then, when the cured article of adhesive compound contains electroconductive particle, can reduce connection resistance.By mixing this electroconductive particle, can prevent nonconducting phenomenon between opposed semiconductor element and substrate.In addition,, then demonstrate the anisotropy of electrical connection, can also be used as anisotropic semiconductor if contain electroconductive particle with above-mentioned blending ratio.
Description of drawings
Fig. 1 is the summary sectional view of an example of the syndeton of expression circuit block of the present invention.
Fig. 2 is the summary sectional view of an example of expression semiconductor device of the present invention.
Embodiment
Below, the embodiment that the present invention suits with reference to description of drawings according to circumstances.Wherein, same key element is used prosign, omit repeat specification.In addition, in the following description, so-called (methyl) acrylate, expression acrylate or the methacrylic ester corresponding with it.
＜adhesive compound 〉
Adhesive compound of the present invention contains thermoplastic resin, free-radical polymerised compound, 1 minute half life temperature and is second radical polymerization initiator that 90～145 ℃ first radical polymerization initiator and 1 minute half life temperature are 150～175 ℃.
Here, the thermoplastic resin that the present invention is correlated with is used to make bonding between the bonding target compound (being designated hereinafter simply as " by bonding object ") to become firm.
Thermoplastic resin as using among the present invention has no particular limits, can use known material.Specifically, can use polymeric amide, phenoxy resin class, poly-(methyl) esters of acrylic acid, polyimide, polyurethanes, polyester, polyvinyl butyral acetal class etc.These resins can separately or mix two kinds or its above use.And then these resins also can have siloxane bond or fluoro substituents at intramolecularly.If mix fully between the blended resin or produce microphase-separated and become muddy state, these can use aptly.
In addition, the molecular weight of this thermoplastic resin more greatly, more can easily form film described later, and, can also set the dissolve viscosity of influence at wide region as the flowability of tackiness agent.If can set at wide region and dissolve viscosity, then when being used for the connection of semiconductor element or liquid crystal cell etc., even narrow and smallization of spacing of interelement and wiring closet, can prevent further that also tackiness agent is attached to the phenomenon on the circumferential component, productivity is improved.Just, if the value of this molecular weight is greater than 150000, just have a tendency with the intermiscibility variation of other composition, and if less than 5000, just have film to form inadequate tendency when using as film described later.Therefore, this molecular weight is in weight-average molecular weight, preferably 5000～150000, be more preferably 10000～80000.
In addition, the free-radical polymerised compound that so-called the present invention is correlated with is meant to have by giving certain energy to produce free radical and this free radical form polymer properties according to the chain reaction polymerization compound.This Raolical polymerizable generally more promptly reacts than cationoid polymerisation or anionoid polymerization.Therefore, use among the present invention of free-radical polymerised compound, can be with relatively shorter time aggregation.
Free-radical polymerised compound as the present invention uses if having the compound of alkenyl in (methyl) propenyl, (methyl) acryl or the vinyl equimolecular, just can use known material ad lib.The free-radical polymerised compound that wherein preferably has (methyl) acryl.
Specifically; as free-radical polymerised compound with (methyl) acryl; can enumerate epoxy (methyl) origoester acrylate; ammonia ester (methyl) origoester acrylate; polyethers (methyl) origoester acrylate; oligopolymer such as polyester (methyl) origoester acrylate; trimethylolpropane tris (methyl) acrylate; polyoxyethylene glycol two (methyl) acrylate; polyalkylene glycol two (methyl) acrylate; dicyclopentenyl (methyl) acrylate; two cyclopentenes oxygen ethyl (methyl) acrylate; neopentyl glycol two (methyl) acrylate; Dipentaerythritol six (methyl) acrylate; isocyanuric acid modification two senses (methyl) acrylate; isocyanuric acid modification trifunctional (methyl) acrylate; 2,2 '-two (methyl) acryloxy diethyl phosphoric acid ester; multifunctional (methyl) acrylic compound such as 2-(methyl) acryloxy ethyl phosphate ester acid etc.These compounds also can individually or mix two kinds or its above use as required.
If use (methyl) acryl in this wise as reactive group, just can be with irrelevant bonding securely by the material of bonding object.As by bonding object, can enumerate with metal and ITO (indium tin oxide, indium tin oxide), silicon nitride (SiN such as the copper headed by the organic substrates such as printed-wiring board (PWB) and polyimide, aluminium x), silicon-dioxide (SiO 2) etc.
And then, if free-radical polymerised compound has two or (methyl) acryl more than it at its intramolecularly, just can further shorten bonding needed heat-up time, further reduce bonding needed Heating temperature, so be preferred.Can think that this is that the intramolecularly of free-radical polymerised compound has more the cause as (methyl) acryl of free radical reaction group.
The blending ratio of this free-radical polymerised compound, for 100 parts of thermoplastic resins, preferably 50～250 mass parts, be more preferably 60～150 mass parts.If the blending ratio of free-radical polymerised compound is less than 50 mass parts, give the tendency that decline is just arranged by the thermotolerance of the adhesive compound cured article of bonding object, if greater than 250 mass parts, just have film to form the inadequate tendency that becomes when adhesive compound is used as film described later.
In addition, adhesive compound of the present invention contains radical polymerization initiator.Free-radical polymerised compound, Once you begin Raolical polymerizable just carries out chain reaction, realizes firm curing, but because make relatively difficulty of free-radical generating at first, can be so contain than the radical polymerization initiator that is easier to generate free radical.
Among the present invention,, and be second radical polymerization initiator that 90～145 ℃ first radical polymerization initiator and 1 minute half life temperature are 150～175 ℃ with 1 minute half life temperature as radical polymerization initiator.
As the first such radical polymerization initiator, if 1 minute half life temperature is 90～145 ℃, then can uses known compound, as second radical polymerization initiator, if 1 minute half life temperature is 150～175 ℃, then can uses known compound.
Wherein, first radical polymerization initiator and second radical polymerization initiator all are preferably the peroxy esters derivative.If all be the peroxy esters derivative, mutual intermiscibility excellence then is so it wholely shows the cured article that obtains more stable bonding strength and be connected characteristic such as resistance.
As first radical polymerization initiator, specifically can enumerate peroxidation neodecanoic acid cumyl ester, peroxidation neodecanoic acid-1,1,3,3-tetramethyl-butyl ester, 1-cyclohexyl-1-methylethyl peroxidation ester in the new last of the ten Heavenly stems, the own ester of peroxidation neodecanoic acid uncle, new peroxide tert-butyl caprate, the peroxidation trimethylacetic acid tert-butyl ester, peroxidation-2 ethyl hexanoic acid-1,1,3,3-tetramethyl-butyl ester, 2,5-dimethyl-2,5-two (peroxidation-2-ethyl hexanoyl) hexane, peroxidation-own the ester of 2 ethyl hexanoic acid uncle, peroxide-2-ethyl hexanoic acid tert-butyl, the new enanthic acid tert-butyl ester of peroxidation, peroxidation-2 ethyl hexanoic acid tert-pentyl ester, peroxidation hexahydroterephthalic acid di tert butyl carbonate, peroxidation-3,5,5-tri-methyl hexanoic acid tert-pentyl ester, peroxidation neodecanoic acid-3-hydroxyl-1,1-dimethyl butyl ester, peroxidation-2 ethyl hexanoic acid 1,1,3,3-tetramethyl-butyl ester, peroxidation tert-pentyl ester in the new last of the ten Heavenly stems, peroxidation-2 ethyl hexanoic acid tert-pentyl ester, 2,2 '-azo-two-(2, the 4-methyl pentane nitrile), 1,1 '-azo-two-(1-acetoxyl group-1-phenylethane), 2,2 '-Diisopropyl azodicarboxylate, 2,2 '-azo-two-(2-methylbutyronitrile), dimethyl-2,2 '-Diisopropyl azodicarboxylate, 4,4 '-azo two (4-cyanopentanoic acid), 1,1 '-azo two (1-cyclohexanenitrile).
And, as second radical polymerization initiator, specifically can enumerate the own ester of peroxidation sec.-propyl list carbonic acid uncle, the peroxidation toxilic acid tert-butyl ester, peroxidation-3,5, the 5-tri-methyl hexanoic acid tert-butyl ester, the peroxidation lauric acid tert-butyl ester, 2,5-dimethyl-2,5-two-(peroxidation-3-toluyl) hexane, peroxidation-2-ethylhexyl list carbonic acid the tert-butyl ester, the own ester of peroxidation phenylformic acid uncle, 2,5-dimethyl-2,5-two-(benzoyl peroxide) hexane, peroxidized t-butyl perbenzoate, peroxidation trimethyladipic acid dibutylester, peroxidation n-caprylic acid tert-pentyl ester, the different n-nonanoic acid tert-pentyl ester of peroxidation, peroxide acid tert-amyl acetate etc.
In addition, adhesive compound of the present invention can be also with first radical polymerization initiator and second radical polymerization initiator, also can use two kinds or its first above radical polymerization initiator, also can use two kinds or its second above radical polymerization initiator.
The molecular weight of first radical polymerization initiator and second radical polymerization initiator is in weight-average molecular weight preferably 180～1000.If first radical polymerization initiator and second radical polymerization initiator all are the molecular weight in the above-mentioned numerical range, intermiscibility excellence then, therefore the cured article that obtains demonstrates more stable bonding strength and is connected characteristic such as resistance in its integral body.
The addition of first radical polymerization initiator and second radical polymerization initiator, for 100 parts of thermoplastic resins, preferably one of them is 0.05～30 mass parts, more preferably the both is 0.05～30 mass parts.In addition, especially preferably all be 0.1～20 mass parts.If the addition of any one party of first radical polymerization initiator and second radical polymerization initiator is less than 0.05 mass parts, just there is radical polymerization to cause inadequate tendency, if the addition of any one party of first radical polymerization initiator and second radical polymerization initiator is greater than 30 mass parts, stability in storage just has the tendency of decline.
In addition, among the present invention, there is no particular limitation as the form of giving energy, can enumerate heat, electron beam, gamma-rays, ultraviolet ray, infrared rays etc.
Also not clear in detail now about using adhesive compound of the present invention just can obtain the factor of the bonding strength cured article very stable with being connected resistance.But people of the present invention think, are because by using 1 minute two kinds of different radical polymerization initiator of half life temperature, even the processing condition difference still can obtain more stable radical polymerization sum velocity as one of its factor.But factor is not limited thereto.
Adhesive compound of the present invention preferably contains electroconductive particle.By containing electroconductive particle, can give this adhesive compound electroconductibility.Like that, just can be in the field of electrical industry such as circuit electrode and semi-conductor and electronic industry as electrically conductive adhesive.
Here operable electroconductive particle then has no particular limits as long as have the electroconductibility that can obtain being electrically connected, and can enumerate for example metal such as Au, Ag, Ni, Cu, scolding tin and carbon etc.In addition, also can be to be nuclear with dielectric glass, pottery, plastics etc., cover the material of above-mentioned metal or carbon at this nuclear.Wherein, preferable alloy is from as the situation of thermally melting metal, or is the situation that nuclear covers the material of metal or carbon with plastics.At this moment, by heating or pressurization the cured article distortion of adhesive compound will be become and be more prone to, so, in the time of between electrode electrically connected, can increase the contact area of electrode and adhesive compound, improve the electroconductibility between the electrode.
In addition, can also use the booklike particle that further covers the surface of this electroconductive particle with macromolecule resin.If in adhesive compound, add electroconductive particle with the booklike particle state, even increase the combined amount of electroconductive particle, also because be covered with, so can further suppress also can improve the insulativity between the telegraph circuit by contacting and the short circuit of generation between the electroconductive particle by resin coating.In addition, these electroconductive particles and booklike particle also can separately or mix two kinds or its above use.
The average particle diameter of electroconductive particle is from viewpoint dispersed, electroconductibility, preferably 1～18 μ m.The blending ratio of electroconductive particle, relative adhesive compound 100 volume %, preferably 0.1～30 volume %, be more preferably 0.1～10 volume %.If this value is less than 0.1 volume %, just have a tendency that can not fully obtain electroconductibility, if greater than 30 volume %, just the tendency that causes short circuit arranged.In addition, the blending ratio of electroconductive particle (volume %), the volume that is each composition before adhesive compound during with 23 ℃ solidifies is the prerequisite decision, the volume of each composition can become the method for volume by utilizing proportion to convert from weight, or do not dissolve and insolublely rise by this composition and in having added well the containers such as graduated cylinder of the appropriate solvent of wetting this composition (water, alcohol etc.), drop into this composition, obtain from the method that the volume that increases is calculated.
In addition, in the adhesive compound of the present invention, the preferred interpolation with alkoxyl silicone alkane derivatives and silazane is the bonding auxiliary agent of the coupler of representative and driving fit rising agent, flow agent etc.Thus, effect of the present invention can be brought into play more significantly, also better adaptation and operability can be given.Specifically, the preferred compound that adds with following general formula (1) expression.
Figure A20061014688700111
Here, R in the formula, 1, R 2, R 3Independent separately expression hydrogen, carbonatoms are that 1～5 alkyl, carbonatoms are that 1～5 alkoxyl group, carbonatoms are 1～5 carbalkoxy or aryl, R 4Expression hydrogen or methyl, n represents 1～10 integer.
Further, preferred R in this general formula (1) 1Be that carbonatoms is 1～5 alkyl or aryl, R 2With R 3Independently be that carbonatoms is 2～3 alkoxyl group separately, n is 2～4, because its cementability is with to be connected resistance excellent more.In addition, also can separately or mix two kinds or its above compound that uses with general formula (1) expression.
In addition, in addition adhesive compound of the present invention also can add other materials according to application target.For example, also can and use the cementability rising agent of the crosslinking rate raising that makes tackiness agent.Thus, can further improve bonding strength.That is, in free-radical polymerised compound with (methyl) acryl, also can further add have allyl group, the compound of functional group that dimaleoyl imino, vinyl etc. can radical polymerizations.Specifically can enumerate N-vinyl imidazole, N-vinyl pyridine, N-vinyl pyrrolidone, N-vinyl formamide, N-caprolactam, 4, two (the N of 4 '-vinylidene, accelerine), N-vinyl acetamide, N, N-DMAA, N-N-isopropylacrylamide, N, N-diethyl acrylamide etc.In addition, these cementability rising agents can separately or mix two kinds or its above use.
In addition, also can and with the fluidity improving agent of simple function (methyl) acrylate etc.Thus, can make mobile the raising.Specifically; can enumerate tetramethylolmethane (methyl) acrylate; 2-cyanoethyl (methyl) acrylate; cyclohexyl (methyl) acrylate; dicyclopentenyl (methyl) acrylate; two cyclopentenes oxygen base ethyl (methyl) acrylate; 2-(2-oxyethyl group) ethyl (methyl) acrylate; 2-ethoxyethyl group (methyl) acrylate; (methyl) ethyl acrylate; the just own ester of (methyl) vinylformic acid; (methyl) vinylformic acid-2-hydroxyl ethyl ester; (methyl) Propylene glycol monoacrylate; (methyl) isobornyl acrylate; (methyl) isodecyl acrylate; (methyl) Isooctyl acrylate monomer; the positive lauryl of (methyl) vinylformic acid; (methyl) vinylformic acid 2-methoxyl group ethyl ester; 2-phenoxy group ethyl (methyl) acrylate; tetrahydrofurfuryl alcohol (methyl) acrylate; 2-(methyl) acryloxy ethyl phosphonic acid ester; N; N-dimethyl aminoethyl (methyl) acrylate; N, N-dimethylaminopropyl (methyl) acrylate; (methyl) acryloyl morpholine.In addition, these fluidity improving agents can separately or mix two kinds or its above use.
Further, also can and use the material of the rubber-like that makes the cementability raising.Also can relax stress thus.Specifically; can enumerate polyisoprene; polyhutadiene; the C-terminal polyhutadiene; the C-terminal polyhutadiene; 1; the 2-polyhutadiene; C-terminal 1; the 2-polyhutadiene; C-terminal 1, the 2-polyhutadiene; acrylic rubber; styrene butadiene rubbers; the C-terminal styrene butadiene rubbers; acrylonitrile-butadiene rubber; contain carboxyl in polymer ends; hydroxyl; the acrylonitrile-butadiene rubber of (methyl) acryl or morpholinyl; carboxylated nitrile rubber; the C-terminal polyoxypropylene; the terminal polyoxypropylene of alkoxysilyl; the polyoxy tetramethylene glycol; the polyalkenes glycol; poly-epsilon-caprolactone.
In addition, rubber type of material is from improving the viewpoint of cementability, preferably at side chain or the terminal high functional group's cyano group of polarity, the rubber type of material of carboxyl of containing, from improving more preferably fraction of mobile viewpoint.Specifically; can enumerate aqueous acrylonitrile-butadiene rubber; contain the aqueous acrylonitrile-butadiene rubber of carboxyl, hydroxyl, (methyl) acryl or morpholinyl, aqueous carboxylated nitrile rubber in polymer ends, more preferably the acrylonitrile content as polar group is 10～60 quality % of these rubber type of material total amounts.In addition, these rubber type of material can separately or mix two kinds or its above use.
And then, also can and be the additives such as stopper of representative in order to tert-butyl catechol, tert.-butyl phenol, p methoxy phenol etc.Can improve stability in storage more thus.
Adhesive compound of the present invention can make pasty state during for liquid at normal temperature and use.When normal temperature is solid, except that pasty state is made in heating, also can use solvent to make pasty state.As operable solvent, so long as with adhesive compound reaction and show that sufficient deliquescent material just has no particular limits, but the boiling point under the preferred normal pressure is 50～150 ℃ a material.If boiling point is lower than 50 ℃, evaporable tendency is easily arranged at room temperature, therefore must under the environment of sealing, carry out polyreaction, and the tendency that is restricted is in the use arranged.In addition, if boiling point is higher than 150 ℃, then solvent evaporates become difficulty, the tendency that can not obtain sufficient adhesion strength is arranged after bonding.
In addition, adhesive compound of the present invention also can be made membranaceous use later on.The manufacture method of this film, on the separability base material of fluororesin film, polyethylene terephthalate film, release paper etc., be coated on the mixed solution that has added solvent in the adhesive compound, perhaps base materials such as non-woven fabrics are soaked into mixed solution and be placed on the separability base material, obtain film by removing to desolvate etc.Like this, adhesive compound is made membranaceous, operability excellence, convenient.
In addition, make film, then can make the anisotropic conductive film if in adhesive compound of the present invention, add electroconductive particle.This anisotropic conductive film is as being placed between the opposite electrode on the substrate, can be bonding can be electrically connected two electrodes the time by heating and pressurizing.Here, the substrate as forming electrode can be suitable for inorganic substance such as semi-conductor, glass, pottery, organism such as polyimide, polycarbonate, the various combinations of these material compound such as glass/epoxy.
And then adhesive compound of the present invention can and come bonding with heating and pressurization.The temperature that Heating temperature is preferred 50～190 ℃.Pressure is not so long as damage by the scope of bonding object and get final product preferred 0.1～10MPa.These heating and pressurization are preferably carried out 0.5～120 second scope.
In addition, adhesive compound of the present invention because can react with the short period of time, stability in storage is also excellent, so suitable to circuit connection material.For example, when being electrically connected the circuit electrode of the circuit electrode of first circuit block and second circuit parts, state with these circuit block arranged opposite is given one of them circuit electrode with adhesive compound of the present invention, and is electrically connected with another circuit electrode by Raolical polymerizable.Like this,, just can be electrically connected with the short period of time if adhesive compound is used as circuit connection material, even carry out technological temperature or time change when bonding, also can stable adhesion intensity be connected characteristics such as resistance.In addition, can also suppress the characteristic reduction of intersexuality at any time of circuit connection material cured article.And then, if this circuit connection material contains electroconductive particle, then can show the anisotropy of electrical connection, the anisotropic conductive circuit connection material that can also use as circuit electrode.
Then, this circuit connection material also can be used as the different inhomogeneity of thermal expansivity by the circuit connection material of bonding object.Specifically can be as being the circuit connection material of representative with anisotropic conductive tackiness agent, silver paste, silverskin etc., can be used as with CSP (chip-scale packing) is the semiconductor element adhesives of representative with elastomerics, CSP with underfilling, LOC (Lead-on-Chip) band etc.
The syndeton of＜circuit block 〉
Then, the suitable embodiment to the syndeton of circuit block of the present invention describes.Fig. 1 is the summary sectional view of an embodiment of the syndeton of expression circuit block of the present invention.As shown in Figure 1, the syndeton 1 of the circuit block of present embodiment possesses opposed mutually first circuit block 20 and second circuit parts 30, between first circuit block 20 and second circuit parts 30, the circuit connecting section part 10 that is electrically connected them is being set.First circuit electrode 22 that first circuit block 20 possesses first circuit substrate 21 and forms on the interarea 21a of circuit substrate 21.And, on the interarea 21a of circuit substrate 21, also can according to circumstances form insulation layer (not illustrating).
On the other hand, the second circuit parts 30 second circuit electrode 32 that possesses second circuit substrate 31 and on the interarea 31a of second circuit substrate 31, form.And, on the interarea 31a of circuit substrate 31, also can according to circumstances form insulation layer (not illustrating).
As first circuit block 20 and second circuit parts 30, just have no particular limits so long as form the electrode that needs to be electrically connected.Specifically can be set forth in ITO that liquid-crystal display uses etc. and form the glass of electrode or plastic base, printed-wiring board (PWB), ceramic wiring board, flexible circuit board, semi-conductor silicon chip etc., these can be used in combination as required.Like this, in this example, can use to comprise printed-wiring board (PWB) and the material that constitutes by organism such as polyimide, metal or ITO (indium tinoxide, indium tin oxide), silicon nitride (SiN such as copper, aluminium x), silicon-dioxide (SiO 2) etc. this circuit block of inorganic materials with varied condition of surface.
Circuit connecting section part 10 contains insulativity material 11 and electroconductive particle 7.Electroconductive particle 7 is not only between opposed first circuit electrode 22 and second circuit electrode 32 but also dispose between interarea 21a and 31a.In the syndeton 1 of the circuit block of present embodiment, first circuit electrode 22 and second circuit electrode 32 is electrically connected by electroconductive particle 7.Therefore, first circuit electrode 22 is reduced fully with the resistance that is connected between the second circuit electrode 32.Thereby, mobile being able to of the electric current between first circuit electrode 22 and the second circuit electrode 32 smoothly can be brought into play the function that circuit has fully.And,, can also show the anisotropy of electrical connection by this electroconductive particle 7 is become above-mentioned blending ratio.
In addition, when circuit connecting section part 10 does not contain electroconductive particle 7,, they are directly contacted or fully closely be electrically connected in order to make the electric current that flows through desired amount between first circuit electrode 22 and the second circuit electrode 32.
Circuit connecting section part 10 is made of the cured article of the circuit connection material that contains above-mentioned adhesive compound, so the bonding strength for the circuit connecting section part 10 of first circuit block 20 or second circuit parts 30 becomes very high, can keep this state over a long time.Thereby, can fully improve the long-term reliability of the electrical characteristic between first circuit electrode 22 and the second circuit electrode 32.
＜semiconductor device 〉
Then, the embodiment to semiconductor device of the present invention describes.Fig. 2 is the summary sectional view of an embodiment of expression semiconductor device of the present invention.As shown in Figure 2, the semiconductor device 2 of present embodiment possesses semiconductor element 50 and becomes the substrate 60 of semi-conductor holding components, between semiconductor element 50 and substrate 60 the semiconductor element interconnecting piece 40 that they are electrically connected is set.And semiconductor element interconnecting piece 40 laminations are on the interarea 60a of substrate 60, and semiconductor element 50 further laminations are on this semiconductor element interconnecting piece 40.
Substrate 60 possesses circuit pattern 61, circuit pattern 61 on the interarea 60a of substrate 60 through semi-conductor interconnecting piece 40 or directly be electrically connected with semiconductor element 50.Then, by sealing material 70 sealings, form semiconductor device 2.
Material as semiconductor element 50 has no particular limits, and can use the various materials of the II-VI compound semiconductor element, CuInSe (ClS) etc. of the III-V compound semiconductor element, HgTe, HgCdTe, CdMnTe, CdS, CdSe, MgSe, MgS, ZnSe, ZeTe etc. of the 4th family's semiconductor element, GaAs, InP, GaP, InGaAs, InGaAsP, AlGaAs, InAs, GaInP, AlInP, AlGaInP, GaNAs, GaNP, GaInNAs, GaInNP, GaSb, InSb, GaN, AlN, InGaN, the InNAsP etc. of silicon, germanium.
Semiconductor element interconnecting piece 40 contains insulativity material 11 and electroconductive particle 7.Electroconductive particle 7 is not only between semiconductor element 50 and the circuit pattern 61, also dispose between semiconductor element 50 and interarea 60a.In the semiconductor device 2 of present embodiment, semiconductor element 50 is electrically connected through electroconductive particle 7 with circuit pattern 61.Therefore, semiconductor element 50 is reduced fully with the resistance that is connected between the circuit pattern 61.Thereby, can flowing of the electric current between semiconductor element 50 and the circuit pattern 61 is level and smooth, can give full play to the function that semi-conductor has.In addition, by this electroconductive particle 7 is become above-mentioned blending ratio, can also show the anisotropy of electrical connection.
In addition, when semiconductor element interconnecting piece 40 does not contain electroconductive particle 7, semiconductor element 50 directly contacted with circuit pattern 61 or fully closely be electrically connected and be connected into the electric current of the desired amount that can flow.
Semiconductor element interconnecting piece 40 is made of the cured article of the adhesive compound that contains above-mentioned adhesive compound, so, bonding strength to the semiconductor element interconnecting piece 40 of semiconductor element 50 and substrate 60 becomes very high, can keep this state for prolonged period of time.Thereby, can fully improve the long-term reliability of electrical characteristic between semiconductor element 50 and the substrate 60.
Below, specify the present invention based on embodiment, but the present invention is not limited thereto.
The allotment of＜electroconductive particle 〉
On the surface of polystyrene particle, the nickel dam of thickness 0.2 μ m is set, and then, makes the electroconductive particle of median size 4 μ m, proportion 2.5 at the gold layer of the arranged outside thickness 0.02 μ m of this nickel dam.
Embodiment 1
(molecular-weight average 45000, ユ ニ オ Application カ one バ イ ト company produce dissolving 50 mass parts phenoxy resins in 75 mass parts methyl ethyl ketones, trade(brand)name: PKHC), make the solution of solids component 40 quality %.
Then, in this solution, as free-radical polymerised compound, (East Asia Synesis Company produces, trade(brand)name: M-215), (common prosperity chemical company produces 20 mass parts urethanum acrylate, trade(brand)name: AT-600), (common prosperity chemical company produces 5 mass parts 2-(methyl) acryloxy ethyl phosphonic acid esters, trade(brand)name: ラ イ ト エ ス テ Le P-2M) to mix 25 mass parts isocyanuric acid EO modification diacrylates; As radical initiator, mix the own ester of 1.5 mass parts peroxidation 2 ethyl hexanoic acid uncles (1 minute half life temperature be 132.6 ℃, Nof Corp. are produced, trade(brand)name: パ one ヘ キ シ Le O), the own ester of 1.5 mass parts peroxidation phenylformic acid uncles (1 minute half life temperature be 160.3 ℃, Nof Corp. are produced, trade(brand)name: パ one ヘ キ シ Le Z).The blending dispersion electroconductive particle makes it become 1.5 volume % in the mixed solution that obtains, and obtains adhesive compound A.
Then, on the fluororesin film of the thickness 80 μ m that monoplanar surface is handled, the adhesive compound A that uses known coating equipment coating to obtain carries out warm air drying with 70 ℃, 10 minutes, obtains the membranaceous circuit connection material A of bed thickness 15 μ m.
Embodiment 2
Except the blending ratio that makes radical polymerization initiator peroxidation-own ester of 2 ethyl hexanoic acid uncle is that the blending ratio of 1 mass parts, the own ester of peroxidation phenylformic acid uncle is 2 mass parts, operation obtains membranaceous circuit connection material B similarly to Example 1.
Comparative example 1
Except the blending ratio that makes radical polymerization initiator peroxidation-own ester of 2 ethyl hexanoic acid uncle is 3 mass parts and does not use the own ester of peroxidation phenylformic acid uncle that operation obtains membranaceous circuit connection material C similarly to Example 1.
Comparative example 2
Except not using the peroxidation-own ester of 2 ethyl hexanoic acid uncle as radical polymerization initiator and making the blending ratio of the own ester of peroxidation phenylformic acid uncle is 3 mass parts, and operation obtains membranaceous circuit connection material D similarly to Example 1.
Comparative example 3
As radical polymerization initiator, mix 3 mass parts di-isopropyl peroxydicarbonates (1 minute half life temperature be 88.3 ℃, Nof Corp. are produced, trade(brand)name: パ one ロ イ Le IPP) to replace beyond peroxidation-own ester of 2 ethyl hexanoic acid uncle and the own ester of peroxidation phenylformic acid uncle, operation obtains membranaceous circuit connection material E similarly to Example 1.
＜evaluation method 1 〉
[mensuration that connects resistance]
Membranaceous circuit connection material A～D that use is obtained by above-mentioned manufacture method is electrically connected the flexible PCB (FPC) of the copper circuit distribution with 500 live widths, 25 μ m, spacing 50 μ m, thickness 18 μ m and the glass (thickness 1.1mm, surface resistivity 20 Ω) of the thin layer of the indium tin oxide (ITO) that forms 0.2 μ m with hot-press arrangement (type of heating: constant heat Xing, East レ エ Application ジ ニ ア リ Application グ company produces) with the 2mm width.At this moment heating and pressurizing condition, Heating temperature are 160 ℃, 170 ℃, 190 ℃, and moulding pressure is 3MPa, and the heating and pressurizing time is 15 seconds.After keeping 120 hours in firm bonding back and in 85 ℃, the hot and humid groove of 85%RH, use the resistance value between the circuit that multitester measuring should be electrically connected.Resistance value is with mean value (x+3 б) expression of 150 of the resistance between adjacent circuit.The result that table 1 expression obtains.
＜evaluation method 2 〉
[mensuration of bonding strength]
Peeling off method according to JIS-Z0237 with 90 degree measures the bonding strength of the membranaceous circuit connection material A～D that is obtained by above-mentioned manufacture method and estimates.Here, the determinator of bonding strength uses テ Application シ ロ Application UTM-4 (peeling rate 50mm/min, 25 ℃, East ocean ボ one Le De ウ イ Application company produces).The result that table 2 expression obtains.
Table 1
Project Heating temperature (℃) Connect resistance (Ω) Bonding strength (N/m)
After just bonding Behind the 120h After just bonding Behind the 120h
Embodiment 1 160 170 190 2.3 2.1 2.4 2.5 2.5 2.8 1050 980 1020 900 930 950
Embodiment 2 160 170 190 1.9 2.1 2.0 2.4 2.7 2.6 1100 1030 1060 1040 980 980
Comparative example 1 160 170 190 2.3 3.6 more than or equal to 10 3.3 8.6 more than or equal to 10 870 730 240 600 550 130
Comparative example 2 160 170 190 4.6 3.8 1.9 More than or equal to 10 more than or equal to 10 3.4 530 740 900 400 475 560
Membranaceous circuit connection material A and the B of embodiment 1,2, when 160～190 ℃ of Heating temperatures, even firm bonding back and in 85 ℃, the hot and humid groove of 85%RH, keep 120 hours after, also show good connection resistance and bonding strength, the Heating temperature for wide region shows good characteristic as can be known.With respect to this, do not adopt the membranaceous circuit connection material C of comparative example 1 of the present invention, during 170 ℃ of heating, after 85 ℃, 85%RH keep 120 hours, and during 190 ℃ of heating, connect resistance and uprise, and, firm bonding back and in 85 ℃, the hot and humid groove of 85%RH, keep 120 hours after, compare with embodiment 1,2, bonding strength all shows low value.And then the connection resistance of the membranaceous circuit connection material D of comparative example 2 when 160～170 ℃ of heating uprises, bonding strength shows low value.
＜evaluation method 3 〉
In vacuum-packed material, take in the membranaceous circuit connection material A and the E that obtain by embodiment 1 and comparative example 3,40 ℃ place 3 after, by above-mentioned hot-press arrangement, under 160 ℃, 3MPa, 10 seconds condition hot pressing FPC and ITO.According to evaluation method 1 and 2, the film that obtains is measured connection resistance and bonding strength.This result of table 2 expression.
Table 2
Project Connect resistance (Ω) Bonding strength (N/m)
Before the placement 40 ℃ place 3 after Before the placement 40 ℃ place 3 after
Embodiment 1 2.3 2.1 1050 1080
Comparative example 3 2.5 More than or equal to 10 650 320
As known from Table 2, the membranaceous circuit connection material A of embodiment 1 before and after 40 ℃ of placements, shows good connection resistance and bonding strength, stability in storage excellence.With respect to this, do not adopt the membranaceous circuit connection material E of comparative example 3 of the present invention,, connect resistance rising and bonding strength and reduce by half after 3 days 40 ℃ of placements, stability is bad.
According to the present invention, can very promptly be cured processing with low temperature, and, be cured the technology amplitude broad when handling, the syndeton and the semiconductor device that can access very stable bonding strength and the adhesive compound that is connected resistance, circuit connection material, circuit block can be provided.

Claims (5)

1. circuit connection material, it is in order to be electrically connected the circuit connection material between the opposed circuit electrode, to it is characterized in that, containing two or more free-radical polymerised compound and two or more radical polymerization initiator.
2. circuit connection material according to claim 1 is characterized in that, further contains thermoplastic resin.
3. circuit connection material according to claim 1 and 2 is characterized in that, at least a in the described free-radical polymerised compound is the urethanum acrylate.
4. according to each the described circuit connection material in the claim 1～3, it is characterized in that, further contain phosphate compound.
5. according to each the described circuit connection material in the claim 1～4, it is characterized in that, further contain electroconductive particle.
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CN104559902A (en) * 2013-10-09 2015-04-29 日立化成株式会社 Circuit connecting material, connection structure of circuit members, and method for manufacturing connection structure of circuit member

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CN1970673B (en) 2012-03-28
CN1696234A (en) 2005-11-16
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KR20070001854A (en) 2007-01-04
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JP2005320455A (en) 2005-11-17
TW200718765A (en) 2007-05-16

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