CN101724271A - Silicone rubber sheet for thermocompression bonding - Google Patents
Silicone rubber sheet for thermocompression bonding Download PDFInfo
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- CN101724271A CN101724271A CN200910179172A CN200910179172A CN101724271A CN 101724271 A CN101724271 A CN 101724271A CN 200910179172 A CN200910179172 A CN 200910179172A CN 200910179172 A CN200910179172 A CN 200910179172A CN 101724271 A CN101724271 A CN 101724271A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/10—Metal compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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Abstract
The invention provides a silicone rubber sheet for thermocompression bonding, which is characterized in that the silicone rubber composition containing components (A) to (E) is formed into sheets and cured to form the silicone rubber sheets, having elongation ratio of 50-120% when being cut under the temperature of 23 DEG C., hardness measured by an A-type hardometer, and heat conduction of 0.5-1.0 W/mK, wherein (A) is 100 weight parts of organopolysiloxane with average degree of polymerization of over 3000; (B) is 50-250 weight parts of at least one heat conductive powder selected from metal, metal oxide, metal nitride and metal carbide; (C) is 5-60 weight parts of carbon soot powder; (D) is 0-40 weight parts of micro-powder reinforced silicon dioxide with BET ratio superficial area of over 50m2/g, with total weight of component (C) and component (D) 10-60 weight parts; and (E) is a curing agent.
Description
Technical field
The present invention relates to a kind ofly have heat conductivity and with to the silicone rubber sheet for thermocompression bonding of being exerted pressure equably by the pressing thing and using into purpose, though particularly relate to the good deterioration that tension set causes when carrying out pressing repeatedly more than 300 ℃ of thermotolerance also less, for the weather resistance of physical disturbance elongation also good, when cutting off little and appropriate and have the hardness of appropriateness and appropriateness thermal conductivity, be used for silicone rubber sheet for thermocompression bonding in the pressing that is connected the anisotropic conductive film of using of the electrode of liquid-crystal display etc.; And the silicone rubber sheet for thermocompression bonding of energy high precision pressing that goes for the shaping of plywood and flexible circuit board.
Background technology
In recent years, extensively popularize with indicating meters such as indicating meter, pick up camera, digital camera, navigationsystem, slim TV machine, liquid crystal panel, plasma display and organic EL panel as mobile phone, portable computer, computer.Recently, as the medium that can rewrite, Electronic Paper begins to popularize, in these display panels, in order to drive image, with the lead-in wire electrode of panel side with carried the lead-in wire electrode that drives with the flexible circuit board of LSI and come hot pressing, thereby be electrically connected and mechanical connection by the anisotropic conductive caking agent.
In recent years, particularly be that the height at the center technique for displaying that becomes more meticulous constantly develops with the liquid crystal panel, require the thin spaceization of described lead-in wire electrode therefrom.But, in the connection operation between the lead-in wire electrode that has used the anisotropic conductive caking agent, tolerance of dimension during except each lead-in wire electrode forming, therefore dislocation (malposition) between lead-in wire electrode when coefficient of thermal expansion difference of bit errors, flexible circuit board and panel between the electrode of also can going between and pressing etc. will connect not a duck soup between the lead-in wire electrode with the thin space setting.
As silicone rubber sheet for thermocompression bonding, known the silicon rubber sheet material (patent documentation 1) that carried out strengthening with woven fiber glass and obtained is for example arranged in silicon rubber in the blending boron nitride, in silicon rubber, strengthen with woven fiber glass in blending boron nitride and the conductive material and given the silicon rubber sheet material (patent documentation 2) of static electricity resistance, good heat conductivity material such as blending pottery or metal and the silicon rubber sheet material (patent documentation 3) that obtains etc. in silicon rubber.But the thermotolerance of the basic demand of these silicone rubber sheet for thermocompression bonding and resiliency etc. do not reach optimizing, therefore when these silicon rubber sheet materials being used to connect between the lead-in wire electrode that is provided with thin space, can't obtain good result.
Patent documentation 1: Japanese kokai publication hei 5-198344 communique
Patent documentation 2: Japanese kokai publication hei 6-36853 communique
Patent documentation 3: Japanese kokai publication hei 6-289352 communique
In addition, also known have in silicon rubber dewater exceptionally volatile component of blending be the silicon rubber sheet material (patent documentation 4) that is improved of carbon black 0.5% below and thermotolerance, be 100m by admixing the BET specific surface area
2The above carbon black of/g further improves stable on heating silicone rubber sheet for thermocompression bonding (patent documentation 5).Yet, though this silicone rubber sheet for thermocompression bonding thermotolerance and weather resistance are very excellent, connecting the sheet material between the lead-in wire electrode that is provided with thin space as reply, it exists elongation, hardness and thermal conductivity etc. when cutting off not to reach optimized shortcoming.As mentioned above, do not obtain to tackle to go between the tendency that electrode is provided with thin space and the silicone rubber sheet for thermocompression bonding of thermotolerance and excellent in te pins of durability as yet.
Patent documentation 4: Japanese kokai publication hei 7-11010 communique
Patent documentation 5: TOHKEMY 2003-261769 communique
For this reason, the present inventor concentrates on studies to not only thermotolerance and excellent in te pins of durability and the silicone rubber sheet for thermocompression bonding that also can tackle the tendency that spacing narrows down between the electrode of lead-in wire electrode.It found that: the hardness under (1) room temperature of silicon rubber sheet material, the elongation when (2) cut off and these three characteristics of (3) thermal conductivity are extremely important for the tendency that spacing between the electrode of reply lead-in wire electrode narrows down, and as the heat conductivity powder, preferred silicon metal powder and/or the crystallinity SiO 2 powder of adopting, when using these powder, therefore can reduce the compression permanent stress of silicon rubber sheet material, be easy to reduce based on the deterioration that tension set caused of pressing repeatedly.In addition, because above-mentioned two kinds of powder are low-gravity, therefore can also alleviate the proportion of sheet material, so the operability of silicon rubber sheet material is also good.
In addition, as the silicon rubber of having admixed silicon metal powder, known have a heat conductivity organopolysiloxane composition (patent documentation 6) of having filled aluminium nitride and silicon metal powder simultaneously, Pure Silicon Metal is incorporated in the silicon rubber and heat conductivity rubber composition that obtains and molding thereof (patent documentation 7) as the heat conductivity weighting agent, the blending median size is the following silicon metal powder of 100 μ m and takes into account high thermoconductivity and the high thermal conductivity rubber composition (patent documentation 8) of low compression permanent stress, having admixed median size is high thermal conductivity heat fixing roll or photographic fixing band rubber composition and the heat fixing roll or the photographic fixing band (patent documentation 9) of the following silicon metal powder of 100 μ m, but they all do not consider the application of silicone rubber sheet for thermocompression bonding, at the hardness of silicone rubber sheet for thermocompression bonding purposes, elongation and thermal conductivity do not reach optimizing.
Patent documentation 6: Japanese kokai publication hei 3-14873 communique
Patent documentation 7: TOHKEMY 2000-63670 communique
Patent documentation 8: TOHKEMY 2007-138100 communique
Patent documentation 9: TOHKEMY 2007-171946 communique
In addition, admixed the silicon rubber sheet material of silicon metal powder as considering the hot pressing purposes, known have admixed the thermal conduction elastic sheet material (patent documentation 10) of silicon metal powder as the agent of thermal conduction electrical isolation.But this sheet material is not owing to hardness, elongation and the thermal conductivity at the hot pressing purposes reaches optimizing, and therefore existing problems when using as the hot pressing sheet material particularly can't connect as thin space really and use with sheet material.
Patent documentation 10: TOHKEMY 2007-311628 communique
Summary of the invention
That is use when, the 1st purpose of the present invention is to provide hot pressing excellent in te pins of durability under the high temperature more than 300 ℃ and the thin space in make liquid-crystal display etc. by anisotropic conductive film to go between pressing between the electrode at interval, be applicable to the silicone rubber sheet for thermocompression bonding that high precision hot press closes.
The 2nd purpose of the present invention is to provide the silicone rubber sheet for thermocompression bonding buffering sheet material, that can realize the high precision shaping that uses when being suitable as plywood or flexible circuit board shaping.
The present inventor concentrates on studies in order to reach above-mentioned each purpose, found that: in the so-called mixed milling type organopolysiloxane high as the polymerization degree of stock polymer, when mixing heat conductivity powder, carbon black powder and solidifying agent by a certain percentage, mixing a certain amount of BET specific surface area as required is 50m
2The micro mist enhancing property silicon-dioxide that/g is above, so that elongation is 50～120% during the cut-out under 23 ℃, by the hardness under fixed 23 ℃ of A type hardness tester instrumentation is 65～75, and thermal conductivity is 0.5～1.0W/mK, make its curing after the composition that obtains is configured as sheet, can obtain good result this moment, thereby finished the present invention.
Promptly, the present invention relates to a kind of silicone rubber sheet for thermocompression bonding, it is characterized in that it is to make its silicon rubber sheet material that is solidified to form after following rubber composition is configured as sheet, described rubber composition contains: (A) mean polymerisation degree is organopolysiloxane 100 mass parts more than 3000; (B) be selected from least a kind of heat conductivity powder 50～250 mass parts in metal, metal oxide, metal nitride and the metallic carbide; (C) carbon black powder 5～60 mass parts; (D) the BET specific surface area of 0～40 mass parts is 50m
2The enhancing fine silica powder that/g is above, and the total amount of composition (C) and composition (D) is 10～60 mass parts; And (E) solidifying agent, elongation is 50～120% during the cut-out of described silicone rubber sheet for thermocompression bonding under 23 ℃, be 65～75 by the hardness under fixed 23 ℃ of A type hardness tester instrumentation, and described thermal conductivity is 0.5～1.0W/mK.
In the present invention, preferred average degree of polymerization is the organopolysiloxane molecule formation a kind or more of the organopolysiloxane of (A) composition more than 3000 by the organopolysiloxane that has average at least 2 alkenyls in 1 molecule that comprises a following average group accepted way of doing sth (1) expression, 0.10～0.30 mole of % of the total R that contains in the organopolysiloxane molecule of above-mentioned (A) composition is a vinyl, regulate described (A) composition and (D) consumption of composition, so that total ethene base unit weight P of organopolysiloxane molecule that should (A) composition (mole %) be 0.20～0.50 with the mass parts of the enhancing SiO 2 powder of (D) composition divided by the value of the total of the numerical value Q addition that obtains after 100, and (E) solidifying agent of composition constitutes by having 2 organic hydride polysiloxane and platinum class catalyzer with Siliciumatom bonded hydrogen atom in 1 molecule at least.
R
nSiO
(4-n)/2 (1)
Wherein, the n in the formula (1) represents 1.9～2.4 positive number, and R represents to replace or unsubstituted monovalence alkyl, and 0.0001～10 mole of % of the R that each molecule had is a vinyl, and 80 moles of % above be methyl.
In the present invention, preferably the heat conductivity powder as (B) composition is a silicon metal powder, and preferred especially median size is 1～20 μ m.The spherical powder that its shape is preferably the unbodied what is called " broken powder " made by comminuting method or is made by atomization etc.Surface at above-mentioned silicon metal powder can form the forced oxidation film.In addition, when the heat conductivity powder as (B) of the present invention composition is a median size when being the crystallinity SiO 2 powder of 1～20 μ m, also be optimal way of the present invention.In addition, the thickness of silicone rubber sheet for thermocompression bonding of the present invention is preferably in the scope of 0.05～1mm.
Silicon rubber sheet material of the present invention is the hot pressing excellent in te pins of durability not only, and the elongation when cutting off is less, therefore have the hardness of appropriateness and the thermal conductivity of appropriateness, being suitable as by anisotropic conductive film is the silicone rubber sheet for thermocompression bonding that uses during hot pressing accurately between the lead-in wire electrode of thin space with interelectrode distance.In addition, silicon rubber sheet material of the present invention when being used as the buffer substrate tablet that uses when plywood or flexible circuit board are shaped, can be realized high-precision shaping.
Description of drawings
Fig. 1 is that silicone rubber sheet for thermocompression bonding of the present invention is used in explanation, the mode chart of the method for the ACF hot pressing that will clip with FPC.
(nomenclature)
1a. copper electrode
1b.ITO electrode
2a. flexible printed circuit running board
2b. sheet glass
3. anisotropic conductive film
4. bearing tool (brace table)
5. silicone rubber sheet for thermocompression bonding
6. heating, pressurization apparatus
Embodiment
At first, the term " median size " that uses in this specification sheets and the meaning of " mean polymerisation degree " are described.
" median size ":
About the sooty median size, measure primary particle size according to the photo of taking with electron microscope, the particle diameter of trying to achieve is carried out arithmetical mean, the promptly so-called median size of utilizing electron microscope method to measure.Usually, sooty primary particle cohesion and form offspring, but the median size that said here median size is not its offspring, and be meant the median size of primary particle.
The median size of heat conductivity powder is meant by optical diffraction/scattering method size-grade distribution, is 50% o'clock particle diameter from its small particle size side quality aggregate-value totally.Concrete mensuration, the particle-size analyzer Micro Track that for example can utilize Nikkiso Company Limited to make waits and carries out.
" mean polymerisation degree ":
The mean value that means the Siliciumatom number of the siloxane bond that becomes skeleton in the organopolysiloxane etc.
Then, the composition that the present invention is used describes.
[composition]
The height that is accompanied by display panels such as liquid crystal panel becomes more meticulous, and the driving that the lead-in wire electrode of panel side and having carried is used to drive image has the tendency that narrows down with spacing between each electrode of the outer lead electrode of the flexible circuit board of LSI.Be directed to this, when utilizing between electrode the anisotropic conductive film between the closely spaced lead-in wire electrode to carry out high-precision hot pressing when connecting, the dislocation when suppressing pressing between the lead-in wire electrode is very important.
The dislocation of the lead-in wire electrode when suppressing above-mentioned hot pressing, silicone rubber sheet for thermocompression bonding of the present invention has the feature of (1) shown below～(3).
Elongation when cutting off under (1) 23 ℃ the room temperature must be less, is 50～120%, is preferably 60～110% especially.Basic, from the viewpoint of the dislocation of lead-in wire electrode, elongation is the smaller the better.But, when elongation is lower than 50%,, therefore have following problem: when being existed concavo-convex by pressing portion or during difference of altitude, partial stress can not being disperseed, thereby disconnect easily because the flexibility of sheet material is not good enough; Perhaps when sheet material was applied the power of overbending direction, sheet material can rupture.
(2) hardness under 23 ℃ of room temperatures that record with A type hardness tester meter (Durometer) is necessary for 65～75, is preferably 67～73 especially.Can not only prevent from the to go between dislocation of electrode of this hardness, can also revisal by the tolerance of the planeness of pressing thing, Flatness or parallelism, take into account the resiliency that is used to transmit uniform pressure.
Thermal conductivity under (3) 23 ℃ of room temperatures is necessary for 0.5～1.0W/mK, is preferably 0.6～0.9W/mK especially.In order to reach anisotropic conductive film from the heat of the heating apparatus of hot pressing device, thermal conductivity is high more good more, but if thermal conductivity greater than 1.0W/mK, then heat can excessively conduct to anisotropic conductive film sharp.At this moment, the viscosity of the anisotropic conductive film before solidifying is excessive descent and flowing out between connection electrode sharp, and it is insufficient that the electrical connection of electrode becomes sometimes.
On the other hand,, then be difficult to conduct heat, therefore have to improve the temperature of heating apparatus to anisotropic conductive film if be lower than 0.5W/mK.In order to improve the temperature of heating apparatus, the burden of hot pressing device.In addition, because the higher heating apparatus of temperature contacts with silicone rubber sheet for thermocompression bonding, can impel the thermal degradation when of silicon rubber sheet material.In addition, pyritous heating apparatus is granted radiant heat to the colour filter of heat labile liquid crystal panel etc., thereby also can cause problem.
Next, promptly (A) composition～(E) composition describes to the necessary composition in the composition of the present invention's use.
(A) composition:
(A) composition that the present invention uses, be that mean polymerisation degree is the organopolysiloxane more than 3000, for example use a following average group accepted way of doing sth (1) to represent.
R
nSiO
(4-n)/2 (1)
Wherein, the n in (1) formula represents 1.95～2.4 positive number, and R represents to replace or unsubstituted monovalence alkyl.
The replacement of representing as R or the object lesson of unsubstituted monovalence alkyl can example illustrate alkyl such as methyl, ethyl, propyl group; Cycloalkyl such as cyclopentyl, cyclohexyl; Alkenyl such as vinyl, allyl group; Aryl such as phenyl, tolyl; Or the part of the hydrogen atom of these groups is replaced by halogen atoms such as chlorine atom, fluorine atoms and the halo alkyl that obtains etc.
As the organopolysiloxane of (A) composition, organopolysiloxane that preferred main chain is made of dimethyl siloxane units or the organopolysiloxane that has imported organic groups such as methyl, vinyl, phenyl, trifluoro propyl at the main chain of this organopolysiloxane.0.0001～10 mole of % of preferred especially above-mentioned organic group is a vinyl, and 80 moles of % above be methyl.In addition, also preferred molecule chain end is by three organosilicon alkyl or hydroxy-end capped.As this three organosilicons alkyl, can TMS, dimethyl vinyl silanes base, trivinyl silylation etc. be shown example.
As the organopolysiloxane of (A) composition, can only use a kind, also can multiple mixing use, 0.10～0.30 mole of % of total R that the organopolysiloxane molecule integral body of (A) composition that preferably above-mentioned (1) formula is represented is had is a vinyl.In addition, in the present invention, the mean polymerisation degree of (A) composition that (1) formula is represented is necessary for more than 3000.If the polymerization degree is lower than 3000, the physical strength after then solidifying descends.
(B) composition:
(B) composition is at least a kind of heat conductivity powder that is selected from metal, metal oxide, metal nitride and the metallic carbide, and it is to give the weighting agent of silicon rubber sheet material of the present invention with heat conductivity.About their object lesson, as metal, can enumerate silver, copper, iron, Pure Silicon Metal, nickel, aluminium etc., as metal oxide, zinc oxide, aluminum oxide, magnesium oxide, silicon-dioxide, ferric oxide etc. can be enumerated,, boron nitride, aluminium nitride, silicon nitride etc. can be enumerated as metal nitride, as metallic carbide, can enumerate silicon carbide, norbide etc.
In the above-mentioned heat conductivity powder, special preferable alloy Si powder and crystallinity SiO 2 powder.By using these powder, can reduce compression molding stress, the deterioration that tension set caused that is produced by pressing repeatedly reduces, thereby can obtain the silicone rubber sheet for thermocompression bonding of excellent in te pins of durability.In addition, two powder are low-gravity, can alleviate the proportion of sheet material, so the operability of silicone rubber sheet for thermocompression bonding is good.
The shape of these powder can be spherical, ellipticity, flats, have corner angle amorphous, that band is circular is amorphous, the arbitrary shape in the needle-like etc., does not have particular restriction.For example for the situation of Pure Silicon Metal, can example illustrate sphere, by pulverizing obtain amorphous etc.
The purity of heat conductivity powder does not have particular restriction, from giving the viewpoint of heat conductivity, is preferably more than 50%, is preferably especially more than 80%, more preferably more than 95%.For the high silicon metal powder of purity, the natural oxide film on surface does not have defective, and high high-temp stability is good, particularly preferably in the surface of silicon metal powder the forced oxidation film is set.By the forced oxidation film is set, the crosslinking reaction of the organopolysiloxane when energy elimination meeting is shaped to sheet material is brought the avtive spot on dysgenic silicon metal powder surface.
The median size of the heat conductivity powder that the present invention uses does not have particular restriction, is preferably 0.1～50 μ m, is preferably 0.5～20 μ m especially, most preferably is 1～10 μ m.If median size is lower than 0.1 μ m, then the specific surface area of powder increases relatively, thus be difficult to carry out highly-filled, thereby cause the insufficient while of thermal conductivity, it is really up to the mark that the rubber after the curing becomes sometimes.On the other hand, greater than 50 μ m, when the rubber after then solidifying became fragile, the surface occurred concavo-convex easily, thereby not preferred as if median size.
For the blending amount of (B) of the present invention composition, with respect to (A) composition 100 mass parts, be necessary for 50～250 mass parts, use in the scope particularly preferably in 70～200 mass parts.If more than 250 mass parts, then blending becomes difficult, and the shaping processability variation.If be less than 50 mass parts, then thermal conductivity deficiency.
(C) composition:
(C) composition that the present invention uses is a carbon black, is improving the stable on heating while by the physical strength that improves the silicon rubber sheet material, the physical strength when particularly heating, the static electricity resistance of giving heat conductivity and producing because of conduction.
Carbon black is divided into furnace treated black, thermally oxidized black, thermal black, Shawinigan black etc. according to its manufacture method, contains the more of impurity such as sulphur usually.It is the following carbon black of 0.5 quality % that the present invention preferably makes the volatile component beyond the water.Shawinigan black particularly is because impurity is few and preferred.
The measuring method of the volatile component beyond the above-mentioned water is on the books in " the rubber grade carbon black test method " of JIS K 6221.Particularly, in crucible, add the carbon black of specified amount, be determined at 950 ℃ of heating volatile losses after 7 minutes down.
(C) the sooty median size of composition is preferably the scope of 10～300nm, is preferably the scope of 15～100nm especially.In addition, the BET specific surface area is preferably 20～300m
2/ g is preferably 30～200m especially
2/ g.
For the blending amount of (C) of the present invention composition, with respect to (A) composition 100 mass parts, be preferably 5～60 mass parts, use in the scope particularly preferably in 10～55 mass parts.If be lower than 5 mass parts, then the raising of heat conductivity and heat-resisting pressing is insufficient, if surpass 60 mass parts, then is difficult to the homogeneous blending, and the shaping processability extreme difference of the composition that obtains.
(D) composition:
(D) composition that the present invention uses, be that the BET specific surface area is 50m
2The above enhancing fine silica powder of/g uses as the enhancing ingredients of silicon rubber.This fine particle silica can be hydrophilic, also can be hydrophobic, but from enhancing property effect aspect, the BET specific surface area is preferably 50～800m
2/ g is preferably 100～500m especially
2The fine particle silica of/g.Specific surface area is lower than 50m
2During/g, effect can't fully be enhanced.
For the blending amount of (D) of the present invention composition, with respect to (A) composition 100 mass parts, be preferably 0～40 mass parts, more preferably 5～35 mass parts are preferably 10～30 mass parts especially.If more than 40 mass parts, then the plasticity number of rubber composition is too high sometimes, the plasticity variation, or the rubber after solidifying is really up to the mark.
In addition, in the present invention, the total amount of composition (C) and composition (D) is necessary for 10～60 mass parts.Be preferably 20～50 mass parts.If be lower than 10 mass parts, the undercapacity of the silicon rubber that then obtains if surpass 60 mass parts, then be difficult to the homogeneous blending, and the plasticity number of the composition that obtains is too high, causes the shaping processability extreme difference.
(E) composition:
(E) composition that the present invention uses is suitably to select to use in the solidifying agent known solidifying agent that can use from the curing of silicon rubber usually.As such solidifying agent, for example can example illustrate: the ditertiary butyl peroxide that a) uses in the free radical reaction, 2, organo-peroxides such as 5-2, dicumyl peroxide; B) when the organopolysiloxane of (A) composition has alkenyl,, contain more than 2 combination with platinum metals class catalyzer such as the organic hydride polysiloxane of Siliciumatom bonded hydrogen atom and platinum, palladiums etc. in 1 molecule as the addition reaction solidifying agent.Among the present invention, for being easy to reasons such as control reaction, reaction residues noresidue, preferred b) the addition reaction solidifying agent, as required also can be with both and usefulness.The addition of these solidifying agent, if with the situation of common silicon rubber under equally, generally as follows.
About solidifying agent a), with respect to A) organopolysiloxane 100 mass parts of composition, use 0.1～20 mass parts.
About solidifying agent b), make and contain the amounts with Organhydridosiloxaneresins above-mentioned Siliciumatom bonded hydrogen atom more than 2 in above-mentioned 1 molecule and be: this Organhydridosiloxaneresins had and Siliciumatom bonded hydrogen atom is 0.5～5 mole for 1 mole with respect to the alkenyl of (A) composition, and the amount of platinum metals class catalyzer is: metal ingredient is the scope of 0.1～1000ppm (quality criteria) with respect to (A) composition.
Connect with high precision and keeping under the closely spaced state in order to use anisotropic conductive film will go between between the electrode, when the hardness of controlling silicon rubber sheet material of the present invention and elongation, the interaction between the crosslinking degree between polysiloxane molecule and powder filler and polysiloxane molecule must be controlled in the suitable scope.Make degree of crosslinking between polysiloxane molecule be easy to control by the control addition reaction, during mixed milling type silicon rubber that particularly polymerization degree is high, can control by the containing ratio that control participates in crosslinked vinyl.Under the situation of silicon rubber, as the interaction between polysiloxane molecule and the powder filler, the false crosslinked interaction that produces that the hydrogen bond of known polysiloxane molecule and enhancing property silicon-dioxide causes is very big.Therefore, for the silicon rubber that is cured as main crosslinking reaction that causes with addition reaction, by the blending of vinyl containing ratio and enhancing property silicon-dioxide is measured these two controlling factors in the suitableeest scope, the hardness and the elongation of silicon rubber sheet material of the present invention can be adjusted to the ideal scope.
Particularly, when making 0.10～0.30 mole of % among the total R that contains in the side chain of the total molecule of organopolysiloxane of (A) composition be vinyl, regulate (A) composition and (D) composition make should (A) composition be the mole % value (P) of the vinyl in the side chain total amount of organopolysiloxane molecule integral body and (D) composition promptly enhancing property fine silica powder be 0.20～0.50 with respect to the aggregate value (P+Q) that the mass parts of (A) composition 100 mass parts obtains divided by 100 numerical value that obtains (Q) additions, carry out addition reaction then it is solidified, the hardness and the elongation of silicon rubber sheet material of the present invention can be adjusted in the ideal scope.
The aggregate value of above-mentioned (P+Q) is lower than at 0.20 o'clock, the false cross-linking set sum deficiency that the cross-linking set that addition reaction produces and hydrogen bond by enhancing property SiO 2 powder and polysiloxane molecule form, so not only elongation is excessive, it is insufficient that hardness also can become.Otherwise if surpass 0.50, then cross-linking set and false cross-linking set sum are excessive, so elongation is too small, and sheet material becomes fragile, and weather resistance descends, and becomes really up to the mark, the resiliency deficiency.
Other composition
In rubber composition of the present invention, can also add tackifier such as dispersion agent, silane coupling agent, titanium coupling agent such as weighting agents such as heat-resisting imparting agent such as cerium oxide, ferric oxide, titanium oxide, potter's clay, lime carbonate, diatomite, titanium dioxide, low molecular weight polyorganosiloxane ester, silanol as required, give flame retardant resistance the platinum metals compounds, improve the polytetrafluoroethylparticle particle etc. of the green strength of sizing material.
Preparation and processing
The rubber composition that the present invention uses, with mixing the getting final product of each composition that mixing machines such as two roller mills, kneader, Banbury mixer will use, usually, having only solidifying agent is to be added to before use, preferably in advance that other compositions are mixing.
As the manufacturing process of silicon rubber sheet material of the present invention, can list with rolling press or forcing machine will admix comprise solidifying agent after the rubber composition of interior all the components is made specific thickness, carry out the solidified method, with the rubber composition of liquid state or be dissolved in the rubber composition that the liquid state that obtains in the toluene equal solvent changed and carrying out solidified method etc. after the coating on the film.
The thickness of the silicon rubber sheet material after so being shaped, solidifying is 0.05～1mm, in the scope particularly preferably in 0.1～0.8mm.If thickness is lower than 0.05mm, then the resiliency deficiency can't be transmitted pressure equably.On the other hand, if thickness surpasses 1mm, then heat passage variation.
Below, enumerate embodiment and illustrate in greater detail the present invention, but the invention is not restricted to these embodiment.
Use following material in the following example.
Organopolysiloxane:
(a-1) constitute by 99.85 moles of % of dimethyl siloxane units and 0.15 mole of % of methyl vinyl siloxane unit, mean polymerisation degree is that 8000 molecular chain two ends are by the end capped methylvinyl-polysiloxane of dimethylvinylsiloxy
(a-2) constitute by 99.5 moles of % of dimethyl siloxane units and 0.5 mole of % of methyl vinyl siloxane unit, mean polymerisation degree is that 8000 molecular chain two ends are by the end capped methylvinyl-polysiloxane of dimethylvinylsiloxy
The heat conductivity weighting agent:
(b-1) median size is the metallic silicon power comminuted powder (handle through forced oxidation on the surface) of 5 μ m
(b-2) median size is the crystallinity silicon-dioxide pulverized powder of 4 μ m
(b-3) median size is the aluminum oxide powder comminuted powder of 4 μ m
Carbon black powder:
(c-1) median size is that the volatile component beyond 35nm, the water is that 0.10 quality %, BET specific surface area are 69m
2The Shawinigan black of/g
Enhancing property fine silica powder:
(d-1) the BET specific surface area is 300m
2The enhancing fine silica powder of/g (trade(brand)name: Aerosil 300, Japanese Aerosil Co., Ltd. system)
Solidifying agent:
(e-1) the vinylsiloxane complex compound of Platinic chloride (platinum content is 1 quality %)
(e-2) the hydrogenated methyl polysiloxane of following formula (1) expression
Other composition:
(f-1) dimethyldimethoxysil,ne
(g-1) the BET specific surface area is 140m
2The ceria oxide powder of/g
(h-1) ethynylcyclohexanol
[embodiment 1]
As (A) composition, employing is by (a-1) 60 mass parts and (a-2) raw material 100 mass parts that constitute of 40 mass parts, to use kneader 170 ℃ of heating 2 hours down as (f-1) 3 mass parts of the surface treatment agent of (d-1) 20 mass parts of (D) composition, conduct (D) composition and ion exchanged water 1 mass parts, admix simultaneously, mixing, thereby homogenizing.
In rubber composition 123 mass parts that obtain, add 130 mass parts as (b-1) of (B) composition, 10 mass parts as (c-1) of (C) composition and 0.5 mass parts (g-1) as heat-resisting rising agent, with pressurization kneader blending, mixing 15 minutes, thus homogenizing.
In rubber composition 100 mass parts that obtain, further with (e-1) 0.05 mass parts, as (h-1) 0.025 mass parts of the control agent of platinum catalyst and (e-2) 0.7 mass parts grind mixing one side with two rollers successively on one side and add by said sequence, prepare curable silicone rubber composition (I).
After using the calendaring molding machine that the rubber composition that obtains is made 0.25mm thickness, be transferred on polyethylene terephthalate (PET) film of thick 100 μ m.With the state of PET film-stack under in 150 ℃ process furnace by 5 minutes, flaky rubber composition is solidified.The PET film is peeled off from the stacked product of the sheet that obtains, and thermal treatment is 4 hours in 200 ℃ drying machine, and making thickness is the silicone rubber sheet for thermocompression bonding of 0.25mm.
[embodiment 2]
To use the pressurization kneader to admix as (c-1) 50 mass parts of (b-2) 140 mass parts of (a-2) 100 mass parts of (A) composition, conduct (B) composition, conduct (C) composition with as (g-1) 0.5 mass parts of heat-resisting rising agent, mixing 15 minutes, thus homogenizing.In rubber composition 100 mass parts that obtain, add (e-1) 0.1 mass parts, as (h-1) 0.04 mass parts of the control agent of platinum catalyst and (e-2) 1.0 mass parts, fully mixing with two roller mills, preparation curable silicone rubber composition (II), similarly be shaped, solidify with the situation of embodiment 1, making thickness is the silicon rubber sheet material of 0.25mm.
[embodiment 3]
Except (B) composition that (b-3) that uses 220 mass parts replaces using among the embodiment 1, operation similarly to Example 1, making thickness is the silicon rubber sheet material of 0.25mm.
Comparative example 1
Except (d-1) 30 mass parts of using (a-2) 100 mass parts as (A) composition, conduct (D) composition, (e-1) 0.1 mass parts, (h-1) 0.04 mass parts and (e-2) 1.0 mass parts, operation similarly to Example 1, making thickness is the silicon rubber sheet material of 0.25mm.
Comparative example 2
Except (a-1) that uses conduct (A) composition replaces (a-2), operation similarly to Example 2, making thickness is the silicon rubber sheet material of 0.25mm.
Comparative example 3
As (A) composition, use is by (a-1) 50 mass parts and (a-2) raw material 100 mass parts that constitute of 50 mass parts, surface treatment agent as (D) composition, use (f-1) 3 mass parts, and use ion exchanged water 1 mass parts, with kneader 170 ℃ down heating admix in 2 hours, mixing, thereby homogenizing.In rubber composition 153 mass parts that obtain, add (b-1) 320 mass parts as (B) composition, use the blending of pressurization kneader, mixing 15 minutes, thus homogenizing.In rubber composition 100 mass parts that obtain, add (e-3) 0.8 mass parts, use two roller mills evenly mixing, obtain curable silicone rubber composition (III).Once add the sulphur temperature is 170 ℃ except making, be shaped similarly to Example 1, solidify then, making thickness is the silicon rubber sheet material of 0.25mm.
[evaluation of basic physical properties]
According to the regulation of JIS K6249, elongation when measuring hardness, tensile strength and cut-out.Wherein,, use A type hardness tester meter about hardness, with the sheet layer of making to build up thickness be 6mm with on measure.Tensile strength and when cutting off elongation use the test film of No. 2, dumb-bell shape to measure.
In addition, thermal conductivity is measured according to the regulation of ASTM E 1530.
[the thickness decrement after 100 pressings]
On the bearing tool of pressing machine, only place the silicon rubber sheet material, use the heating apparatus be heated to 400 ℃, with 10 seconds be the interval, carry out directly pushing with the pressing force of 4MPa for 100 times 10 seconds action continuously.
With " the initial stage thickness of [(the initial stage thickness of sheet material)-(thickness after 100 pressings of sheet material)]/sheet material " with the numeral of the percentage record thickness decrement after as 100 pressings.
[thin space connects evaluation]
As shown in Figure 1, make the FPC (flexible printing wiring board) that is provided with 50 copper electrode 1a by 32 μ m spacings (live width 16 μ m, spacing 16 μ m) with equally by 32 μ m spacings (live width 16 μ m, spacing 16 μ m) be provided with 50 ITO electrode 1b sheet glass 2b to be provided with copper electrode 1a separately relative with the face of ITO electrode 1b side, sandwich the ACF (anisotropic conductive film) 3 of thick 22 μ m, wide 1.2mm betwixt, on the bearing tool 4 that places the pressing machine under this state.Then, with the silicone rubber sheet for thermocompression bonding 5 made in embodiment 1～3 or the comparative example 1～3 with the contacted mode mounting of the upper surface of above-mentioned FPC 2a.Then, from above-mentioned silicon rubber sheet material 5, pushed 10 seconds with the pressing force of 4MPa with the pressurization apparatus 6 that is heated to 350 ℃.So behind pressing ACF3 between FPC 2a and the sheet glass 2b, estimate conducting between copper electrode 1a and the ITO electrode 1b.The result is as shown in table 1.
[table 1]
※ vinyl+enhancing property silicon-dioxide adds up to
(A) numerical value of the mole % of the vinyl in the total amount of the side chain of the organopolysiloxane molecule integral body of the composition enhancing SiO 2 powder that adds (D) composition is with respect to the mass parts of (A) composition 100 mass parts aggregate value divided by 100 numerical value that obtain.
The silicone rubber sheet for thermocompression bonding of making of embodiment 1～3 of the present invention can be realized the connection of reply thin space, but as comparative example 1 under the situation really up to the mark, owing to resiliency is insufficient, so interelectrode conducting is incomplete.In addition, the silicon rubber sheet material that obtains in the comparative example 1 and 3 is highly brittle, and sheet material produces and breaks when folding.On the other hand, under the situation of comparative example 2, the elongation of sheet material is excessive, produces the dislocation of electrode, poor flow therefore occurs.
The possibility of industrial utilization
Even silicone rubber sheet for thermocompression bonding of the present invention is few in the deterioration that permanent deformation causes when carrying out repeatedly pressing more than 300 ℃ of the hot pressing excellent in te pins of durability under the high temperature more than 300 ℃, percentage elongation good for the durability of mechanical damage, when cutting off is little and appropriate and have the hardness of appropriateness and the pyroconductivity of appropriateness, thereby be applicable to being closed by the high precision hot press of anisotropic conductive film with Jie between the lead-in wire electrode of thin space setting of the shaping of high-precision flexible circuit board and liquid crystal display etc.
Claims (8)
1. silicone rubber sheet for thermocompression bonding, it is characterized in that, it is following rubber composition to be configured as sheet and to make its silicon rubber sheet material that is solidified to form, and described rubber composition contains: (A) mean polymerisation degree is organopolysiloxane 100 mass parts more than 3000; (B) be selected from least a kind of heat conductivity powder 50～250 mass parts in metal, metal oxide, metal nitride and the metallic carbide; (C) carbon black powder 5～60 mass parts; (D) the BET specific surface area of 0～40 mass parts is 50m
2The enhancing fine silica powder that/g is above, and the total amount of composition (C) and composition (D) is 10～60 mass parts; And (E) solidifying agent,
Elongation is 50～120% during the cut-out of described silicone rubber sheet for thermocompression bonding under 23 ℃, be 65～75 by the hardness under fixed 23 ℃ of A type hardness tester instrumentation, and thermal conductivity is 0.5～1.0W/mK.
2. silicone rubber sheet for thermocompression bonding as claimed in claim 1, it is characterized in that, described mean polymerisation degree is the organopolysiloxane molecule formation a kind or more of the organopolysiloxane of (A) composition more than 3000 by the organopolysiloxane that has average at least 2 alkenyls in 1 molecule that comprises a following average group accepted way of doing sth (1) expression
0.10～0.30 mole of % of the total R that contains in the organopolysiloxane molecule of described (A) composition is a vinyl, regulate described (A) composition and (D) consumption of composition, so that total ethene base unit weight P of organopolysiloxane molecule that should (A) composition be 0.20～0.50 with the mass parts of the enhancing SiO 2 powder of (D) composition divided by the value of the total P+Q of the numerical value Q addition that obtains after 100, the solidifying agent of (E) composition constitutes by having 2 organic hydride polysiloxane and platinum class catalyzer with Siliciumatom bonded hydrogen atom in 1 molecule at least simultaneously, described total ethene base unit weight P is in mole %
R
nSiO
(4-n)/2(1)
Wherein, the n in the formula (1) represents 1.9～2.4 positive number, and R represents to replace or unsubstituted monovalence alkyl, and 0.0001～10 mole of % of the R in each molecule is a vinyl, and 80 moles of % above be methyl.
3. silicone rubber sheet for thermocompression bonding as claimed in claim 1 or 2 is characterized in that, is silicon metal powder as the heat conductivity powder of described (B) composition.
4. silicone rubber sheet for thermocompression bonding as claimed in claim 3 is characterized in that, described silicon metal powder is that median size is the pulverized powder of 1～20 μ m.
5. silicone rubber sheet for thermocompression bonding as claimed in claim 3 is characterized in that, described silicon metal powder is that median size is the spherical powder of 1～20 μ m.
6. silicone rubber sheet for thermocompression bonding as claimed in claim 3 is characterized in that, has formed the forced oxidation film on the surface of described silicon metal powder.
7. silicone rubber sheet for thermocompression bonding as claimed in claim 1 or 2 is characterized in that, is that median size is the crystallinity SiO 2 powder of 1～20 μ m as the heat conductivity powder of described (B) composition.
8. silicone rubber sheet for thermocompression bonding as claimed in claim 1 or 2 is characterized in that, the thickness of sheet material is the scope of 0.05～1mm.
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| JP271646/2008 | 2008-10-22 | ||
| JP2008271646A JP5058938B2 (en) | 2008-10-22 | 2008-10-22 | Silicone rubber sheet for thermocompression bonding |
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| CN102424725A (en) * | 2011-11-29 | 2012-04-25 | 四川大学 | High-temperature resistant and erosion resistant rubber composition and preparation method thereof |
| CN103215008A (en) * | 2012-01-20 | 2013-07-24 | 先锋材料科技股份有限公司 | Adhesive composition and adhesive comprising the same |
| CN104497583A (en) * | 2014-12-17 | 2015-04-08 | 苏州锦腾电子科技有限公司 | Silicone rubber with high thermal conductivity and high wear-resisting property and preparation method of silicone rubber |
| CN104497585A (en) * | 2014-12-17 | 2015-04-08 | 苏州锦腾电子科技有限公司 | High-thermal-conductivity silicone rubber and preparation method thereof |
| CN105153703A (en) * | 2014-06-11 | 2015-12-16 | 傲优新材料科技（上海）有限公司 | Ceramic silicone rubber and preparation method thereof |
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| JP3078155B2 (en) * | 1993-06-28 | 2000-08-21 | 信越化学工業株式会社 | Heat resistant heat conductive thermocompression bonding sheet |
| JP4353451B2 (en) * | 2001-11-26 | 2009-10-28 | 信越化学工業株式会社 | Silicone rubber sheet for thermocompression bonding |
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| JP2004311577A (en) * | 2003-04-03 | 2004-11-04 | Shin Etsu Chem Co Ltd | Thermally conductive composite sheet and method of manufacturing the same |
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| JP4739009B2 (en) * | 2005-12-19 | 2011-08-03 | 信越化学工業株式会社 | Heat resistant and heat conductive silicone rubber sheet for thermocompression bonding |
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| TW201022390A (en) | 2010-06-16 |
| KR20100044710A (en) | 2010-04-30 |
| TWI449765B (en) | 2014-08-21 |
| KR101589312B1 (en) | 2016-01-27 |
| JP2010100692A (en) | 2010-05-06 |
| JP5058938B2 (en) | 2012-10-24 |
| CN101724271B (en) | 2013-02-06 |
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