WO2016167245A1 - 導電性接着フィルムおよびダイシングダイボンディングフィルム - Google Patents

導電性接着フィルムおよびダイシングダイボンディングフィルム Download PDF

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WO2016167245A1
WO2016167245A1 PCT/JP2016/061795 JP2016061795W WO2016167245A1 WO 2016167245 A1 WO2016167245 A1 WO 2016167245A1 JP 2016061795 W JP2016061795 W JP 2016061795W WO 2016167245 A1 WO2016167245 A1 WO 2016167245A1
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Prior art keywords
conductive adhesive
adhesive film
acid
compound
film according
Prior art date
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PCT/JP2016/061795
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English (en)
French (fr)
Inventor
尚明 三原
切替　徳之
二朗 杉山
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古河電気工業株式会社
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Application filed by 古河電気工業株式会社 filed Critical 古河電気工業株式会社
Priority to JP2016547129A priority Critical patent/JP6462702B2/ja
Priority to SG11201704918VA priority patent/SG11201704918VA/en
Priority to CN201680003698.XA priority patent/CN107075317B/zh
Priority to MYPI2017703846A priority patent/MY190140A/en
Priority to EP16780036.6A priority patent/EP3216837B1/en
Priority to US15/527,232 priority patent/US20180026003A1/en
Priority to KR1020177015131A priority patent/KR101935705B1/ko
Publication of WO2016167245A1 publication Critical patent/WO2016167245A1/ja
Priority to PH12017501894A priority patent/PH12017501894A1/en
Priority to US15/990,153 priority patent/US20180294242A1/en

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    • C—CHEMISTRY; METALLURGY
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • C—CHEMISTRY; METALLURGY
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    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
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    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
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    • C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
    • C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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    • C09J201/00—Adhesives based on unspecified macromolecular compounds
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    • C09J7/00—Adhesives in the form of films or foils
    • C—CHEMISTRY; METALLURGY
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    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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    • C09J9/02—Electrically-conducting adhesives
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    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • 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
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    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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    • H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/32245—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
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    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
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    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
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    • H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H01L2224/48247—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a bond pad of the item
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    • H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H01L2224/8319—Arrangement of the layer connectors prior to mounting
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    • H01L2224/91—Methods for connecting semiconductor or solid state bodies including different methods provided for in two or more of groups H01L2224/80 - H01L2224/90
    • H01L2224/92—Specific sequence of method steps
    • H01L2224/922—Connecting different surfaces of the semiconductor or solid-state body with connectors of different types
    • H01L2224/9222—Sequential connecting processes
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    • H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
    • H01L23/3107—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed
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    • 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
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    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
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    • H01L2924/20104—Temperature range 100 C=<T<150 C, 373.15 K =< T < 423.15K
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    • H01L2924/20105—Temperature range 150 C=<T<200 C, 423.15 K =< T < 473.15K
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    • H01L2924/20106—Temperature range 200 C=<T<250 C, 473.15 K =<T < 523.15K

Definitions

  • the present invention relates to a conductive adhesive film and a dicing die bonding film formed by bonding the adhesive film and an adhesive tape.
  • solder has been widely used to join semiconductor power elements such as IGBTs and MOS-FETs to metal lead frames, but recently, the toxicity of lead has been regarded as a problem.
  • semiconductor power elements such as IGBTs and MOS-FETs
  • the toxicity of lead has been regarded as a problem.
  • power devices using wide-gap semiconductors such as SiC and GaN that can withstand junction temperatures of 200 ° C. or higher is progressing against the background of higher density energy control. Since the eutectic melting point of the solder is low, the lack of heat resistance at the joint is a bottleneck.
  • diffusion-sintered solder such as Cu / Sn solder
  • these diffusion sintered solders have a low melting point during mounting, they have an irreversible high melting point after the diffusion sintering reaction, so both heat resistance and mounting reliability are better than conventional lead-free solders. It is advantageous.
  • the wettability is slightly inferior to lead-free solder, so there is still a risk of solder removal when joining large-area elements of 5 mm ⁇ or more, and the sintered body is hard. Since it is brittle and has low stress relaxation properties, it has low heat fatigue resistance and has the disadvantage of shortening the device life.
  • Patent Document 3 a flux such as pine resin or alcohol for the purpose of removing a metal oxide film.
  • a flux such as pine resin or alcohol
  • Patent Document 3 Easy to bleed out, and these conventional fluxes are not so high in removal capability of metal oxide film, so it may be necessary to add a large amount of bleed out, so there is a lot of bleed out, so reflow reliability reliability of semiconductor element bonding
  • flux cleaning after soldering has been required in the past, the labor and processing of cleaning waste liquid are becoming a problem.
  • the amount of flux added is reduced to reduce bleed out, the ability to remove the oxide film is insufficient, and it is difficult to develop conductivity and other performances.
  • An object of the present invention is to provide means that is excellent in heat resistance and mounting reliability, is lead-free, and has a low environmental load when a semiconductor power element is bonded to a metal lead frame.
  • the present invention relates to a conductive adhesive film that is selected.
  • the total amount of antimony and arsenic components is preferably less than 0.1 wt%.
  • the Lewis acid compound or thermal acid generator is boron fluoride or a complex thereof, fluorinated boronate or polyfluoroalkyl boronic acid or a salt thereof, polyfluoroaryl boronic acid or polyfluoroalkylfluorophosphoric acid or It is preferably selected from the salt thereof, polyfluoroarylfluorophosphoric acid or a salt thereof.
  • the Lewis acid compound or thermal acid generator is preferably selected from arylsulfonium cation salts and aryliodonium cation salts.
  • the weight fraction of the Lewis acid compound or the thermal acid generator is 0.3 to 3 wt%, and the weight fraction of the metal particles is 70 to 96 wt%. preferable.
  • the boiling point or sublimation point of the Lewis acid compound or thermal acid generator is preferably 200 ° C. or higher at normal pressure.
  • the total amount of lead, mercury, antimony and arsenic components in the conductive adhesive film is preferably less than 0.1 wt%. Moreover, it is preferable that at least 1 part of the said metal particle contains either Cu, Ni, or Sn. Moreover, it is preferable that the said metal particle is a mixture of 2 or more types of metals containing the combination which can form an intermetallic compound mutually. Moreover, it is preferable that at least two of the two or more types of metal particles are selected from Cu, Ag, Ni, Ti, Al, Sn, Zn, Au, and In.
  • thermosetting resin preferably contains a maleic imide compound containing 2 units or more of imide groups in one molecule.
  • the maleic imide compound preferably includes a skeleton derived from a C10 or higher aliphatic amine.
  • the conductive adhesive film of the present invention preferably further contains an epoxy compound.
  • the present invention relates to a dicing die bonding film formed by laminating the conductive adhesive film and an adhesive tape.
  • a conductive adhesive film provided by the present invention or a dicing die bonding film in which a dicing tape and a dicing tape are combined, it can be mounted at a low temperature but has excellent heat resistance after sintering, no solder removal failure, and a flux cleaning process. Even if this is omitted, it has become possible to provide an inexpensive and environmentally friendly means that can electrically bond a power semiconductor to a lead frame or the like, which is excellent in heat fatigue and reflow resistance after moisture absorption.
  • the conductive adhesive film of the present invention includes at least metal particles, a thermosetting resin, and a Lewis acid compound or a thermal acid generator.
  • the metal particles are responsible for electrical conductivity and thermal conductivity, and the thermosetting resin imparts relaxation properties to the film properties before sintering and the stress generated by the thermal cycle after sintering, and a Lewis acid compound or thermal acid.
  • the generator has a so-called “flux” function that assists its function by removing the oxide film on the surface of the metal particles.
  • Metal particles It is preferable that at least a part of the metal particles according to the present invention includes a combination capable of forming an intermetallic compound with each other from the viewpoint of having heat resistance equal to or higher than the mounting temperature after sintering while lowering the mounting temperature.
  • a combination of metals capable of forming an intermetallic compound for example, a combination of Cu or Ni or Ag and Sn or Zn, a combination of Ag and Sn, a combination of Ni or Sn or Al and Ti, or a combination of Au and
  • a combination containing Sn having a low melting point is preferable from the viewpoint of lowering the mounting temperature, and a combination containing Cu or Ni and Sn is particularly preferable.
  • metals capable of forming the intermetallic compound may be added as necessary.
  • other metal components may be added as necessary.
  • the weight fraction of the metal particles in the conductive adhesive film is preferably 70 to 96 wt%. (In this case, the “adhesive film” does not include the weight of a substrate such as PET. The same shall apply hereinafter.)
  • the metal particles preferably contain as little lead, mercury, antimony and arsenic as possible, specifically less than 0.1 wt% in the conductive adhesive film from the viewpoint of low environmental load.
  • the component Before sintering, which will be described later after dicing, there is a melting point that can be attributed to at least one metal component observed as an endothermic peak by DSC, so that the component can be applied to the surface of the adherend at a low temperature. To be advantageous.
  • the component has a high melting point due to a diffusion reaction between metals after sintering, so that it can withstand heat resistance after wire bonding with a high melting point lead-free solder or reflow treatment after mounting. Have sex.
  • the mounting temperature is preferably 100 to 250 ° C, more preferably 100 to 200 ° C.
  • the heat resistant temperature is preferably 250 ° C. or higher, more preferably 300 ° C. or higher.
  • thermosetting resin is preferably a maleic imide resin (maleimide resin) or an epoxy resin containing two or more units of imide groups in one molecule from the viewpoint of heat resistance and film properties when metal particles are mixed.
  • the maleic imide resin is obtained, for example, by condensing maleic acid or an anhydride thereof with diamine or polyamine, etc., and those containing a skeleton derived from C10 or higher aliphatic amine are preferable from the viewpoint of stress relaxation, Particularly preferably, it is C30 or more, and those having a skeleton such as the following formula (1) are preferred.
  • the maleic imide resin contains a skeleton derived from an acid component other than maleic acid, such as benzenetetracarboxylic acid or its anhydride, hydroxyphthalic acid bisether or its anhydride, etc. to adjust the molecular weight or Tg. May be.
  • an acid component other than maleic acid such as benzenetetracarboxylic acid or its anhydride, hydroxyphthalic acid bisether or its anhydride, etc.
  • Tg. benzenetetracarboxylic acid or its anhydride
  • hydroxyphthalic acid bisether or its anhydride etc.
  • Examples of the bismaleimide resin having such a structure include those shown in the following structural formula.
  • C 36 has the following structure.
  • epoxy As the thermosetting resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin and combinations thereof are preferable from the viewpoint of balance between stress relaxation and film properties, and more preferably epoxy resin having a large molecular weight with them. It is a mixture with a phenoxy resin.
  • an acid anhydride, a phenol resin, an amine, imidazole, dicyandiamide, or the like can be selected.
  • the sintered body of the conductive adhesive film of the present invention has a thermal fatigue characteristic because the conventional lead-free solder containing only metal is hard and brittle. In addition to overcoming the disadvantage of being bad, the film properties before sintering are ensured.
  • the metal oxide film can be removed much more easily than an acid or the like, and therefore, it is effective even in a much smaller amount than a conventional flux.
  • the “thermal acid generator” is a compound that exhibits Lewis acidity upon heating, and is a material that does not necessarily exhibit strong Lewis acidity at room temperature but exhibits strong Lewis acidity when heated.
  • a thermal acid generator of the type that generates protonic acid by drawing hydrogen when heated to about 80-200 ° C in the presence of hydrocarbon compounds, etc. It is suitable in that it can be stored for a long period of time and acts as a flux quickly during sintering.
  • thermal acid generator examples include a combination of boron trifluoride and a Lewis basic compound, or a combination of an aryliodonium cation or arylsulfonium cation and a proton acid or the same anion as its salt.
  • the acid dissociation constant pKa of fluorinated boronic acid tetrafluoroboric acid
  • the value of the acid dissociation constant pKa may not be determined, but the relative acid strength can be defined by the reactivity.
  • boron fluoride or a complex thereof for example, boron trifluoride or boron trifluoride and an amine complex of phenol, pyridine, bipyridine or the like.
  • fluorinated antimonates, polyfluoroalkylborates, and polyfluoroarylborates are particularly high in oxide film removal ability, and many of them have a boiling point or sublimation point of 20 at atmospheric pressure.
  • polyfluoroalkylborates or polyfluoroarylborates are highly toxic antimony From the viewpoint of low environmental load, and since it is oleophilic, it can be easily dissolved in an organic solvent or the like and dispersed in a thermosetting resin. preferable.
  • Lewis acid salts or thermal acid generators also act as latent curing agents for epoxy and maleimide resins, or latent curing catalysts.
  • the weight fraction of the Lewis acid compound or thermal acid generator in the conductive adhesive film has sufficient ability to remove the metal oxide film, but avoids the risk of lowering the reflow reliability after moisture absorption due to bleed out. From the viewpoint, it is preferably 0.3 to 3 wt%, more preferably 0.5 to 1 wt%. As described above, since the flux component is extremely small, the bleed-out risk can be reduced without sufficient flux cleaning, and sufficient reliability can be ensured.
  • the weight fraction of metal particles is preferably 70 to 96 wt%. By setting the weight fraction of the metal particles to 70 wt% or more, contact between the metal particles can be obtained, and the volume resistivity can be reduced. Moreover, the film property which forms a composition in a film form can be ensured by making the weight fraction of a metal particle into 96 wt% or less.
  • the conductive adhesive film of the present invention is in the form of a film, for example, it is attached to the back surface of a wafer on which a power semiconductor element is formed, and the adhesive film is divided for each wafer in a dicing process in which the wafer is divided into chips.
  • This makes it possible to easily mount the adhesive film on the entire back surface of the device without excess or deficiency, regardless of the problems caused by the liquid, such as the wettability of the solder, that is, wetting spread and protrusion. it can.
  • the adhesive film with a predetermined thickness in advance it is possible to control the height of the element after die bonding with higher accuracy than conventional solder or conductive paste.
  • the adhesive film and the dicing tape can be bonded to the wafer at one time, and the process can be omitted.
  • FIG. 1 is a cross-sectional view showing a dicing die bonding film 10 according to the present invention.
  • the dicing die bonding film 10 is mainly composed of a dicing tape 12 and an adhesive film 13.
  • the dicing die bonding film 10 is an example of a tape for semiconductor processing, and may be cut (precut) into a predetermined shape in advance according to a use process or an apparatus, or may be cut for each semiconductor wafer. It may be a long roll shape.
  • the dicing tape 12 includes a support base 12a and an adhesive layer 12b formed thereon.
  • the release treatment PET11 covers the dicing tape 12 and protects the pressure-sensitive adhesive layer 12b and the adhesive film 13.
  • the support substrate 12a is preferably radiolucent, and specifically, plastic or rubber is usually used, and is not particularly limited as long as it transmits radiation.
  • the base resin composition of the pressure-sensitive adhesive layer 12b is not particularly limited, and a normal radiation curable pressure-sensitive adhesive is used.
  • An acrylic pressure-sensitive adhesive having a functional group capable of reacting with an isocyanate group such as a hydroxyl group is preferred.
  • the acrylic pressure-sensitive adhesive preferably has an iodine value of 30 or less and has a radiation-curable carbon-carbon double bond structure.
  • the configuration of the adhesive film 13 according to the present invention is a semiconductor adhesive that is a conductive adhesive film containing metal particles, a thermosetting resin, a Lewis acid compound or a thermal acid generator.
  • a semiconductor adhesive that is a conductive adhesive film containing metal particles, a thermosetting resin, a Lewis acid compound or a thermal acid generator.
  • the dicing die bonding film 10 of the present invention can be suitably used.
  • the peeling treatment PET 11 is removed from the dicing die bonding film 10, and an adhesive film 13 is attached to the semiconductor wafer 1 and the side portion of the dicing tape 12 is fixed by the ring frame 20 as shown in FIG.
  • the ring frame 20 is an example of a dicing frame.
  • the adhesive film 13 is laminated on a portion of the dicing tape 12 where the semiconductor wafer 1 is bonded. There is no adhesive film 13 in the portion of the dicing tape 12 that contacts the ring frame 20.
  • the semiconductor wafer 1 is diced into a predetermined size using the dicing blade 21 while the lower surface of the dicing tape 12 is sucked and fixed by the suction table 22 to manufacture a plurality of semiconductor chips 2.
  • the tape push-up ring 30 is raised, the central portion of the dicing tape 12 is bent upward, and radiation such as ultraviolet rays is radiated.
  • the adhesive strength of the dicing tape 12 is weakened.
  • the push-up pin 31 is raised at a position corresponding to each semiconductor chip, and the semiconductor chip 2 is picked up by the suction collet 32.
  • the picked-up semiconductor chip 2 is bonded to a supporting member such as the lead frame 4 or another semiconductor chip 2 (die bonding process), and as shown in FIG. A semiconductor device is obtained through steps such as resin molding, heat curing, and sintering.
  • wt% shows weight%
  • Examples 1 to 7 A mixture of 92 wt% metal particles, 7 wt% resin, a compound having Lewis acidity or 1 wt% thermal acid generator (flux) with the composition shown in Table 1 was stirred in a planetary mixer. After that, it was thinly applied onto the release-treated PET and dried at 120 ° C. to obtain an adhesive film having a thickness of 40 ⁇ m.
  • a color reagent (triphenylmethanol) was dissolved in a mixed solvent of diethyl ether: 1,2-dichloroethane and 1: 1 to prepare a color reagent solution A.
  • each acid shown in Table 1 was diluted or dissolved in diethyl ether to prepare an acid solution B having the same concentration as the color reagent solution A.
  • Triphenylmethanol was dissolved in 1,4-dioxane to prepare a color reagent solution A ′.
  • a color reagent solution A ′ Triphenylmethanol was dissolved in 1,4-dioxane to prepare a color reagent solution A ′.
  • an acid generator solution B ′ having the same concentration as the color reagent solution A ′, 100
  • the mixture was stirred at 0 ° C. for 1 hour, and acid generation treatment was performed by a hydrogen abstraction reaction from triphenylmethane to the acid generator.
  • ⁇ Support base material> Resin beads made of commercially available low density polyethylene (Novatec LL, manufactured by Nippon Polyethylene Co., Ltd.) were melted at 140 ° C. and formed into a long film having a thickness of 100 ⁇ m using an extruder.
  • ⁇ Adhesive composition> Disperse a 200: 10: 5: 2 (weight ratio) mixture of n-octyl acrylate, 2-hydroxyethyl acrylate, methacrylic acid and benzoyl peroxide as a polymerization initiator in an appropriate amount of toluene, and adjust the reaction temperature and reaction time.
  • a solution of an acrylic resin having a functional group was obtained.
  • 2 parts by weight of coronate L (manufactured by Nippon Polyurethane) as a polyisocyanate and 100 parts by weight of the acrylic resin solution and an appropriate amount of toluene as an additional solvent are added and stirred to form an adhesive composition.
  • Product 1 was obtained.
  • ⁇ Dicing tape> The pressure-sensitive adhesive composition was applied on a supporting substrate so that the thickness of the pressure-sensitive adhesive composition 1 after drying was 5 ⁇ m, and dried at 120 ° C. for 3 minutes to prepare a dicing tape.
  • Table 2 shows the results of evaluating the following items in the adhesive films obtained in Examples 1 to 5 and Comparative Examples 1 to 3 and the dicing die bond tape using the adhesive films.
  • DSC A DSC measuring device (DSC7000, manufactured by Hitachi High-Technology) was used to confirm the presence or absence of an endothermic peak in the temperature range of 200 to 250 ° C. for each sample before sintering. Next, the same measurement was performed on each sample sintered at 250 ° C. for 4 hours under nitrogen.
  • Adhesive strength The die bonding film is adjusted by bonding the adhesive film to the dicing tape, and the back surface is bonded to an Au-plated Si wafer at 100 ° C., then diced to 5 mm ⁇ to be separated into individual pieces. Chips and adhesive films were obtained.
  • the shear adhesive strength at 260 ° C. was measured with a die shear measuring machine (Arctech series 4000). It was measured.
  • Adhesive strength after TCT The same sample as above was subjected to a thermal shock (TCT) treatment of ⁇ 40 to + 150 ° C. ⁇ 200, and then the shear adhesive strength at 260 ° C. was measured.
  • TCT thermal shock
  • a conductive adhesive film comprising metal particles, a thermosetting resin, and a Lewis acid compound or thermal acid generator as a flux, which is a pka of the Lewis acid compound or thermal acid generator.
  • the conductive adhesive films of Examples 1 to 7 with a value less than ⁇ 0.4 do not use lead solder with high environmental load, and heat resistance and moisture absorption reliability even though the amount of flux added is as low as 1 wt%. It has been proved that there is a remarkable effect which is not present in the prior art and has both the reliability and the coupling reliability.
  • Comparative Examples 1 and 2 using abietic acid since much flux was used, it was proved that the moisture absorption reliability and the bonding reliability were difficult, such as internal peeling even after the MSL test.
  • Comparative Example 3 in which the amount of abietic acid added was the same as that of the Example the difference from the Example of the present application is more apparent, and it was proved that the adhesive strength was significantly inferior to that of the Example. It was.
  • the oxide film cannot be removed with a small amount of addition as in the embodiment. Therefore, the oxide film becomes a barrier, and the diffusion reaction between the metals does not proceed, so that an endothermic peak remains after sintering.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Manufacturing & Machinery (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Die Bonding (AREA)
  • Dicing (AREA)
  • Adhesive Tapes (AREA)
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Abstract

半導体パワー素子を金属リードフレームに接合する際、耐熱性と実装信頼性に優れ、かつ鉛フリーであり環境への付加の小さい手段を提供することを目的とする。　具体的には、金属粒子と、熱硬化性樹脂と、ルイス酸性を有する化合物または熱酸発生剤とを含む導電性接着フィルムであって、前記ルイス酸性を有する化合物または熱酸発生剤が、フッ化ホウ素またはその錯体、ｐＫａ＝－０．４以下のプロトン酸、またはその塩と同一のアニオンと、水素イオンまたはその他のカチオンとを組み合わせた塩または酸から選択されるものであることを特徴とする導電性接着フィルム。および、前記導電性接着フィルムと、粘着テープとを貼り合せてなる、ダイシングダイボンディングフィルム。

Description

導電性接着フィルムおよびダイシングダイボンディングフィルム
　本発明は、導電性接着フィルム、およびそれと粘着テープとを貼り合せてなるダイシングダイボンディングフィルムに関する。
　ＩＧＢＴ、ＭＯＳ－ＦＥＴなどの半導体パワー素子を金属リードフレームに接合する際、従来は鉛フリーはんだが広く使われてきたが、昨今は鉛の有害性が問題視されている。
　また、近年はより高密度なエネルギー制御が求められている事を背景に、２００℃以上のジャンクション温度に耐えるＳｉＣ、ＧａＮなどのワイドギャップ半導体を用いたパワー素子の研究が進んでいるが、鉛はんだの共晶融点が低い為に接合部分の耐熱性不足がネックとなっている。
　上記の背景から、鉛を含まない様々なタイプの鉛フリーはんだが登場しており、その中でもＡｕＧｅなどの高融点はんだがワイドギャップ半導体素子の接合材として注目されている（特許文献１）が、材料が高価な事、実装温度が高くなることでプロセスコストが高くなる事がネックとなっており、普及が進んでいない。また、多くの鉛フリーはんだは鉛はんだよりも濡れ性が悪い為にダイパッド部分にはんだが塗れ拡がらず、ダイの角などではんだが抜けた状態になり易く、その部分が接合不良のリスクを引き起こす事が問題となっている。鉛フリーはんだの濡れ性は融点が高くなるほど更に悪くなる傾向がある為、耐熱性と実装信頼性の両立が難しい。
　上記の課題を解決する為、Ｃｕ／Ｓｎ系はんだ等の拡散焼結型のはんだの研究が進められている。これら拡散焼結型のはんだは実装時の融点が低いにも拘らず、拡散焼結反応後は不可逆的に高融点化する為、耐熱性と実装信頼性の両立が従来の鉛フリーはんだよりも有利である。しかしながら、拡散焼結型はんだでも尚、濡れ性が鉛フリーはんだにはやや劣る為、５ｍｍ□以上の大面積素子の接合の際にはやはりはんだ抜けのリスクがあり、かつ焼結体が硬くて脆く、応力緩和性が低い為に耐熱疲労特性が低く、素子寿命を短くしてしまう欠点がある。
　上記鉛フリーはんだの他に、Ａｇペーストなども用いられているが、材料コストが非常に高価となる点と、Ａｇイオンのマイグレーションによる汚染が問題となっている。
　また、鉛はんだや鉛フリーはんだの多くには金属の酸化被膜を除去する目的で、松脂やアルコールなどのフラックスを添加する事が一般的である（特許文献３）が、これらフラックス成分は吸湿後にブリードアウトし易く、またこれらの従来型フラックスは金属酸化被膜の除去能がさして高くない為に多量に添加する必要もあることもあってブリードアウト分が多い為に半導体素子の接合の耐リフロー信頼性に悪影響を与えることが知られており、従来ははんだ付後のフラックス洗浄が必要とされてきたが、その手間や洗浄廃液の処理が問題視されつつある。とはいえ、ブリードアウトを低減する為にフラックスの添加量を少なくすると酸化膜の除去能が不足し、導電性その他の性能が発現しにくかった。
特開２００２－３０７１８８号公報 特開２００７－１５２３８５号公報 ＵＳ２０１４／１２０３５６　Ａ１
　本発明は、半導体パワー素子を金属リードフレームに接合する際、耐熱性と実装信頼性に優れ、かつ鉛フリーであり環境への負荷の小さい手段を提供することを目的とする。
　出願人は鋭意検討の結果、上記課題を解決する導電性接着フィルムの発明に至ったものである。
　すなわち本発明は、金属粒子と、熱硬化性樹脂と、ルイス酸性を有する化合物または熱酸発生剤とを含む導電性接着フィルムであって、前記ルイス酸性を有する化合物または熱酸発生剤が、フッ化ホウ素またはその錯体、ｐＫａ＝－０．４以下のプロトン酸、またはｐＫａ＝－０．４以下のプロトン酸の塩と同一のアニオンと、水素イオンまたはその他のカチオンとを組み合わせた塩または酸から選択されるものであることを特徴とする導電性接着フィルムに関する。
　また、前記ルイス酸性を有する化合物または熱酸発生剤において、アンチモンおよびヒ素成分の総量が０．１ｗｔ％未満であることが好ましい。
　また、前記ルイス酸性を有する化合物または熱酸発生剤が、フッ化ホウ素またはその錯体、フッ化ホウ素酸塩またはポリフルオロアルキルホウ素酸またはその塩、ポリフルオロアリールホウ素酸またはポリフルオロアルキルフルオロリン酸またはその塩、ポリフルオロアリールフルオロリン酸またはその塩から選択されるものであることが好ましい。
　また、前記ルイス酸性を有する化合物または熱酸発生剤が、アリールスルホニウムカチオンの塩、アリールヨードニウムカチオンの塩から選択されるものであることが好ましい。
　また、前記導電性接着フィルム中、前記ルイス酸性を有する化合物または熱酸発生剤の重量分率が０．３～３ｗｔ％であり、かつ金属粒子の重量分率が７０～９６ｗｔ％であることが好ましい。
　また、前記ルイス酸性を有する化合物または熱酸発生剤の沸点または昇華点が、常圧で２００℃以上であることが好ましい。
　また、前記導電性接着フィルム中、鉛および水銀およびアンチモンおよびヒ素成分の総量が０．１ｗｔ％未満であることが好ましい。
　また、前記金属粒子の少なくとも１部が、Ｃｕ、Ｎｉ、Ｓｎのいずれかを含むことが好ましい。
　また、前記金属粒子が、相互に金属間化合物形成が可能な組み合わせを含む２種以上の金属の混合物であることが好ましい。
　また、前記２種以上の金属粒子の少なくとも２種がＣｕ、Ａｇ、Ｎｉ、Ｔｉ、Ａｌ、Ｓｎ、Ｚｎ、Ａｕ、Ｉｎから選択されるものであることが好ましい。
　さらに、焼結前はＤＳＣ（示差走査熱量測定）により観測される吸熱ピークが１００℃～２５０℃において少なくとも１つ存在し、かつ、焼結後はそれが観測されなくなるものであることが好ましい。
　さらに、前記熱硬化性樹脂が、イミド基を１分子に２単位以上含むマレイン酸イミド化合物を含むことが好ましい。
　さらに、マレイン酸イミド化合物が、Ｃ１０以上の脂肪族アミンに由来する骨格を含むことが好ましい。
　くわえて、本発明の導電性接着フィルムは、さらにエポキシ化合物を含むことが好ましい。
　くわえて、本発明は、前記導電性接着フィルムと、粘着テープとを貼り合せてなる、ダイシングダイボンディングフィルムに関する。
　本発明が提供する導電性接着フィルム、あるいはそれとダイシングテープを組合わせたダイシングダイボンディングフィルムを用いることによって、低温で実装できながらも焼結後の耐熱性に優れ、はんだ抜け不良なく、フラックス洗浄工程を省いたとしても耐熱疲労および吸湿後耐リフロー性に優れた、パワー半導体をリードフレーム等に電気的に接合できる、安価かつ環境への負荷も小さい手段を供する事を可能とした。
本発明の実施形態に係るダイシング・ダイボンディングフィルムを示す断面図である。 本発明のダイシング・ダイボンディングフィルムを半導体に貼合した状態を示す図である。 ダイシング工程を説明するための図である。 ピックアップ工程を説明するための図である。 ダイボンディング工程を説明するための図である。 モールドずみ半導体素子の断面を示す図である。 各酸のモル吸光係数スペクトルを示す図である。
　本発明の導電性接着フィルムは、少なくとも金属粒子と、熱硬化性樹脂と、ルイス酸性を有する化合物または熱酸発生剤とを含むことを特徴とする。
　金属粒子は導電性および熱伝導性を担い、熱硬化性樹脂は焼結前のフィルム性および焼結後の熱サイクルによって発生する応力等に対する緩和性を付与し、ルイス酸性を有する化合物若しくは熱酸発生剤は金属粒子表面の酸化膜を除去することでその働きを助ける、所謂“フラックス”の機能を有する。
（金属粒子）
　本発明にかかる金属粒子は、その少なくとも１部が相互に金属間化合物形成が可能な組み合わせを含むことが、実装温度を低くしつつも焼結後実装温度以上の耐熱性を有する点から好ましい。
　金属間化合物形成が可能な金属の組合せとして、例えばＣｕ或いはＮｉ或いはＡｇとＳｎ或いはＺｎとの組合せ、ＡｇとＳｎとの組合せ、Ｎｉ或いはＳｎ或いはＡｌとＴｉとの組合せ、ＡｕとＩｎとの組合せなどが挙げられるが、取り分け実装温度を低くする観点から低融点のＳｎを含む組合せが好ましく、特に好ましくはＣｕ或いはＮｉとＳｎとを含む組合せである。
　前記金属間化合物形成が可能な金属の組合せに加えて、必要に応じてその他の金属成分を加えても良い。例えば、ＳｎにＺｎやＢｉ、Ａｇ、Ｉｎ、Ｇａ、Ｐｄ、等を加えて予め合金化したものを粒子化して用いることで、更に低融点化することも可能である。
　前記金属粒子の導電性接着フィルム中における重量分率は、７０～９６ｗｔ％であることが好ましい。（なお、この場合の「接着フィルム」は、ＰＥＴなどの基材重量を含まない。以下同じ。）
　前記金属粒子には、鉛および水銀およびアンチモンおよびヒ素をなるべく含まない、具体的には導電性接着フィルム中０．１ｗｔ％未満であることが、低環境負荷の観点から好ましい。
　後で述べるダイシング後に行う焼結前においては、ＤＳＣによって吸熱ピークとして観測される少なくとも１種の金属成分に帰属できる融点があることで、被着体表面にその成分が塗れることが低温での実装を有利にする。さらにその成分が、焼結後においては金属間の拡散反応により高融点化することで、例えば実装後に高融点鉛フリーはんだでワイヤーボンドしたりリフロー処理等をかけたりしても耐えうる十分な耐熱性を有する。実装温度は１００～２５０℃が好ましく、更に好ましくは１００～２００℃である。耐熱温度は２５０℃以上が好ましく、更に好ましくは３００℃以上である。
（熱硬化性樹脂）
　熱硬化性樹脂は、耐熱性と金属粒子を混ぜた際のフィルム性の観点から、イミド基を１分子に２単位以上含むマレイン酸イミド樹脂（マレイミド樹脂）或いはエポキシ樹脂が好ましい。前記マレイン酸イミド樹脂は、例えばマレイン酸或いはその無水物とジアミン或いはポリアミンとを縮合する等によって得られるが、Ｃ１０以上の脂肪族アミンに由来する骨格を含むものが応力緩和性の観点から好ましく、特に好ましくはＣ３０以上であり、下記式（１）のような骨格を有するものが好ましい。
式（１）
Figure JPOXMLDOC01-appb-C000001
前記マレイン酸イミド樹脂には、マレイン酸以外の酸成分、例えばベンゼンテトラカルボン酸或いはその無水物、ヒドロキシフタル酸ビスエーテル或いはその無水物等に由来する骨格を含む事により分子量やＴｇなどを調整しても良い。マレイン酸イミド樹脂の硬化剤としては、フェノール樹脂、ラジカル発生剤などが好ましい。
　このような構造のビスマレイミド樹脂としては、例えば下記の構造式に示す様なものが挙げられる。
Figure JPOXMLDOC01-appb-C000002
　なお、上式中、「Ｃ３６」とは、下記構造である。
Figure JPOXMLDOC01-appb-C000003
　熱硬化性樹脂としてエポキシを選択する場合、応力緩和性とフィルム性のバランスの観点からビスフェノールＡ型エポキシ樹脂とビスフェノールＦ型エポキシ樹脂およびそれらの組合せが好ましく、更に好ましくはそれらと分子量の大きなエポキシ樹脂であるフェノキシ樹脂との混合物である。エポキシ樹脂の硬化剤としては、酸無水物、フェノール樹脂、アミン、イミダゾールやジシアンジアミド等を選択できる。
　上記の様な応力緩和性を備えた熱硬化性樹脂を含むことで、本発明の導電性接着フィルムの焼結体は、従来の金属のみの鉛フリーはんだの硬くて脆い為に熱疲労特性が悪いという欠点を克服するとともに、焼結前のフィルム性が担保される。
（ルイス酸性を有する化合物または熱酸発生剤）
　ルイス酸性を有する化合物または熱酸発生剤は、ｉ）フッ化ホウ素またはその錯体、あるいはｉｉ）ｐＫａ＝－０．４以下のプロトン酸、またはｉｉｉ）ｐＫａ＝－０．４以下のプロトン酸の塩と同一のアニオンと、水素イオン或いはその他のカチオンとの組み合わせた塩または酸　である事により、従来鉛はんだ或いは鉛フリーはんだのフラックスとしてよく用いられてきたｐＫａ＝＋４～＋５程度のアビエチン酸やアニス酸等よりも遥かに金属酸化膜の除去能にすぐれ、したがって従来のフラックスよりもずっと少ない量でも効果を発揮する。なお、「熱酸発生剤」とは、加熱によってルイス酸性を示す化合物であり、室温では必ずしも強いルイス酸性を示さないものの、加熱した際に強いルイス酸性を示す材料である。とりわけ炭化水素化合物等との共存下にて、８０～２００℃程度の加熱時に水素引き抜きによりプロトン酸を発生させるタイプの熱酸発生剤が、焼結前の材料を室温にて未反応状態で物性を安定させて長期保管しつつ、焼結時には速やかにフラックスとして作用する点で好適である。この様な熱酸発生剤としては、例えば３フッ化ホウ素とルイス塩基性化合物とを組み合わせた錯体や、アリールヨードニウムカチオンやアリールスルホニウムカチオンと、プロトン酸またはその塩と同一のアニオンとを組み合わせた塩が挙げられる。
　ここで、フッ化ホウ素酸（テトラフルオロホウ酸）の酸解離定数ｐＫａは－０．４であり、ｐＫａ＝－０．４以下のプロトン酸とはフッ化ホウ素酸以上に強い酸を意味する。物質によっては、酸解離定数ｐＫａの値を求められない場合もあるが、相対的な酸の強弱は反応性によって定義することができる。例えば，次のような平衡状態において、
　　　　　　　　　Ａ’＋　Ａ:Ｂ　⇔　Ａ ＋　Ａ’:Ｂ
反応が右へ大きく進行すれば，Ａ’はＡよりも強い酸である。このような反応性からフッ化ホウ素酸に対する酸の強さを得ることができる。
　このようなルイス酸性を有する化合物または熱酸発生剤としては、ｉ）フッ化ホウ素またはその錯体　については、例えば３フッ化ホウ素、または３フッ化ホウ素と、フェノールまたはピリジンやビピリジン等とのアミン錯体などが挙げられ、上記　ｉｉ）ｐＫａ＝－０．４以下のプロトン酸　については、４フッ化ホウ素酸アニオン、６フッ化リン酸アニオンまたはフッ化アンチモン酸アニオンまたはポリフルオロアルキルホウ素酸アニオンまたはポリフルオロアリールホウ素酸アニオンまたはポリフルオロアルキルフルオロリン酸アニオンと、プロトンとを組み合わせた酸などが挙げられ、ｉｉｉ）ｐＫａ＝－０．４以下のプロトン酸の塩と同一のアニオンと、水素イオンまたはその他のカチオンとを組み合わせた塩または酸　におけるカチオンについては、アリールヨードニウムカチオンまたはアリールスルホニウムなどが挙げられる。この中でも３フッ化ホウ素のフェノールまたはアミンとの錯体や、４フッ化ホウ素酸アニオンまたは６フッ化リン酸アニオンまたはフッ化アンチモン酸アニオンまたはポリフルオロアルキルホウ素酸アニオンまたはポリフルオロアリールホウ素酸アニオンまたはポリフルオロアルキルフルオロリン酸アニオンまたはポリフルオロアリールフルオロリン酸アニオンと、アリールヨードニウムカチオンまたはアリールスルホニウムカチオンとを組み合わせた塩が、エポキシ樹脂やポリイミド樹脂などの熱硬化性樹脂成分との相溶性および保存安定性の面から好ましく、さらにフッ化アンチモン酸塩、ポリフルオロアルキルホウ素酸塩、ポリフルオロアリールホウ素酸塩が、特に酸化膜の除去能が高くかつその多くが沸点または昇華点が常圧で２００℃以上であることから、焼結時に接着フィルム中にボイドを生じて接合の強度及び信頼性を低下させるリスクが小さく、さらにポリフルオロアルキルホウ素酸塩或いはポリフルオロアリールホウ素酸塩が毒性の高いアンチモンを含まないことから低環境負荷の面で好ましく、更には親油性であることから有機溶剤等に溶解させて熱硬化性樹脂に分散させるのも容易であることからフィルムの製造性の面からも好ましい。
　これらのルイス酸性を有する塩または熱酸発生剤は、エポキシやマレイミド樹脂の潜在性硬化剤、或いは潜在性硬化触媒としても作用する。
　前記ルイス酸性を有する化合物または熱酸発生剤の導電性接着フィルム中における重量分率は、金属酸化膜の除去能を十分に有しつつも、ブリードアウトによる吸湿後リフロー信頼性低下のリスクを避ける観点から、０．３～３ｗｔ％が好ましく、更に好ましくは０．５～１ｗｔ％である。この様にフラックス成分が極めて少ないことにより、フラックス洗浄を経なくてもブリードアウトリスクを低減でき、十分な信頼性を担保できる。
金属粒子の重量分率は７０～９６ｗｔ％が好ましい。金属粒子の重量分率を７０ｗｔ％以上とすることにより、金属粒子どうしの接触が得られ、体積抵抗率を低下させることができる。また、金属粒子の重量分率を９６ｗｔ％以下とすることにより、組成物をフィルム状に形成するフィルム性を確保することができる。
　本発明の導電性接着フィルムはフィルム状であることで、例えばパワー半導体素子が形成されたウェハの裏面に貼りつけ、ウェハを素子毎に分割・チップ化するダイシング工程において接着フィルムをウェハごと分割することが可能であり、これによりはんだの濡れ性、すなわち濡れ拡がりやはみ出しなどの、液体であることにより生ずる問題とは無関係に、過不足なく素子の裏面全体に接着フィルムを容易に実装することができる。また、予め所定の厚みにて接着フィルムを調整することで、従来のはんだや導電ペーストよりもダイボンド後の素子の高さ制御を精度よく行うこともできる。
　更に、本発明の導電性接着フィルムをダイシングテープと組み合わせてダイシングダイボンディングフィルム化することで、接着フィルムとダイシングテープを一度にウエハに貼合でき、工程を省略化できる。
　上記態様について、図面に基づいて説明する。
　図１は、本願発明にかかるダイシングダイボンディングフィルム１０を示す断面図である。ダイシングダイボンディングフィルム１０は、主にダイシングテープ１２、接着フィルム１３から構成されている。ダイシングダイボンディングフィルム１０は、半導体加工用テープの一例であり、使用工程や装置にあわせて予め所定形状に切断（プリカット）されていてもよいし、半導体ウエハ１枚分ごとに切断されていてもよいし、長尺のロール状を呈していてもよい。
　ダイシングテープ１２は、支持基材１２ａと、その上に形成された粘着剤層１２ｂとから構成されている。
　剥離処理ＰＥＴ１１は、ダイシングテープ１２を覆っており、粘着剤層１２ｂや接着フィルム１３を保護している。
　支持基材１２ａとしては、放射線透過性であることが好ましく、具体的には、通常、プラスチック、ゴムなどを用い、放射線を透過する限りにおいて特に制限されるものではない。
　粘着剤層１２ｂの粘着剤のベース樹脂組成物は、特に限定されるものではなく、通常の放射線硬化性粘着剤が用いられる。好ましくは水酸基などのイソシアネート基と反応しうる官能基を有するアクリル系粘着剤がある。特に制限されるものではないが、アクリル系粘着剤はヨウ素価３０以下であり、放射線硬化性炭素－炭素二重結合構造を有するのが好ましい。
　本願発明にかかる接着フィルム１３の構成としては、上述した通り、金属粒子と、熱硬化性樹脂と、ルイス酸性を有する化合物または熱酸発生剤とを含む導電性接着フィルムであることが、半導体パワー素子を金属リードフレームに接合する際、耐熱性と実装信頼性に優れ、かつ環境への付加の小さい点で非常に好ましい。
（ダイシングダイボンディングフィルムの使用方法）
　半導体装置の製造にあたり、本発明のダイシングダイボンディングフィルム１０を好適に使用することができる。
　まず、ダイシングダイボンディングフィルム１０から剥離処理ＰＥＴ１１を取り除き、図２に示す通り、半導体ウエハ１に接着フィルム１３を貼り付けてダイシングテープ１２の側部をリングフレーム２０で固定する。リングフレーム２０はダイシング用フレームの一例である。接着フィルム１３はダイシングテープ１２の半導体ウエハ１が貼合される部位に積層されている。ダイシングテープ１２のリングフレーム２０と接する部位には接着フィルム１３はない。
　その後、図３に示す通り、ダイシングテープ１２の下面を吸着テーブル２２で吸着・固定しながら、ダイシングブレード２１を用いて半導体ウエハ１を所定サイズにダイシングし、複数の半導体チップ２を製造する。
　その後、図４に示す通り、リングフレーム２０によりダイシングテープ１２を固定した状態で、テープ突き上げリング３０を上昇させ、ダイシングテープ１２の中央部を上方に撓ませるとともに、紫外線などの放射線をダイシングテープ１２に照射し、ダイシングテープ１２の粘着力を弱める。その後、半導体チップごとにこれに対応した位置で突き上げピン３１を上昇させ、半導体チップ２を吸着コレット３２によりピックアップする。
　その後は、図５に示す通り、ピックアップした半導体チップ２を、リードフレーム４などの支持部材や他の半導体チップ２に接着（ダイボンディング工程）し、図６に示す通り、Ａｌワイヤの付設や、樹脂モールド、加熱硬化、焼結などの工程を経ることにより、半導体装置が得られる。
　以下、実施例によって本発明を具体的に説明するが、本発明は当該実施例によって何ら限定・拘束されるべきものではない。なお、ｗｔ％は、重量％を示す。
＜実施例１～７＞
　表１の組成にて、金属粒子９２ｗｔ％、樹脂７ｗｔ％、ルイス酸性を有する化合物または熱酸発生剤（フラックス）１ｗｔ％の混合物に、トルエンを加えてスラリー化したものをプラネタリーミキサーにて撹拌の後、離形処理されたＰＥＴ上に薄く塗って１２０℃で乾燥させ、厚さ４０μｍの接着フィルムを得た。表１中、ＢＭＩ－３０００とは、下記構造（ｎ＝１～１０）である。
Figure JPOXMLDOC01-appb-C000004
  
　なお、実施例１～７で用いられている酸発生剤（フラックス）のｐｋａの値は求められていないが、フッ化ホウ素酸に対する反応性から、ｐＫａ＝－０．４以下であるか否かを判定した。具体的な方法を示す。
　呈色試薬（トリフェニルメタノール）をジエチルエーテル：１，２－ジクロロエタン、１：１混合溶媒に溶解させ、呈色試薬溶液Ａを調整した。次に、表１に記載の各酸をジエチルエーテルにて希釈もしくは溶解させ、前記呈色試薬溶液Ａと同じ濃度の酸溶液Ｂを調整した。呈色試薬溶液Ａと酸溶液Ｂの混合溶液Ｃについて、紫外・可視分光光度計（（株）島津製作所製ＵＶ－１８００）を用いて、下記反応式に示す呈色試薬トリフェニルメタノールの脱水によるトリフェニルメチリウム化呈色反応に由来する４５０ｎｍの吸光度を測定し、それを元に混合溶液Ｃ中における呈色試薬の濃度に基づいてモル吸光係数を計算し、表１に示す通り、酸のｐＫａが小であるほど、該モル吸光係数が大きくなる事を確かめた。このモル吸光係数スペクトルを図７に示す。
　ここで、図７におけるスペクトルは、それぞれ下記の通りである。
Ａ：トリフェニルエタノールのみ（酸なし）
Ｂ：吉草酸
Ｃ：トリクロロ酢酸
Ｄ：テトラフルオロホウ酸
Ｅ：スルホニウム塩（加熱）
Ｆ：スルホニウム塩（非加熱）
Figure JPOXMLDOC01-appb-C000005
  
 
Figure JPOXMLDOC01-appb-T000006
　トリフェニルメタノールを１，４－ジオキサンに溶解させ、呈色試薬溶液Ａ’を調整した。次に、実施例の各酸発生剤および水素源としてのトリフェニルメタンをトルエン若しくは炭酸プロピオンに溶解させ、前記呈色試薬溶液Ａ’と同じ濃度の酸発生剤溶液Ｂ’を調整した後、１００℃で１ｈ撹拌してトリフェニルメタンからの酸発生剤への水素引き抜き反応による酸発生処理を行った。呈色試薬溶液Ａ’と酸発生剤溶液B’の混合溶液Ｃ’について、紫外・可視分光光度計（（株）島津製作所製ＵＶ－１８００）を用いて、上記反応式に示す呈色試薬トリフェニルメタノールの脱水によるトリフェニルメチリウム化呈色反応に由来する４５０ｎｍの吸光度を測定し、それを元に混合溶液Ｃ’中における呈色試薬の濃度に基づいてモル吸光係数を計算し、ｐＫａ ＝ －０．４ のテトラフルオロホウ酸と比較して大小何れかであるかにより、ｐＫａの値が－０．４ 以下であるか否かを判定した。これにより、実施例で用いられている酸発生剤（フラックス）のｐｋａの値が－０．４以下であることが確認された。
＜比較例１、２＞
　表２の組成にて、金属粒子８５ｗｔ％、樹脂８ｗｔ％、フラックス７ｗｔ％の組成とした他は、実施例と同じ方法で接着フィルムを作製した。なお、比較例２で用いられているアビエチン酸のｐｋａは、約＋４．６である。
＜比較例３＞
　表２の組成にて、実施例と同じ方法で接着フィルムを作製した。すなわち、比較例２において、フラックスであるアビエチン酸の添加量を１ｗｔ％とした。
＜支持基材＞
　市販の低密度ポリエチレンよりなる樹脂ビーズ（日本ポリエチレン（株）製　ノバテックＬＬ）を１４０℃で溶融し、押し出し機を用いて厚さ１００μｍの長尺フィルム状に成形した。
＜粘着剤組成物＞
　ｎ－オクチルアクリレート、２－ヒドロキシエチルアクリレート、メタクリル酸、重合開始剤としてベンゾイルペルオキシドの２００：１０：５：２（重量比）混合物を適量のトルエン中に分散し、反応温度および反応時間を調整し、官能基を持つアクリル樹脂の溶液を得た。次にこのアクリル樹脂溶液に、ポリイソシアネートとしてコロネートＬ（日本ポリウレタン製）を前記アクリル樹脂溶液１００重量部に対して２重量部と、追加の溶媒として適量のトルエンを加え、攪拌して粘着剤組成物１を得た。
＜ダイシングテープ＞
　支持基材上に粘着剤組成物１の乾燥後の厚さが５μｍになるように前記粘着剤組成物を塗工し、１２０℃で３分間乾燥させてダイシングテープを作成した。
　実施例１～５、比較例１～３によって得られた接着フィルム、およびそれを用いたダイシングダイボンドテープにおいて、以下に記す項目について評価を行った結果について、同じく表２に示す。
・体積抵抗率・・・ＪＩＳ－Ｋ７１９４に準拠した四探針法にて測定
・ＤＳＣ・・・ＤＳＣ測定装置（日立ハイテク製　ＤＳＣ７０００）を用いて、焼結前の各サンプルについて２００～２５０℃の温度領域において吸熱ピークの有無を確認した。
次いで、各サンプルを窒素下２５０℃にて４時間焼結したものについても同様の測定を実施した。
・接着力・・・接着フィルムをダイシングテープと貼り合せることでダイボンディングフィルムを調整し、裏面をＡｕメッキされたＳｉウェハに１００℃で貼合の後、５ｍｍ□にダイシングして、個片化したチップおよび接着フィルムを得た。Ａｇメッキされた金属リードフレーム上に１４０℃でダイボンディングした後、２３０℃で３時間焼結した作成したサンプルについて、ダイシェアー測定機（アークテック製　シリーズ４０００）にて２６０℃におけるせん断接着力を測定した。
・ＴＣＴ後の接着力・・・上記と同じサンプルを－４０～＋１５０℃×２００の冷熱衝撃（ＴＣＴ）処理後に、２６０℃におけるせん断接着力を測定した。
・ＭＳＬ－Ｌｖ１、Ｌｖ２後のＰＫＧ剥離の有無・・・接着力と同じサンプルをエポキシ系のモールド樹脂にて封止した後、ＪＥＤＥＣ　Ｊ－ＳＴＤ－０２０Ｄ１に定める吸湿後リフロー試験（鉛フリーはんだ準拠）のＭＳＬ－Ｌｖ１、Ｌｖ２（表３参照）にて処理した後、超音波画像装置（日立パワーソリューション製　ＳＡＴ）にて内部に剥離が生じていないかを観察した。
[規則26に基づく補充 26.05.2016]　
Figure WO-DOC-TABLE-2
Figure JPOXMLDOC01-appb-T000008
　上記結果から、金属粒子と、熱硬化性樹脂と、フラックスとしてルイス酸性を有する化合物または熱酸発生剤とを含む導電性接着フィルムであって、前記ルイス酸性を有する化合物または熱酸発生剤のｐｋａが－０．４を下回る実施例１～７の導電性接着フィルムは、環境負荷の高い鉛はんだを用いず、また、フラックスの添加量が１ｗｔ％と少ないにもかかわらず、耐熱性、吸湿信頼性、結合信頼性を併せ持つ、従来技術にない顕著な効果を奏することが証明された。
　これに対して、フラックスとしてルイス酸や熱酸発生剤ではないテトラエチレングリコールを用いた比較例１、ルイス酸ではあるもののｐＫａが高いアビエチン酸を用いた比較例２では、ＴＣＴ後の接着力が低く、さらに、比較例１、２ではフラックスを多く用いているため、ＭＳＬ試験後にも内部剥離を示すなど、吸湿信頼性、結合信頼性に難があることが証明された。また、アビエチン酸の添加量を実施例と同じく少量とした比較例３からは、本願実施例との差異がますます明らかであり、接着力が実施例と比較して大幅に劣ることが証明された。また、アビエチン酸は弱酸であるため、実施例のような少量の添加では酸化膜を除去することができない。よって酸化膜が障壁となり、金属間の拡散反応が進まないため、焼結後も吸熱ピークが残ってしまう結果となった。
１：半導体ウェハ
１ａ：裏面Ａｕメッキ層
２：半導体チップ
４：金属リードフレーム
４ａ：Ａｇメッキ層
５：モールド樹脂
６：Ａｌワイヤ
１０：ダイシング・ダイボンディングフィルム
１１：剥離処理PET
１２：ダイシングテープ
１２ａ：支持基材
１２ｂ：粘着剤層
１３：接着フィルム
２０：リングフレーム
２１：ダイシングブレード
２２：吸着ステージ
３０：テープ突き上げリング
３１：突き上げピン
３２：吸着コレット

Claims (15)

  1. 　金属粒子と、熱硬化性樹脂と、ルイス酸性を有する化合物または熱酸発生剤とを含む導電性接着フィルムであって、
    前記ルイス酸性を有する化合物または熱酸発生剤が、
    フッ化ホウ素またはその錯体、
    ｐＫａ＝－０．４以下のプロトン酸、
    またはｐＫａ＝－０．４以下のプロトン酸の塩と同一のアニオンと、水素イオンまたはその他のカチオンとを組み合わせた塩または酸
    から選択されるものである
    ことを特徴とする導電性接着フィルム。
  2. 　前記ルイス酸性を有する化合物または熱酸発生剤において、アンチモンおよびヒ素成分の総量が０．１ｗｔ％未満であることを特徴とする、請求項１記載の導電性接着フィルム。
  3. 　前記ルイス酸性を有する化合物または熱酸発生剤が、フッ化ホウ素またはその錯体、フッ化ホウ素酸塩またはポリフルオロアルキルホウ素酸またはその塩、ポリフルオロアリールホウ素酸またはポリフルオロアルキルフルオロリン酸またはその塩、ポリフルオロアリールフルオロリン酸またはその塩から選択されるものであることを特徴とする、請求項１または２に記載の導電性接着フィルム。
  4. 　前記ルイス酸性を有する化合物または熱酸発生剤が、アリールスルホニウムカチオンの塩、アリールヨードニウムカチオンの塩から選択されるものであることを特徴とする、請求項１または２に記載の導電性接着フィルム。
  5. 　前記導電性接着フィルム中、前記ルイス酸性を有する化合物または熱酸発生剤の重量分率が０．３～３ｗｔ％であり、かつ金属粒子の重量分率が７０～９６ｗｔ％であることを特徴とする、請求項１～４いずれか記載の導電性接着フィルム。
  6. 　前記ルイス酸性を有する化合物または熱酸発生剤の沸点または昇華点が、常圧で２００℃以上であることを特徴とする、請求項１～５いずれか記載の導電性接着フィルム。
  7. 　前記導電性接着フィルム中、鉛および水銀およびアンチモンおよびヒ素成分の総量が０．１ｗｔ％未満であることを特徴とする、請求項１～６いずれか記載の導電性接着フィルム。
  8. 　前記金属粒子の少なくとも１部が、Ｃｕ、Ｎｉ、Ｓｎのいずれかを含むことを特徴とする、請求項１～７いずれか記載の導電性接着フィルム。
  9. 　前記金属粒子が、相互に金属間化合物形成が可能な組み合わせを含む２種以上の金属の混合物であることを特徴とする、請求項１～８いずれか記載の導電性接着フィルム。
  10. 　前記２種以上の金属粒子の少なくとも２種がＣｕ、Ａｇ、Ｎｉ、Ｔｉ、Ａｌ、Ｓｎ、Ｚｎ、Ａｕ、Ｉｎから選択されるものであることを特徴とする、請求項９記載の導電性接着フィルム。
  11. 　焼結前はＤＳＣ（示差走査熱量測定）により観測される吸熱ピークが１００℃～２５０℃において少なくとも１つ存在し、かつ、焼結後はそれが観測されなくなることを特徴とする、請求項１～１０いずれか記載の導電性接着フィルム。
  12. 　前記熱硬化性樹脂が、イミド基を１分子に２単位以上含むマレイン酸イミド化合物を含むことを特徴とする、請求項１～１１いずれか記載の導電性接着フィルム。
  13. 　マレイン酸イミド化合物が、Ｃ１０以上の脂肪族アミンに由来する骨格を含むことを特徴とする、請求項１２記載の導電性接着フィルム。
  14. 　エポキシ化合物を含むことを特徴とする、請求項１～１３いずれか記載の導電性接着フィルム。
  15. 　請求項１～１４いずれか記載の導電性接着フィルムと、粘着テープとを貼り合せてなる、ダイシングダイボンディングフィルム。
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