CN103476897A - Release agent composition and release film for ceramic green sheet mold - Google Patents

Release agent composition and release film for ceramic green sheet mold Download PDF

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CN103476897A
CN103476897A CN2012800156288A CN201280015628A CN103476897A CN 103476897 A CN103476897 A CN 103476897A CN 2012800156288 A CN2012800156288 A CN 2012800156288A CN 201280015628 A CN201280015628 A CN 201280015628A CN 103476897 A CN103476897 A CN 103476897A
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organopolysiloxane
contained
remover combination
ceramic green
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CN103476897B (en
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市川慎也
深谷知巳
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Lintec Corp
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
    • C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups

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Abstract

The invention provides a release agent composition. The release agent composition contains: a polyorganosiloxane (A) which has at least two alkenyl groups in a molecule, and has an aryl group on each side chain of at least one silicon atom in a siloxane skeleton; and a polyorganosiloxane (B) which has an alkenyl group at only both ends in a molecule, but does not have an aryl group. The solid component ratio of the polyorganosiloxane (A) with respect to the total amount of the polyorganosiloxane (A) and the polyorganosiloxane (B) is 40 to 98 percent by mass, and the mass average molecular weight of the polyorganosiloxane (A) is 100,000 to 800,000. The release agent composition is excellent for ceramic slurry coatability, and is excellent for ceramic green sheet releasability.

Description

Remover combination and ceramic green moulding stripping film
Technical field
The stripping film that the present invention relates to remover combination and use ceramic green (green sheet) moulding of this remover combination to use.
Background technology
Up to now, in order to manufacture the multilayer ceramic goods that are called laminated ceramic capacitor or multilayer ceramic substrate, general passing through the ceramic green moulding, the ceramic green layer poststack sintering then multi-disc obtained is manufactured.
Ceramic green is that the ceramic size by containing the stupaliths such as barium titanate or titanium oxide is coated on stripping film and moulding.As stripping film, the general film substrate (patent documentation 1～8) that uses silicon-type compound lift-off processing such as passing through polysiloxane and obtain.For this stripping film, require to have and strip down and the separability that can not break from this stripping film will take shape in thin ceramic green on this stripping film.
In recent years, along with miniaturization and the high performance of electronic machine, laminated ceramic capacitor or multilayer ceramic substrate are to miniaturization and multiple stratification development, and ceramic green develops to filming.
The prior art document
Patent documentation
Patent documentation 1: JP 2002-011710 communique
Patent documentation 2: JP 2004-182836 communique
Patent documentation 3: JP 2004-216613 communique
Patent documentation 4: JP 2008-254207 communique
Patent documentation 5: JP 2009-034947 communique
Patent documentation 6: JP 2009-215428 communique
Patent documentation 7: JP 2009-227976 communique
Patent documentation 8: JP 2009-227977 communique
Summary of the invention
The problem that invention will solve
If by the ceramic green filming and to make its dried thickness be below 3 μ m, when then the coating ceramic size makes it dry, following phenomenon easily occurs: shrink the coating end of ceramic size, the thickness thickening of this coating end, be that shrink so-called end, produce pin hole or crawling.In addition, when by moulding ceramic green when stripping film strips down, the unfavorable condition such as break that easily occurs that strength degradation due to ceramic green causes.
And then, use the electronic material of ceramic green according to its purposes, the materials such as inorganics wherein, adhesive resin, dispersion agent, organic solvent are different, and according to the kind of ceramic size used, ceramic size changes to some extent to the coating of stripping film.Therefore, for stripping film, it is difficult reaching the coating that has both ceramic size and the separability of ceramic green.
The present invention develops in view of this present situation just, and purpose is, provides the coating of ceramic size good, the also good ceramic green moulding stripping film of separability of ceramic green, and the remover combination that is applicable to this stripping film simultaneously.
For solving the means of problem
In order to achieve the above object, the 1st aspect, the invention provides remover combination, it is characterized in that, contain: organopolysiloxane (A) has in its 1 molecule on two side chains of at least 2 thiazolinyls and at least 1 Siliciumatom in siloxane backbone and has aryl; Organopolysiloxane (B), its do not there is aryl and in 1 molecule only two ends there is thiazolinyl; Above-mentioned organopolysiloxane (A) is 40～98 quality % with respect to the solids component ratio of the total amount of above-mentioned organopolysiloxane (A) and above-mentioned organopolysiloxane (B), and the matter average molecular weight of above-mentioned organopolysiloxane (A) is 100000～800000(invention 1).
If adopt the stripping film that uses the described remover combination of foregoing invention (inventing 1) to obtain, can make the coating excellence of ceramic size, specifically, when the surface coated ceramic size at peeling agent layer and while making it dry, can suppress the coating end contraction of ceramic size and the thickness thickening of this coating end, suppress the generation that shrink so-called end.In addition, if adopt above-mentioned stripping film, can make moulding the separability of ceramic green also excellent, only need just ceramic green can be stripped down from peeling agent layer with low peeling force.
In foregoing invention (inventing 1), the matter average molecular weight of above-mentioned organopolysiloxane (B) is preferably 50000～800000(invention 2).
In foregoing invention (inventing 1,2), preferably also contain the platinum metals based compound as catalyzer (inventing 3).
In foregoing invention (inventing 1～3), preferably also contain linking agent (C) (inventing 4).
In foregoing invention (inventing 1～4), the thiazolinyl number alkyl number contained with respect to above-mentioned organopolysiloxane (A) that above-mentioned organopolysiloxane (A) is contained, meter, be preferably 0.005～0.1(invention 5 in molar ratio).
In foregoing invention (inventing 1～5), the aryl number alkyl number contained with respect to above-mentioned organopolysiloxane (A) that above-mentioned organopolysiloxane (A) is contained, meter, be preferably 0.01～0.5(invention 6 in molar ratio).
In foregoing invention (inventing 1～6), the thiazolinyl number alkyl number contained with respect to above-mentioned organopolysiloxane (B) that above-mentioned organopolysiloxane (B) is contained, meter, be preferably 0.0005～0.01(invention 7 in molar ratio).
In foregoing invention (inventing 4～7), the content of the linking agent in above-mentioned remover combination (C), preferably can make the contained hydrosilyl groups number of linking agent (C) be calculated in molar ratio as 1.0～5.0 required amounts (inventing 8) with respect to organopolysiloxane (A) and the contained thiazolinyl number of organopolysiloxane (B).
The 2nd aspect, the invention provides ceramic green moulding stripping film, the peeling agent layer that it possesses base material and at least forms on the one side of above-mentioned base material, is characterized in that, above-mentioned peeling agent layer is (the inventing 9) of using above-mentioned remover combination (inventing 1～8) to form.
The invention effect
If adopt the stripping film that uses remover combination of the present invention to obtain or adopt ceramic green moulding stripping film of the present invention, can make the coating excellence of ceramic size, specifically, when the surface coated ceramic size at peeling agent layer and while making it dry, can suppress the coating end contraction of ceramic size and the thickness thickening of this coating end, suppress the generation that shrink so-called end.In addition, if adopt the stripping film that uses remover combination of the present invention to obtain or adopt ceramic green moulding stripping film of the present invention, can make moulding the separability of ceramic green also excellent, only need just ceramic green can be stripped down from peeling agent layer with low peeling force.
Embodiment
Below, embodiments of the present invention are described.
Remover combination
The remover combination of present embodiment contains:
Organopolysiloxane (A), have in its 1 molecule on two side chains of at least 2 thiazolinyls and at least 1 Siliciumatom in siloxane backbone and have aryl; With
Organopolysiloxane (B), its do not there is aryl and in 1 molecule only two ends there is thiazolinyl;
Preferably also contain linking agent (C) and/or catalyzer (D).
Organopolysiloxane (A) is the polymkeric substance by the silicon-containing compound of following general formula (a) expression.
[changing 1]
Figure BDA00003884017900041
In formula (a), l is the integer more than 1.In addition, R 1and R 2for the alkyl of carbon number 1～12, for example can enumerate methyl, ethyl, propyl group, butyl, amyl group, hexyl, octyl group etc.R 1and R 2can be identical or different.R 1and R 2be preferably methyl.
In formula (a), m is the integer more than 1.In addition, R 3and R 4for aryl, R 3and R 4can be identical or different, be preferably identical.Like this, the structure that there is aryl on two side chains of organopolysiloxane (A) for the Siliciumatom in siloxane backbone.By this structure, when being coated on base material by remover combination, in the peeling agent layer obtained, organopolysiloxane (A) is present in the base material side of peeling agent layer more than organopolysiloxane (B), think and can obtain effect described later by such structure.
As aryl, can enumerate phenyl, benzyl, tolyl, o-Xylol base etc., wherein, preferred phenyl.
In formula (a), n is more than 1 or 2 above integers.R 5～R 8at least 2 be thiazolinyl, that is, in 1 molecule, at least 2 is thiazolinyl.For example, can be R 7and R 8both sides are thiazolinyl (n is more than 1), can be also R 7and R 8in a side be thiazolinyl, R 5and R 6in a side or both be thiazolinyl (n is more than 1), work as R 7and R 8during for the functional group beyond thiazolinyl, can be R 5and R 6both sides are thiazolinyl (n is more than 1), or can be also R 5and R 6in a side be thiazolinyl (n is more than 2).Being explained, can be R 5and R 6the compound that both sides are thiazolinyl and R 5and R 6in a side be thiazolinyl compound is mixed in together.Each R 5can be identical or different.In addition, each R 6can be identical or different.
As thiazolinyl, can enumerate vinyl, allyl group, propenyl, butenyl, pentenyl, hexenyl, heptenyl, octenyl etc., wherein, vinyl particularly preferably.
R 5and R 6in the alkyl that is carbon number 1～12 of the functional group except thiazolinyl, for example can enumerate, methyl, ethyl, propyl group, butyl, amyl group, hexyl, octyl group etc., be preferably methyl.As R 7and R 8in functional group except thiazolinyl, can enumerate and R 5and R 6identical alkyl, silanol group, hydrosilyl groups etc.
The aryl number that organopolysiloxane (A) is contained, the contained alkyl number with respect to organopolysiloxane (A), meter, be preferably 0.01～0.5 in molar ratio, is particularly preferably 0.05～0.3.By making the aryl number in this scope, can so that, when being coated on base material by remover combination, in the peeling agent layer obtained, organopolysiloxane (A) is present in the base material side of peeling agent layer more than organopolysiloxane (B), think and can obtain effect described later by such structure.
In addition, the thiazolinyl number that organopolysiloxane (A) is contained, the contained alkyl number with respect to organopolysiloxane (A), meter, be preferably 0.005～0.1 in molar ratio, is particularly preferably 0.01～0.05.By the thiazolinyl number is had more than 2 in 1 molecule, preferably, in above-mentioned scope, can make it be formed with the high crosslinking structure of cross-linking density that helps the aftermentioned effect.
The matter average molecular weight of organopolysiloxane (A) is necessary for 100000～800000, is preferably 150000～600000, is particularly preferably 200000～380000.Be explained, the matter average molecular weight in this specification sheets is the value by polystyrene conversion that adopts gel permeation chromatography (GPC) method to measure.
If the matter average molecular weight of organopolysiloxane (A) is less than 100000, when being coated on base material by remover combination, can filming and shrink etc., the coating variation, be difficult to obtain uniform condition of surface.In addition, if the matter average molecular weight of organopolysiloxane (A) surpasses 800000, the viscosity rise of remover combination, be difficult to be dissolved in diluting solvent.
On the other hand, organopolysiloxane (B) is the polymkeric substance by the silicon-containing compound of following general formula (b) expression.
[changing 2]
Figure BDA00003884017900061
In formula (b), p is the integer more than 1.In addition, R 9and R 10for the alkyl of carbon number 1～12, for example, methyl, ethyl, propyl group, butyl, amyl group, hexyl, octyl group etc., can not be aryl or thiazolinyl.R 9and R 10can be identical or different.R 9and R 10be preferably methyl.By making this organopolysiloxane (B) not containing aryl, when being coated on base material by remover combination, in the peeling agent layer obtained, organopolysiloxane (B) be present in more peeling agent layer than organopolysiloxane (A) with base material opposing face side (face side of peeling agent layer), think and can obtain effect described later by such structure.
In formula (b), R 11at least 1 be thiazolinyl, and R 12at least 1 be thiazolinyl.That is, organopolysiloxane (B) has thiazolinyl at two ends.As thiazolinyl, can enumerate vinyl, allyl group, propenyl, butenyl, pentenyl, hexenyl, heptenyl, octenyl etc., wherein, vinyl particularly preferably.R 12in thiazolinyl beyond functional group's alkyl that is carbon number 1～12, for example can enumerate, methyl, ethyl, propyl group, butyl, amyl group, hexyl, octyl group etc., be preferably methyl.Each R 11can be identical or different.In addition, each R 12can be identical or different.
By make organopolysiloxane (B) in its 1 molecule only two ends there is thiazolinyl, can be formed with the low crosslinking structure of cross-linking density that helps the aftermentioned effect.
The contained thiazolinyl number of organopolysiloxane (B) with respect to organopolysiloxane (B) contained alkyl number count and be preferably 0.0005～0.01 in molar ratio, be particularly preferably 0.001～0.005.
The matter average molecular weight of organopolysiloxane (B) is preferably 50000～800000, is particularly preferably 100000～700000, and more preferably 300000～500000.
If the matter average molecular weight of organopolysiloxane (B) is less than 50000, likely be difficult to be formed with the low crosslinking structure of cross-linking density that helps the aftermentioned effect.In addition, if the matter average molecular weight of organopolysiloxane (B) surpasses 800000, the viscosity rise of remover combination, likely be difficult to be dissolved in diluting solvent.And, the solidified nature variation of remover combination, siloxanes also likely increases to the transfer amount of ceramic green.
Organopolysiloxane (A) is 40～98 quality % with respect to the solids component ratio of the total amount of organopolysiloxane (A) and organopolysiloxane (B), is preferably 50～95 quality %.If the solids component ratio of organopolysiloxane (A) is outside above-mentioned scope, even the coating of ceramic size is good, the separability of ceramic green also can significantly descend.
As linking agent (C), so long as can make organopolysiloxane (A) and/or organopolysiloxane (B) that crosslinked linking agent occurs, just be not particularly limited, be preferably organopolysiloxane (A) and organopolysiloxane (B) in addition, there are at least 2 organopolysiloxane that are bonded to the hydrogen atom on Siliciumatom in 1 molecule.As this organopolysiloxane, such as the hydrogenated methyl polysiloxane of the dimethyl siloxane of the dimethyl siloxane that can enumerate dimethyl hydrogenation siloxy-end-blocking-hydrogenated methyl silicone copolymers, trimethylsiloxy end-blocking-hydrogenated methyl silicone copolymers, trimethylsiloxy end-blocking, poly-(silicon hydride sesquioxyalkane) etc.
Matter average molecular weight as the organopolysiloxane of linking agent (C) is preferably 100～5000, is particularly preferably 500～2000.
The content of the linking agent in the remover combination of present embodiment (C) is preferably and can makes: the number of the bridging property functional groups such as hydrosilyl groups that linking agent (C) is contained is calculated in molar ratio as 1.0～5.0 required amounts with respect to the number of organopolysiloxane (A) and the contained thiazolinyl of organopolysiloxane (B), and being particularly preferably and can making this mol ratio is 1.5～3.0 required amounts.
Linking agent (C), owing to making organopolysiloxane (A) and/or organopolysiloxane (B) crosslinked, therefore can be given stable separability to the peeling agent layer obtained.
As catalyzer (D), as long as can make the remover combination of present embodiment solidify, just be not particularly limited, wherein, the preferred platinum group metal based compound.As the platinum metals based compound, for example can enumerate microgranular platinum, the olefin(e)complex that is adsorbed on microgranular platinum on carbon powder carrier, Platinic chloride, pure modification Platinic chloride, Platinic chloride, palladium, rhodium etc.By making remover combination contain this catalyzer (D), can make the curing reaction of this remover combination more effectively carry out.
The content of catalyzer in the remover combination of present embodiment (D), with respect to the total amount of catalyzer (D) composition in addition, be preferably 1～1000ppm left and right.
The remover combination of present embodiment, except mentioned component (A)～(D), can also contain reaction suppressor, adaptation rising agent etc.
By making remover combination described above contain according to the specified ratio above-mentioned organopolysiloxane (A) and organopolysiloxane (B), the coating that can form ceramic size separability good, ceramic green simultaneously is very good peeling agent layer also.Therefore, so long as the peeling agent layer formed by the remover combination of present embodiment, at the surface coated ceramic size of peeling agent layer and while making it dry, shrink and the thickness thickening (being that shrink so-called end) of this coating end and suppress the phenomenons such as generation pin hole, crawling the coating end that can suppress ceramic size.In addition, even during moulding, also can, under the condition of unfavorable conditions such as not cracking, break, with low-down peeling force, ceramic green be stripped down from peeling agent layer on this peeling agent layer at the ceramic green of the film like that intensity is low.Although its principle is not yet clear, but as mentioned above, supposition be because, when organopolysiloxane (A) has aryl and organopolysiloxane (B) only when two ends have thiazolinyl, organopolysiloxane (A) is present in the base material side of peeling agent layer more, and organopolysiloxane (B) is present in the top layer side of peeling agent layer more, result, think the effect of end contraction, pin hole, crawling etc. of can being inhibited.。
(ceramic green moulding stripping film)
The ceramic green of present embodiment is stripping film (following sometimes referred to as " stripping film ") for moulding, base material and the peeling agent layer that forms on the one side of base material, consists of.
As base material, be not particularly limited, can be from select aptly any base material known base material in the past.As this base material, for example can enumerate, by polyesters such as polyethylene terephthalate or PENs; The polyolefine such as polypropylene or polymethylpentene; The film that the plastics such as polycarbonate, polyvinyl acetate form, base material can be individual layer, can be also the identical or different multilayer more than 2 layers of kind.Wherein, preferred polyester film, polyethylene terephthalate film particularly preferably, the further preferred polyethylene terephthalate film of two-way stretch.Due to the polyethylene terephthalate film, adding man-hour, be difficult for producing dust etc. in while using etc., therefore, can effectively prevent bad etc. such as the ceramic size coating caused by dust etc.And then, by the polyethylene terephthalate film is carried out to antistatic treatment, can improve the effect that prevents from being coated with bad grade.
In addition, in this base material, in order to improve and the adaptation that is arranged at its surperficial peeling agent layer, can as required, to its single face or two sides, implement to utilize the surface treatment of oxidation style or concavo-convexization method etc. or undercoat to process.As above-mentioned oxidation style, such as enumerating Corona discharge Treatment, plasma discharge processing, chromium oxide treatment (wet type), flame treating, hot blast processing, ozonize, uviolizing processing etc., in addition, as concavo-convexization method, such as enumerating sand-blast, spraying plating facture etc.These surface preparations can the suitable selection according to the kind of base material film, generally speaking, from aspects such as effect and operability, considers, preferably adopts the Corona discharge Treatment method.
The thickness of base material is generally 10～300 μ m and gets final product, and is preferably 15～200 μ m, is particularly preferably 20～125 μ m.
Peeling agent layer in present embodiment is formed by above-mentioned remover combination.Specifically, peeling agent layer is by the coating fluid that coating contains remover combination and organic solvent as required on the one side of base material, and then drying is solidified to form it.As coating process, such as using intaglio plate coating method, excellent painting method, spraying method, spin-coating method, spread coating, rolling method, die coating method etc.
Be not particularly limited as above-mentioned organic solvent, can use various organic solvents.Such as using the hydrocarbon compounds such as toluene, hexane, heptane, and acetone, ethyl acetate, butanone, methyl iso-butyl ketone (MIBK) and their mixture etc.
Coated as mentioned above remover combination is preferably carried out to thermofixation.Now, Heating temperature is preferably 90～140 ℃, is preferably heat-up time about 10～120 seconds.
The thickness of peeling agent layer is not particularly limited, and is preferably 0.01～3 μ m, more preferably 0.03～1 μ m.If the thickness deficiency of peeling agent layer 0.01 μ m,, due to the difference of the material that forms peeling agent layer etc., can not give full play to the function as peeling agent layer sometimes.On the other hand, if the thickness of peeling agent layer surpasses 3 μ m,, when stripping film is coiled into to the cylinder shape, often stick together, at the extraction film, sometimes produce unfavorable condition.
For using stripping film described above, adopt slit die coating method or scraper plate coating method etc., by the surface coated ceramic size at peeling agent layer and make its drying, by the ceramic green moulding.Now, the stripping film of present embodiment can suppress the generation of the coating end contraction of ceramic size and the thickness thickening of this coating end (being that shrink so-called end), and can suppress the generation of pin hole or crawling.On the other hand, even at the ceramic green of the film like that intensity is low in the situation that moulding on peeling agent layer, the unfavorable condition such as can not crack, break yet, as long as apply low peeling force, particularly be less than the peeling force of 13mN/100mm, just ceramic green can be stripped down from peeling agent layer.Like this, while adopting the stripping film of present embodiment, the coating excellence of ceramic size, simultaneously, the separability of ceramic green is also excellent.
Embodiment described above is in order more easily to understand the present invention, rather than in order to limit scope of the present invention.Therefore, in above-mentioned embodiment, disclosed each key element is equivalent to also comprise whole design variant and the Equivalent that belongs to the technology of the present invention category.
For example, on base material 1 and the surface peeling agent layer opposition side or between base material 1 and peeling agent layer, other layers such as antistatic layer can also be set.
Embodiment
Below, wait and be described more specifically the present invention with embodiment, but scope of the present invention is not limited to these embodiment etc.
(embodiment 1)
2 above vinyl will be there are in 1 molecule, and not containing the part of vinyl by organopolysiloxane (A) 95 mass parts that dimethyl siloxane-the diphenyl siloxane multipolymer forms, not containing aryl, and in 1 molecule only two ends there is vinyl, the organopolysiloxane that other functional groups are methyl (B) 5 mass parts are mixed, after the linking agent (C) that interpolation consists of the hydrogenated methyl polysiloxane of trimethylsiloxy end-blocking, the organic solvent diluting that is principal constituent in order to toluene, the coating fluid of the remover combination that the preparation solid component concentration is 1.5 quality %.Be explained, organopolysiloxane (A) is shown in table 1 with respect to the solids component ratio (quality %) of the total amount of organopolysiloxane (A) and organopolysiloxane (B).
Herein, the matter average molecular weight of organopolysiloxane (A) is 360000, the contained phenyl number (number of contained methyl number with respect to organopolysiloxane (A)) of organopolysiloxane (A) is calculated in molar ratio as 0.125, and the contained vinyl number (number of contained methyl number with respect to organopolysiloxane (A)) of organopolysiloxane (A) is calculated in molar ratio as 0.025.
In addition, the matter average molecular weight of organopolysiloxane (B) is 440000, and the contained vinyl number (number of contained methyl number with respect to organopolysiloxane (B)) of organopolysiloxane (B) is calculated in molar ratio as 0.0024.
On the other hand, the matter average molecular weight of linking agent (C) is 1000, and the content of the linking agent in remover combination (C) is for can make the contained hydrosilyl groups number of linking agent (C) be calculated in molar ratio as 1.91 required amounts with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B).
Press the solids component ratio, add platinum group catalyst (chemical industry society of SHIN-ETSU HANTOTAI system in above-mentioned coating fluid 100 mass parts, PL-50T) 7 mass parts, adopt Meyer rod coating method, the coating fluid obtained is coated on to polyester film (resin society of the Mitsubishi system as the two-way stretch of base material equably, ダ イ ア ホ イ Le T-100, thickness: 38 μ m) upper, so that dried thickness is 0.1 μ m.Then, with hot air circulation type drying machine, 135 ℃ of lower heat treated 60 seconds, the silicone resin stripper is solidified, obtain closing at layers on substrates the stripping film of peeling agent layer.
(embodiment 2)
Organopolysiloxane (A) 90 mass parts and organopolysiloxane (B) 10 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 1.91, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(embodiment 3)
Organopolysiloxane (A) 70 mass parts and organopolysiloxane (B) 30 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 1.95, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(embodiment 4)
Organopolysiloxane (A) 50 mass parts and organopolysiloxane (B) 50 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 2.00, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 1)
Do not use organopolysiloxane (B), only use organopolysiloxane (A) 100 mass parts, add linking agent (C), make the contained hydrosilyl groups number of linking agent (C) with respect to organopolysiloxane (A) contained vinyl number count in molar ratio, be 1.90, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 2)
Organopolysiloxane (A) 99 mass parts and organopolysiloxane (B) 1 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 1.90, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 3)
Organopolysiloxane (A) 30 mass parts and organopolysiloxane (B) 70 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 2.11, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 4)
Organopolysiloxane (A) 10 mass parts and organopolysiloxane (B) 90 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A) and the contained vinyl number of organopolysiloxane (B), be 2.42, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 5)
Do not use organopolysiloxane (A), only use organopolysiloxane (B) 100 mass parts, add linking agent (C), make the contained hydrosilyl groups number of linking agent (C) with respect to organopolysiloxane (B) contained vinyl number count in molar ratio, be 3.00, in addition, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 6)
To there are 2 above vinyl in 1 molecule and do not mixed by organopolysiloxane (A ') 95 mass parts of dimethyl siloxane-methylphenyl siloxane multipolymer (on a side chain of siloxane backbone, thering is aryl) formation and organopolysiloxane (B) 5 mass parts of embodiment 1 use containing the part of vinyl, after the linking agent (C) that interpolation consists of the hydrogenated methyl polysiloxane of trimethylsiloxy end-blocking, the organic solvent diluting that is principal constituent in order to toluene, the coating fluid of the remover combination that the preparation solid component concentration is 1.5 quality %.Be explained, organopolysiloxane (A ') is shown in table 1 with respect to the solids component ratio (quality %) of the total amount of organopolysiloxane (A ') and organopolysiloxane (B).
Herein, the matter average molecular weight of organopolysiloxane (A ') is 390000, the contained phenyl number (number of contained methyl number with respect to organopolysiloxane (A ')) of organopolysiloxane (A ') is calculated in molar ratio as 0.012, and the contained vinyl number (number of contained methyl number with respect to organopolysiloxane (A ')) of organopolysiloxane (A ') is calculated in molar ratio as 0.019.
In addition, the content of the linking agent in remover combination (C), be calculated in molar ratio as 2.53 required amounts for making the contained hydrosilyl groups number of linking agent (C) with respect to organopolysiloxane (A ') and the contained vinyl number of organopolysiloxane (B).
Except using above-mentioned coating fluid, operation preparation coating fluid, make stripping film similarly to Example 1.
(comparative example 7)
Organopolysiloxane (A ') 50 mass parts and organopolysiloxane (B) 50 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A ') and the contained vinyl number of organopolysiloxane (B), be 2.57, in addition, with the same operation preparation of comparative example 6 coating fluid, make stripping film.
(comparative example 8)
Do not use organopolysiloxane (B), only use organopolysiloxane (A ') 100 mass parts, add linking agent (C), make the contained hydrosilyl groups number of linking agent (C) with respect to organopolysiloxane (A ') contained vinyl number count in molar ratio, be 2.53, in addition, with the same operation preparation of comparative example 6 coating fluid, make stripping film.
(comparative example 9)
Organopolysiloxane (A ') 10 mass parts and organopolysiloxane (B) 90 mass parts are mixed, add linking agent (C), the contained hydrosilyl groups number of linking agent (C) is counted in molar ratio with respect to organopolysiloxane (A ') and the contained vinyl number of organopolysiloxane (B), be 2.76, in addition, with the same operation preparation of comparative example 6 coating fluid, make stripping film.
(test example 1) (evaluation of ceramic size coating)
To barium titanate (BaTiO 3; Sakai chemical industry society system, BT-03) 100 mass parts, polyvinyl butyral (ponding chemical industry society system, エ ス レ ッ Network BK BM-2) 10 mass parts and dioctyl phthalate (DOP) (Northeast chemistry society system, 1 grade of dioctyl phthalate (DOP) assurance purity) add mixed solution (mass ratio 6:4) 115 mass parts of toluene and ethanol in 5 mass parts, by its blending dispersion, prepare ceramic size with ball mill.
The stripping film of preserving at normal temperatures 48 hours in embodiment and comparative example after manufacturing is (wide: on peeling agent layer surface 300mm), use die type coating machine (wide 250mm) evenly to be coated with above-mentioned ceramic size, making dried thickness is 3 μ m, then, make its dry 1 minute with drying machine under 80 ℃.Manufacture thus the stripping film volume 300m with ceramic green.
To the volume of the stripping film with the ceramic green 300m obtained, range estimation confirms whether to occur in the width end end is shunk.Its result, be evaluated as zero by the sample that does not occur to shrink end, the sample that occurs to shrink end is evaluated as *.And then range estimation is confirmed whether to occur small contractions of filming of the ceramic size that can be found out by naked eyes, so-called pin hole or due to the caused crawling of coating thickness inequality of ceramic size.The pin hole that do not occur with the naked eye to find out and the sample of crawling are evaluated as to zero, the sample that pin hole or crawling occur is evaluated as *.The results are shown in table 1.
(test example 2) (evaluation of the separability of ceramic green)
The stripping film with ceramic green that will obtain equally with test example 1 is in the atmosphere of 23 ℃ of room temperatures, humidity 50% after standing 24 hours, be cut into the size of 100mm * 100mm, paste on one side at it from the ceramic green face side and count the acrylic adhesive tape that length is 100mm (day Dong electricity Gong She system, 31B adhesive tape).This sample is fixed on dull and stereotyped upper, the stripping film face side is contacted with this flat board, using the end avris that is pasted with acrylic adhesive tape as downside, be arranged on electronic stripping tester (society of Shimadzu Seisakusho Ltd. system, AG-IS 500N) according to 45 ° of inclinations.Then, from the limit of the end that is pasted with acrylic adhesive tape, stripping film is stripped down from ceramic green, the acrylic adhesive tape side is arranged on the fixture of electronic stripping tester.Under this state, with the peeling rate of 200mm/min, acrylic adhesive tape vertically is pulled upwardly, measure the peeling force (mN/100mm) while from stripping film, ceramic green being peeled off.The results are shown in table 1.
In addition, owing to as the ceramic green moulding, by the preferred peeling force of stripping film, being less than 13mN/100mm, the sample that therefore peeling force recorded is less than to 13mN/100mm is evaluated as zero, by peeling force be sample more than 13mN/100mm be evaluated as *.The results are shown in table 1.
Figure BDA00003884017900161
From the result shown in table 1, find out, the stripping film obtained in embodiment 1～4, the coating excellence of its ceramic size, as long as and apply low peeling force and just ceramic green can be peeled off, the separability of ceramic green is also excellent.On the other hand, the stripping film obtained in comparative example 1～9, although the coating excellence of its ceramic size, only applying high peeling force could peel off ceramic green, the separability of ceramic green is poor.
Industrial applicability
Remover combination of the present invention is applicable to form the peeling agent layer of ceramic green moulding with stripping film.In addition, the separability that ceramic green moulding of the present invention can be used as the excellent and ceramic green of the coating of ceramic size with stripping film is very excellent stripping film also.

Claims (9)

1. remover combination, is characterized in that, contains:
Organopolysiloxane (A), have in its 1 molecule on two side chains of at least 2 thiazolinyls and at least 1 Siliciumatom in siloxane backbone and have aryl, and
Organopolysiloxane (B), its do not there is aryl and in 1 molecule only two ends there is thiazolinyl;
Described organopolysiloxane (A) is 40～98 quality % with respect to the solids component ratio of the total amount of described organopolysiloxane (A) and described organopolysiloxane (B),
The matter average molecular weight of described organopolysiloxane (A) is 100000～800000.
2. remover combination claimed in claim 1, is characterized in that, the matter average molecular weight of described organopolysiloxane (B) is 50000～800000.
3. the described remover combination of claim 1 or 2, is characterized in that, also contains the platinum metals based compound as catalyzer.
4. the described remover combination of claim 1～3 any one, is characterized in that, also contains linking agent (C).
5. the described remover combination of claim 1～4 any one, is characterized in that, the thiazolinyl number alkyl number contained with respect to described organopolysiloxane (A) that described organopolysiloxane (A) is contained, and meter, be 0.005～0.1 in molar ratio.
6. the described remover combination of claim 1～5 any one, is characterized in that, the aryl number alkyl number contained with respect to described organopolysiloxane (A) that described organopolysiloxane (A) is contained, and meter, be 0.01～0.5 in molar ratio.
7. the described remover combination of claim 1～6 any one, is characterized in that, the thiazolinyl number alkyl number contained with respect to described organopolysiloxane (B) that described organopolysiloxane (B) is contained, and meter, be 0.0005～0.01 in molar ratio.
8. the described remover combination of claim 4～7 any one, it is characterized in that, the content of the linking agent in described remover combination (C) is for to make the contained hydrosilyl groups number of linking agent (C) be calculated in molar ratio as 1.0～5.0 required amounts with respect to organopolysiloxane (A) and the contained thiazolinyl number of organopolysiloxane (B).
9. ceramic green moulding stripping film, the peeling agent layer that it possesses base material and at least forms on the one side of described base material, is characterized in that, described peeling agent layer is that right to use requires the described remover combination of 1～8 any one to form.
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