WO2003099556A1 - Film detachable - Google Patents

Film detachable Download PDF

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Publication number
WO2003099556A1
WO2003099556A1 PCT/JP2003/006473 JP0306473W WO03099556A1 WO 2003099556 A1 WO2003099556 A1 WO 2003099556A1 JP 0306473 W JP0306473 W JP 0306473W WO 03099556 A1 WO03099556 A1 WO 03099556A1
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WO
WIPO (PCT)
Prior art keywords
film
release
layer
silicone
release layer
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Application number
PCT/JP2003/006473
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English (en)
Japanese (ja)
Inventor
Masanori Nishiyama
Original Assignee
Teijin Dupont Films Japan Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Teijin Dupont Films Japan Limited filed Critical Teijin Dupont Films Japan Limited
Priority to AU2003242434A priority Critical patent/AU2003242434A1/en
Priority to KR1020047010442A priority patent/KR100919440B1/ko
Priority to JP2004507063A priority patent/JP3950462B2/ja
Publication of WO2003099556A1 publication Critical patent/WO2003099556A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents

Definitions

  • the present invention relates to a release film. More specifically, the present invention relates to a release film having excellent surface characteristics in which surface irregularities are not transferred to a molded sheet, and having excellent workability and release properties.
  • Conventional field
  • Release films are used, for example, for molding resin sheets, for releasing adhesives, for medical use, and for manufacturing electrical and electronic components.
  • a molded article such as a resin sheet molded from a release film
  • flattening the surface of the molded article is an important issue. It is no exaggeration to say that the quality of a molded product formed from a film depends on the accuracy and quality of its surface, that is, the accuracy and quality of the surface of the release film.
  • the release film itself is formed by providing a polyester film with a resin layer having a release property, for example, a silicone resin layer.
  • a resin layer having a release property for example, a silicone resin layer.
  • particles are blended in a polyester film to improve processability, for example, slipperiness and winding characteristics, but in general, handling is improved by adding particles to the film, but the surface of the film is improved. Coarse. If the mixing of the particles is stopped to avoid this and create a flat surface, the resulting film will have extremely poor slipperiness and air bleeding properties, and will have seams during processing and will be rolled up. Will not be.
  • the silicone layer covers the protrusions on the surface of the polyester film, thereby further reducing the processability.
  • release films used as process materials for electronic components have particularly high requirements for surface characteristics.
  • a ceramics slurry in which ceramic powder and a binder agent are dispersed in a liquid medium on a release film and use a very thin sheet of 3 m or less. Create The thinner the sheet, the higher the demands on the surface properties of the release film because the surface irregularities of the release film directly increase the defective rate of the molded sheet.
  • the release film surface is required to have a smooth surface by making the molded sheet thinner. Disclosure of the invention
  • An object of the present invention is to solve the drawbacks of the prior art, and to have excellent surface characteristics in which large irregularities on the surface of the release film are not transferred to the molding sheet, as well as excellent workability and good release characteristics.
  • An object of the present invention is to provide a release film.
  • a release film characterized by comprising (hereinafter, referred to as a first release film of the present invention).
  • the above objects and advantages of the present invention are: (a ') a polyester film having a surface having a centerline average roughness Ra of 5 nm or less and a ten-point average roughness Rz of 30 nm or less; and
  • d is the average particle size of the inert particles (nm) and t is the thickness of the silicon release layer (nm)
  • a release film (hereinafter, referred to as a second release film of the present invention) comprising a silicone release layer having a thickness of 300 nm or less and containing inert particles satisfying the following.
  • the first release film comprises a polyester film (a) and a silicone release layer (b) formed on its surface.
  • polyester for the polyester film (a) a polyester containing an aromatic dicarboxylic acid as a main acid component and an aliphatic glycol as a main glycol component is preferably used.
  • the dark polyester is substantially linear and has film formability, especially film formability by melt molding.
  • Aromatic dicarboxylic acids include, for example, terephthalic acid, naphthalenedicarboxylic acid, isophthalic acid, diphenoxyethane dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl terdicarboxylic acid, diphenyl sulfone dicarboxylic acid, diphenyl ketone dicarboxylic acid and Anthracene dicarboxylic acid can be mentioned.
  • aliphatic glycol examples include polymethylene glycol having 2 to 10 carbon atoms such as ethylene glycol, trimethylene glycol, tetramethylene glycol, pentamethylene glycol, hexamethylene glycol and decamethylene glycol, and cyclohexane.
  • Alicyclic diols such as xanthyl alcohol can be mentioned.
  • polyester alkylene terephthalate or a Those containing ruchilennaphthalate as a main component are preferably used.
  • polyethylene terephthalate or polyethylene-1,2,6-naphthalate is preferable.
  • the polyethylene terephthalate includes copolymers wherein, for example, at least 80 mole% of the total dicarboxylic acid component is terephthalic acid and at least 80 mole% of the total glycol component is ethylene glycol. It is.
  • the polyethylene mono-2,6-naphthalate contains, for example, at least 80 mol% of the total dicarboxylic acid component is 2,6-naphthalenedicarboxylic acid and at least 80 mol% of the total dalicol component is e.g. It should be understood that copolymers that are ethylene glycol are included.
  • terephthalic acid or another dicarboxylic acid component different from 2,6-naphthalenedicarboxylic acid.
  • dicarboxylic acid components include, for example, aromatic dicarboxylic acids as described above; for example, alicyclic dicarboxylic acids such as adipic acid and sebacic acid, and alicyclic dicarboxylic acids such as cyclohexane-1,4-dicarponic acid.
  • 20 mol% or less of the total glycol component can be another glycol component different from ethylene glycol.
  • Such other dalicol components are, for example, dalicol as described above; for example, an aromatic diol such as hydroquinone, resorcin, 2,2-bis (4-hydroxyphenyl) propane; and a fat having an aromatic ring such as 1,4-dihydroxydimethylbenzene.
  • Group diols or polyalkylene glycols (polyoxyalkylene glycols) such as polyethylene diol, polypropylene glycol and polytetramethylene glycol.
  • a component derived from an oxycarboxylic acid such as an aromatic oxyacid such as hydroxybenzoic acid or an aliphatic oxyacid such as ⁇ -hydroxycabronic acid may be used as a dicarboxylic acid component or an oxycarboxylic acid component.
  • an oxycarboxylic acid such as an aromatic oxyacid such as hydroxybenzoic acid or an aliphatic oxyacid such as ⁇ -hydroxycabronic acid
  • polyesters may contain tri- or higher functional polycarboxylic acids or polyhydroxy compounds in amounts that are substantially linear, for example, up to 2 mole percent, based on the total acid component.
  • Substances for example, those obtained by copolymerizing trimellitic acid and pentaerythritol.
  • the polyester is known per se and can be produced by a method known per se.
  • those having an intrinsic viscosity of 0.4 to 0.9 measured at 35 ° C. as a solution in phenol with O-cloth are preferable.
  • the polyester film (a) preferably contains inert particles.
  • the average particle size of the inert particles is preferably less than 1 m, more preferably 0.01 m or more and less than 1 m, more preferably 0.03 111 or more and less than 1111.
  • the inert particles may be either organic particles or inorganic particles, or may be mixed particles of organic particles and inorganic particles.
  • the ratio of the major axis to the minor axis (major axis / minor axis) of the inert particles is preferably from 1.0 to 1.2. By blending these inert particles, appropriate irregularities can be formed on the film surface.
  • inert particles include inorganic particles such as calcium carbonate, kaolin, gen oxide, barium sulfate, titanium oxide, oxidized alumina; crosslinked polystyrene, crosslinked silicone resin particles, crosslinked acrylic resin particles, crosslinked.
  • examples include organic resin particles such as polystyrene particles and particles in which an inorganic material and an organic material take the form of a shell core structure.
  • inert particles can be used alone or in combination of two or more, for example, three or four.
  • the amount of the inert particles to be added is 0.01 to 0.3% by weight based on the polyester.
  • the polyester film (a) preferably has a thickness of 0.1 to 30 times the average particle size of the inert particles contained therein.
  • the thickness of the polyester layer is less than 0.1 times the average particle size, the contained inert particles are likely to fall off, which is not preferable. On the other hand, if the average particle diameter exceeds 30 times, the inert particles contained in the polyester layer are liable to overlap, and irregularities are easily formed on the surface of the film.
  • the polyester film (a) has a center line average roughness Ra of 15 nm or less.
  • the surface has a ten-point average roughness Rz of 30 to 500 nm. If Ra exceeds 15 nm, shape transfer will occur on the surface of the molded body.
  • Ra is preferably from 1 to 13 nm.
  • Rz is preferably between 50 and 300 nm.
  • the thickness of the polyester film (a) is preferably from 10 to 100 m, more preferably from 25 to 50 m.
  • the first release film of the present invention is obtained by forming a silicone release layer (b) described below on the surface having the above Ra and Rz of the polyester film (a). b) Another polyester layer may be provided on the surface opposite to the surface on which is formed.
  • Such another polyester layer can be formed as a laminated film together with the polyester film (a).
  • the laminated film can be composed of at least two layers, and is preferably manufactured by co-extrusion.
  • the polyester constituting the layer may be the same or different, but the same is preferred.
  • a polyester film (a) layer / layer B a polyester film (a) layer ZB layer Z a polyester film (a) layer or a polyester film (a )
  • a laminated structure such as layer / layer B / layer C can be adopted.
  • the outermost layer on the opposite side of the polyester film (a) layer forming the release layer (b), for example, the B layer and the C layer in the above example, contain inert particles.
  • the inert particles preferably have an average particle size of from 0.1 to 1.0 m.
  • the laminated film preferably has a total thickness of 10 to 100 m, more preferably 25 to 50 m, as a total thickness including the polyester film (a) layer.
  • the polyester film (a) and the laminated polyester film itself can be obtained by a conventionally known method or a method accumulated in the art.
  • the polyester is melted at a temperature of melting point (Tm: ° C) or (Tm + 70) ° C and coextruded to obtain an intrinsic viscosity of 0.4 to 0.8 dLZ g.
  • the unstretched film is (Tg-10) to (Tg + 70) in the uniaxial direction (longitudinal direction or horizontal direction). Stretching at a temperature of C (Tg: glass transition temperature of polyester) of 2.5 times or more, preferably 3 times or more, and then Tg to (Tg + 70) ° in a direction perpendicular to the above stretching direction. The film is stretched at a temperature of C at a ratio of at least 2.5 times, preferably at least 3 times. Further, if necessary, the film may be stretched again in the machine direction and / or the cross direction.
  • the total stretching ratio is preferably 9 times or more, more preferably 12 to 35 times, particularly preferably 15 to 25 times as the area stretching ratio.
  • the biaxially oriented film can be heat-set at a temperature of (Tg + 70) ° C to (Tm-10) ° C (where Tm is the melting point of the polyester), for example, 180 to 250 °. C is preferred.
  • the heat setting time is preferably 1 to 60 seconds.
  • the melting point and the glass transition temperature are the melting point and the glass transition temperature of the polyester having a higher melting point and a higher glass transition temperature.
  • the first release film of the present invention is obtained by forming a silicone release layer (b) on the surface of a polyester film (a).
  • the silicone release layer (b) may be formed on one side or both sides of the polyester film (a).
  • the release layer is preferably made of polydimethylsiloxane or a mixture containing the same as a main component and the following component (1) or (2), or modified by the following (3) or (4). It is composed of polydimethylsiloxane or the addition type silicone resin of the following (5).
  • a silicone resin having the following D unit, T unit and Z or Q unit structure in a polydimethylsiloxane polymer This silicone resin is blended with polydimethylsiloxane to increase the surface tension by adjusting the concentration of methyl groups in the release layer. Can be made.
  • the silicone resin is preferably mixed at a solid content of 10 to 60% by weight. If the resin content is less than 10% by weight, wettability may be poor when forming a molded sheet, and the resin sheet may repel. On the other hand, if it is more than 60% by weight, the peeling force is too high, and the molded body cannot be peeled.
  • R represents an alkyl group, preferably a methyl group, or an aromatic hydrocarbon group, preferably a phenyl group.
  • silica filler By blending a silica filler in the polydimethylsiloxane polymer, the concentration of one Si SH group in the release layer can be adjusted to be higher.
  • the silica filter preferably has an average particle size of 1 m or less. If the average particle size exceeds 1 m, the haze of the film will increase, which may hinder the use of the film in applications requiring transparency, or may cause separation when the film is run in the processing process. It is not preferable because the mold layer may be scraped.
  • the mixing ratio of the silica filler is preferably from 0.01 to 1% by weight in terms of solid content.
  • the compounding ratio is less than 0.01% by weight, the slipperiness of the roll with the silicone surface deteriorates, and if it exceeds 1% by weight, it is not preferable because it may be shaved off the silica filler release layer and fall off.
  • the substitution ratio of the phenyl group is preferably 10 to 60 mol%. If the substitution ratio is less than 10 mol%, the molded layer tends to repel and may not be applied. If the substitution ratio is more than 60 mol%, the releasability between the release layer and various adhesives or various sheets may be poor. It is not preferable because there is.
  • polydimethylsiloxane polymer having a relatively high concentration of reactive groups such as silanol group and methoxy group with an organic shelf having a hydroxyl group in the molecule (eg, alkyd resin, polyester resin, acrylic resin)
  • a modified polydimethylsiloxane obtained by the reaction is preferably 10 to 30% by weight. If this ratio is less than 10% by weight, the releasability may be poor, and if it exceeds 30% by weight, silicone transfer occurs, which is not preferable.
  • An addition reaction type silicone resin for example, an addition reaction type silicone resin composed of polydimethylsiloxane having a vinyl group introduced therein and hydrogen silane.
  • the ratio of polydimethylsiloxane having a vinyl group to hydrogen silane is such that the vinyl group in polydimethylsiloxane is 1.0 to 2.0 per 1.0 mole of one SiH group in hydrogen silane. A molar ratio is preferred.
  • the silicone resin of the above (1) may be blended with the silicone resin.
  • the mixing ratio of the silicone resin is preferably not more than 60% by weight, more preferably 0.1 to 30% by weight, in terms of solid content, from the viewpoint of obtaining an appropriate peeling force.
  • the polydimethylsiloxane having a vinyl group may contain one SiAr 2 — and one SiAr (R) group in addition to the —Si (CH 3 ) 2 — group.
  • the Ar group is an aromatic hydrocarbon group, and is preferably a phenyl group.
  • the R group is an alkyl group, preferably a methyl group.
  • the polydimethylsiloxane having a pinyl group contains one —S i Ph (CH 3 ) group or _S i (Ph) 2 — group. From the viewpoint of suppressing the disorder of the molecular structure and securing an appropriate peeling force and sufficient hardness, these groups should be 0.5 mol or less with respect to 1 mol of one S i (CH 3 ) 2 — group. Is preferred.
  • Ph is a phenyl group.
  • the addition reaction type silicone resin may have a three-dimensional crosslinked structure, and the three-dimensional crosslinked structure can be obtained by reacting with a platinum catalyst.
  • a curing type using ultraviolet rays or a silicone type using an electron beam may be used as the type of curing silicone. It is important that the thickness of the silicone release layer is not more than 0.8 times the ten-point average roughness Rz of the surface of the polyester film (a) on which the silicone release layer is formed.
  • the silicone resin will enter the recesses of the slightly uneven portion due to the particles in the film, and as a result, the center line average roughness Ra and the ten-point average roughness R of the surface of the release layer will be obtained. z becomes low, resulting in poor handling properties in the process and problems due to blocking of the release layer (backside transfer).
  • the silicone release layer preferably contains inert particles having an average particle size of 5 to 8 O nm. By containing the inert particles, it is possible to obtain good handling characteristics in the process and an effect of improving blocking.
  • the first release film of the present invention preferably has a center line average roughness Ra of the exposed surface of the silicone release layer (b) of 15 nm or less and a ten-point average roughness Rz of 10 or less. 0 to 500 nm.
  • the sum of the center line average roughnesses Ra of both exposed surfaces is preferably 12 nm or more. If it is less than 12 nm, winding in a roll form and slippage with a pass roll are poor, resulting in poor handling of the process and blocking of the release layer (backside transfer).
  • additives can be added to the release layer as long as the object of the present invention is not hindered.
  • an ultraviolet absorber for example, an ultraviolet absorber, a pigment, an antifoaming agent, or an antistatic agent may be added as needed.
  • an adhesive layer is provided between the polyester film (a) and the release layer (b) in order to enhance the adhesion between the polyester film (a) and the release layer (b).
  • a silane coupling agent can be preferably used.
  • the silane coupling agent include those represented by the formula Y- S i- X 3.
  • Y represents a functional group represented by, for example, an amino group, an epoxy group, a vinyl group, a methacryl group, a mercapto group
  • X represents a hydrolyzable functional group represented by an alkoxy group.
  • the preferred thickness of the above-mentioned adhesive layer is about 0.05 to 1 m, particularly preferably 0.02 to 0.5 m.
  • the adhesion between the polyester film (a) and the release layer (b) becomes good, and the polyester film provided with the adhesive layer (b) is difficult to block, so that it is difficult to handle. It is hard to cause trouble.
  • the release layer can be provided, for example, by applying a coating liquid containing the components of the release layer to a film and drying by heating.
  • a coating liquid containing the components of the release layer
  • any known coating method can be applied.
  • Applicable coating methods include, for example, a mouth-coating method and a blade-coating method, but are not limited to these methods.
  • the heating and drying for forming the coating layer is preferably performed at 70 to 170 ° C. for 20 to 60 seconds.
  • the second release film comprises a polyester film (a ') and a release film (b') formed on the surface thereof.
  • polyester of the polyester film (a ') the same polyesters as those described for the first release film can be used.
  • the polyester film (a ′) may or may not contain inert particles. When it is contained, the same inert particles as those described for the polyester film (a) of the first release film can be used as the inert particles. These inert particles can be used alone or in combination of two or more. Such inert particles can be blended in an amount of 0.2% by weight or less based on the polyester.
  • the polyester film (a ′) has a surface having a center line average roughness (R a) of 5 nm or less and a ten-point average surface roughness (R z) of 3 O nm or less.
  • Ra is preferably 0-5 nm, and Rz is preferably 3-3 Onm.
  • the thickness of the polyester film (a ') is preferably from 10 to 100 m, and more preferably from 15 to 50 m.
  • the second release film of the present invention is obtained by forming a silicone release layer (b ′) described later on the surface having the above Ra and Rz of the polyester film (a ′).
  • Another polyester layer may be provided on the surface opposite to the surface on which the mold layer (b ') is formed.
  • Such another polyester layer can be formed as a laminated film together with the polyester film (a ').
  • the description given for the first release film is applied as it is by replacing the polyester film (a) with the polyester film (a ').
  • polyester film (a ′) and the laminated film can be manufactured in the same manner as the manufacturing method described for the first release film.
  • the second release film of the present invention is obtained by forming a silicone release layer (b ′) on the surface of a polyester film (a ′).
  • the silicone release layer ( ⁇ ′) may be formed on one side or both sides of the polyester film (a ′).
  • the release layer is preferably made of polydimethylsiloxane or a main component thereof, and the release layer of the first release film is blended with the component (1) or (2) described above. It comprises the modified polydimethylsiloxane of (3) or (4) or the addition-type silicone resin of (5). Of these, addition silicone resins are preferred.
  • the silicone release layer preferably has a hardness of 10 Omg fZ / xm 2 or more in microhardness measurement.
  • a hardness of 10 Omg fZ / xm 2 or more By setting the hardness to 10 Omg ⁇ / urn 2 or more, blocking can be prevented, the contact area when the film is wound into a roll can be sufficiently reduced, and peeling charge can be suppressed.
  • the thickness of the silicone release layer is 30 O nm or less, preferably 30 to 300 nm, and more preferably 50 to 200 nm. Above 300 nm, blocking tends to occur. If the thickness is less than 3 O nm, the peeling properties are not stable, and the peeling may be undesirably heavy.
  • the silicone release layer contains inert particles.
  • the inert particles impart many fine irregularities to the flat release layer surface. Since the unevenness is very fine, even if the shape of the unevenness is transferred from the release film to the molded sheet, it is not at a level that causes a problem. By adding the inert particles, transfer (blocking) to the back surface of the release layer is improved, and process suitability is improved.
  • the average particle size of the inert particles is preferably from 1 to 10 O nm, more preferably from 3 to 80 nm, particularly preferably from 3 to 50 nm. Further, the ratio of the major axis to the minor axis (major axis / minor axis) of the inactive particles is preferably 1.0 to 1.2.
  • Such inert particles may be either organic particles or inorganic particles, or may be mixed particles of organic particles and inorganic particles.
  • inert particles include inorganic particles such as calcium carbonate, kaolin, silicon oxide, barium sulfate, titanium oxide, oxidized alumina, magnesium oxide, and oxidized zirconium; crosslinked polystyrene resin particles, and crosslinked silica.
  • examples thereof include organic resin particles such as cone resin particles, crosslinked acrylic resin particles, and crosslinked polystyrene resin particles, and particles in which an inorganic material and an organic material have a shell core structure. In particular, in the case of fine particles, inorganic particles are preferred.
  • the mixing amount of the inert particles in the silicone release layer is preferably 0.1 to 25% by weight, and more preferably 0.3 to 5% by weight. If the addition amount is less than 0.1, slipperiness and blocking of the release layer occur, and the release characteristics of the release layer become unstable, which is not preferable. If it exceeds 25% by weight, the transparency is lowered, and aggregation is likely to occur, and coarse aggregates are generated, which is not preferable.
  • the silicone release layer has the following formula (1):
  • t (nm) is the thickness of the silicone release layer and d (nm) is inactive Average particle size of the conductive particles
  • the thickness t (nm) of the silicone release layer is less than 0.3 d, the inert particles will fall off and cause foreign matter, and if it exceeds 2.5 d, fine irregularities on the surface will be formed. This results in poor slipperiness, which results in poor handling, winding, and peeling electrification.
  • the projections on the exposed surface of the release layer satisfy the following expressions (2) and (3).
  • HD 5 is the number of protrusions with a height of 5 nm or more
  • HD 10 is the number of protrusions with a height of 10 nm or more.
  • HD5 is less than 500, slipperiness is poor, and handling, winding properties, and peeling electrification are poor. If HD10 exceeds 100, the shape is transferred to the surface of the molded sheet, which causes unevenness in the thickness of the sheet, which is not preferable.
  • HD5 and HD10 have the following relationships (2 ') and (3'):
  • the second release film of the present invention preferably has a center line average roughness Ra of 5 nm or less and a ten-point average roughness Rz of 30 nm or less on the exposed surface of the silicone release layer (b '). It is.
  • Additives may be added to the release layer in the present invention as long as the object of the present invention is not hindered.
  • the additive include an ultraviolet absorber, a pigment, an antifoaming agent, and an antistatic agent. Further, separately from the release layer, such an additive may be blended into a resin, and the resin may be applied to the surface of the polyester film (a ′).
  • the polyester film (a ') is subjected to corona treatment or polyester treatment to enhance the adhesion between the polyester film (a') and the release layer.
  • An adhesive layer may be provided between the release film (a ') and the release layer. It is preferable to use a silane coupling agent for the adhesive layer. The same silane coupling agent as that described for the first release film is used.
  • the preferable thickness of the above-mentioned adhesive layer is about 0.005 to 0.1 m, and particularly preferably 0.01 to 0.1 fim. When the thickness of the adhesive layer is in the above range, the adhesion between the polyester film (a ') and the release layer becomes good.
  • the release layer can be formed in the same manner as described for the first release film. It should be understood that items not described for the second release film are applied as they are for the first release film, or as they are obvious to those skilled in the art. Example
  • each characteristic value of the film was measured by the following method.
  • the center line average roughness (Ra) is a value defined by JIS-B0601, and was measured using a stylus type surface roughness meter (SURFCORDER SE-30C) of Kosaka Laboratory Co., Ltd.
  • the measurement conditions are as follows. (a) Stylus tip radius 2 ⁇ , ⁇
  • the center line average roughness (Ra) is measured by using a non-contact type surface roughness meter of WYK CORPORATION ON 2000-2.
  • the measurement conditions are as follows.
  • HD5 and HD10 For HD5 and HD10, from WYKO measurement data, the particle size and the distribution of protrusions were determined, and the number of protrusions at a particle size of 5 nm was set to HD5, and the number of protrusions at a particle size of 10 nm was set to HD10. .
  • the ten-point average roughness (Rz) is a value defined in JIS-B0601. In the present invention, it is obtained by using a stylus type surface roughness meter (SURFCORDER SE-30C) of Kosaka Seisakusho Co., Ltd. The difference between the average of the peaks up to the fifth peak and the average of the peaks of the valleys from the deepest to the fifth is shown for the part extracted by the reference length from the section curve of the night.
  • SURFCORDER SE-30C stylus type surface roughness meter
  • the ten-point average surface roughness Rz is measured using a non-contact surface roughness meter of WYKO CORPORATI ON NT-2000.
  • the measurement conditions are as follows.
  • Silicone film thickness measurement (Ts i (nm)) The cross section of the release film is cut with a microtome, and the thickness of the silicone layer is measured by observing the obtained sample with a TEM.
  • Two release films are stacked on a glass plate, the film on the lower side of the laminated film (the film in contact with the glass plate) is pulled on a constant speed roll, and the detector is fixed to one end of the upper film.
  • the film make a 200 gZ50 cm 2 load (P).
  • the film surface is worn with black paper, and the occurrence of white powder is visually observed and evaluated according to the following criteria. ⁇ : No white powder
  • the hardness of the release layer film was measured directly by using ENT-1100a manufactured by Elionix Inc. For the measurement, apply a load of 2 mgf with a triangular pyramid indenter, and calculate the hardness from the amount of deformation of the release layer.
  • dimethyl terephthalate and ethylene glycol were used, manganese acetate was used as a transesterification catalyst, antimony trioxide was used as a polymerization catalyst, phosphorous acid was used as a stabilizer, and the average particle diameter was 0 as inert particles of a lubricant.
  • 0.3% by weight of l ⁇ m acid sulfide was mixed and polymerized by a conventional method to obtain polyethylene terephthalate A having an intrinsic viscosity (orthochlorophenol, 35 ° C) of 0.62.
  • polyethylene terephthalate B was obtained in the same manner as in the above-mentioned poly (ethylene terephthalate) A, except that 0.4% by weight of m.
  • the film was stretched 6 times, quenched, then supplied to stainless steel overnight, and stretched 3.9 times horizontally at 105 ° C.
  • the obtained biaxially oriented film was heat-set at a temperature of 205 ° C for 5 seconds, and the thickness was 38 ⁇ (the thickness of the polyester layer on the side where the release layer was provided was 36 m, and the thickness of the polyester B layer on the opposite side.
  • a 2 m) heat-set biaxially oriented laminated polyester film was obtained.
  • a curable silicone (KS-847 (H) manufactured by Shin-Etsu Silicone Co., Ltd.) of the type that adds a platinum catalyst to a mixed solution of polydimethylsiloxane and dimethylhydrogensilane to cause an addition reaction
  • KS-847 (H) manufactured by Shin-Etsu Silicone Co., Ltd.
  • Isobutyl ketone and toluene were dissolved in a mixed solvent to prepare a solution with a total solid concentration of 3% by weight, and then applied by a conventional roll coating method to a dry film thickness of 55 ⁇ m.
  • a film was obtained. Heat drying for 30 seconds at 160 became.
  • Table 1 shows the properties of the release film.
  • Inert particles mixed with polyethylene terephthalate A in Example 1 were changed to 0.12% by weight of crosslinked silicone particles having an average particle size of 0.3 m, and polyethylene terephthalate B was mixed with inert particles. Changed to something that does not.
  • the polyethylene terephthalate rate was co-extruded with a multi-manifold die so as to have an A / BA configuration, and the extrusion amount was adjusted so that the thickness configuration was mZ34 / im / 2m.
  • the release layer had a thickness of 77 nm. Except for these, a release film was obtained in the same manner as in Example 1.
  • Example 2 Using only the polyethylene terephthalate A used in Example 2, a film of 38 m was produced, and the release layer had a thickness of 77 nm. Except for these, a release film was obtained in the same manner as in Example 2.
  • Dimethyl terephthalate and ethylene glycol are polymerized by a conventional method using manganese acetate as a transesterification catalyst, antimony trioxide as a polymerization catalyst, phosphorous acid as a stabilizer, and an intrinsic viscosity (orthochlorophenol, 3 5 ° C) was obtained.
  • 0.05% by weight of silicon oxide having an average particle size of 1.7 m is blended in polyethylene terephthalate as inert fine particles of lubricant to obtain a single layer film, and the thickness of the release layer is set to 98 nm. Except for the above, a release film was obtained in the same manner as in Example 1.
  • a release film was obtained in the same manner as in Comparative Example 1, except that the inert particles in Comparative Example 1 were replaced with particles having an average particle size of 0.1 m.
  • a release film was obtained in the same manner except that the silicone release film thickness was applied to the film obtained in Example 1 so as to be 20 O nm.
  • Table 1 Polyestenolefinolem release film
  • dimethyl terephthalate and ethylene glycol are polymerized by a conventional method using manganese acetate as a transesterification catalyst, antimony trioxide as a polymerization catalyst, and phosphorous acid as a stabilizer, and an intrinsic viscosity.
  • manganese acetate as a transesterification catalyst
  • antimony trioxide as a polymerization catalyst
  • phosphorous acid as a stabilizer
  • the pellets of polyethylene terephthalate were supplied to an extruder hopper after drying at 170 ° C for 3 hours, melted at a melting temperature of 280 to 300 ° C, and then extruded using an extrusion die. It was extruded on a rotary cooling drum having a surface finish of about 0.3 s and a surface temperature of 20 ° C. to obtain an unstretched film having a thickness of 540 m.
  • This unstretched film is preheated to 75 ° C and heated between the low-speed roll and the high-speed mouth by one IR heater with a surface temperature of 900 ° C from 15 mm above. Then, the film was uniaxially stretched 3.6 times in the machine direction, then quenched, and then supplied to the stenter, and stretched 3.9 times in the transverse direction at 105 ° C to obtain a biaxially oriented film. .
  • the biaxially oriented film was heat-set at a temperature of 205 ° C. for 5 seconds to obtain a heat-set biaxially oriented film having a thickness of 38 zm.
  • an aqueous solution of 3-glycidoxypropyltrimethoxysilane was applied by a kiss coat method as an anchor treatment of the silicone.
  • a curable silicone resin (Shin-Etsu Silicone Co., Ltd.) is used in which a platinum catalyst is added to a mixed solution of polydimethylsiloxane and dimethylhydrogensilane having a phenyl group content of 1.0 mol% or less and a platinum catalyst is added.
  • a platinum catalyst is added to a mixed solution of polydimethylsiloxane and dimethylhydrogensilane having a phenyl group content of 1.0 mol% or less and a platinum catalyst is added.
  • the polyethylene terephthalate pellets are supplied to an extruder hopper after drying at 170 for 3 hours, melted at a melting temperature of 280 to 300 ° C, and surface-finished for about 0.3 s using an extrusion die. Extruded on a rotating cooling drum at a temperature of 20 ° C, thickness 5
  • This unstretched film is preheated to 75 ° C, and heated vertically by a single IR heater with a surface temperature of 900 ° C from 15 mm above between the low speed roll and the high speed roll.
  • the film was uniaxially stretched twice, quenched and then supplied to a stenter, and stretched 3.9 times in the transverse direction at 105 ° C. to obtain a biaxially oriented film.
  • This biaxially oriented film was heat set at a temperature of 205 ° C for 5 seconds to obtain a heat fixed biaxially oriented film having a thickness of 38 zm.
  • an aqueous solution of 3-glycidoxypropyltrimethoxysilane was applied by a kiss coat method as a silicone anchor treatment.
  • a silicone resin (KS-774 manufactured by Shin-Etsu Silicone Co., Ltd.) of a type in which a platinum catalyst is added to a mixed solution of polydimethylsiloxane and dimethylhydrogensilane to cause an addition reaction, Dissolved in a mixed solvent of butyl ketone, isopropyl ketone and toluene, added 2% by weight of silicone oxide particles (R972 average particle size 3 Onm, manufactured by Nippon Air Gill Co., Ltd.) as inorganic particles, 2% by weight per silicone resin component.
  • silicone oxide particles R972 average particle size 3 Onm, manufactured by Nippon Air Gill Co., Ltd.
  • a solution having a concentration of 1% by weight was prepared, and applied by a conventional roll coating method so that the dry film thickness became 45 nm, to obtain a release film.
  • Heat drying by the roll coating method was performed at 150 ° C for 20 seconds. Table 2 shows the properties of this release film.
  • a release film was obtained in the same manner as in Example 4, except that no inorganic particles were added to the silicone release layer of Example 1.
  • Table 2 shows the properties of this release film.
  • a release film was obtained in the same manner as in Example 4, except that the thickness of the silicone release layer in Example 4 was set to 100 nm. Table 2 shows the properties of this release film.
  • a release film was obtained in the same manner as in Example 4, except that the amount of particles added to the silicone release layer in Example 4 was 30% by weight. Table 2 shows the characteristics of this release film.
  • a release film was obtained in the same manner as in Example 4, except that diphenylsiloxane was added so that the diphenylsiloxane content in the release layer was 5 mol%. Table 2 shows the characteristics of this release film.
  • Example 4 0.93 108 1200 70 1.5 ⁇ ⁇ Example 5 3.8 28 104 9600 95 2 ⁇ ⁇ ⁇ Example 6 0.93 108 1300 72 1.5 ⁇ ⁇ Comparative Example 4 0.7.10 105 100 40 X ⁇ Comparative example 5 13 48 104 8 300 180 3.3 3.3 XX Comparative example 6 26 63 102 13000 230 1.5 ⁇ X Comparative example 7 0.78 13 93 1100 75 1.5 X ⁇

Abstract

L'invention concerne un film détachable comprenant un film à base de polyester ayant une surface présentant une irrégularité adéquate et une couche détachable de silicone ou comprenant un film à base de polyester ayant une surface plane et lisse et une couche détachable de silicone présentant une irrégularité adéquate. Le film détachable fait preuve d'excellentes caractéristiques de surface de manière qu'il est exempt de problèmes, à savoir les concavités et convexités de la surface sont transférées à la surface d'une feuille formée, fait preuve d'une excellente capacité au traitement et d'excellentes caractéristiques détachables.
PCT/JP2003/006473 2002-05-27 2003-05-23 Film detachable WO2003099556A1 (fr)

Priority Applications (3)

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AU2003242434A AU2003242434A1 (en) 2002-05-27 2003-05-23 Releasing film
KR1020047010442A KR100919440B1 (ko) 2002-05-27 2003-05-23 이형 필름
JP2004507063A JP3950462B2 (ja) 2002-05-27 2003-05-23 離型フィルム

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JP2002-152484 2002-05-27
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ITMI20150550A1 (it) * 2015-04-16 2016-10-16 Siliconature S P A Procedimento per la siliconatura di pellicole di polietilene tereftalato (pet).
US9728768B2 (en) 2013-03-15 2017-08-08 Sion Power Corporation Protected electrode structures and methods
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AU2003242434A1 (en) 2003-12-12
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CN100379553C (zh) 2008-04-09
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