Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
  • C09J7/00—Adhesives in the form of films or foils
  • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
  • C09J7/22—Plastics; Metallised plastics
  • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
  • C09J7/255—Polyesters
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
  • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the groups H01L21/18 - H01L21/326 or H10D48/04 - H10D48/07 e.g. sealing of a cap to a base of a container
  • H01L21/52—Mounting semiconductor bodies in containers
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
  • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
  • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
  • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
  • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors

Definitions

• the present invention relates to a base film for processing a semiconductor wafer using a biaxially oriented film containing polyethylene-1,2,6-naphthalenedicarboxylate as a main component. More specifically, when used as a base material of a pack grinding tape or a base material of a dicing tape in semiconductor wafer processing, particularly in a pack grinding process or a dicing process, a bag having excellent dimensional stability, smoothness, and strength.
• the present invention relates to a base film for grinding tape or dicing tape.
• plastic films such as polyolefin and its copolymer, polychlorinated vinyl and its copolymer, polyester, polycarbonate, polyamide, and polyimide have been used as the base film of the adhesive film and the release film of the dicing tape.
• plastic films such as polyolefin and its copolymer, polychlorinated vinyl and its copolymer, polyester, polycarbonate, polyamide, and polyimide have been used as the base film of the adhesive film and the release film of the dicing tape.
• polyester films are being used.
• a germanium compound is applied to a polymerization catalyst for the purpose of preventing a decrease in the yield of a silicon wafer caused by impurities contained in the polyester / reflective film and the silicone resin release layer
• Japanese Patent Laid-Open A method is disclosed.
• a technology relating to a release film for protecting an adhesive layer in storage of a knock grind tape or a dicing tape is disclosed in Japanese Patent Application Laid-Open No. H11-2010. .
• the conventional polishing method has problems such as damage to the wafer and longer polishing time than before. For example, a plasma etching method has been devised as a processing technique. Is coming.
• the processing temperature is higher than that of the conventional processing method.
• mechanical strength are becoming issues.
• the adhesive strength of the adhesive is reduced by calorie heat or UV irradiation, and then the tape is expanded to pick up each cut chip, or the chips are removed from the tape side.
• the push-up method There is a gap between the chips by using the push-up method.1 It is often said that if the tape shrinks greatly when the heat of calorie heats up, a chip pick-up force S occurs and the production efficiency of semiconductor wafers deteriorates. ing.
• Patent Document 1 Japanese Patent Application Laid-Open No. 5-1755332
• Patent Document 2 Japanese Patent Application Laid-Open No. Hei 11-5838
• Patent Literature 3 Japanese Patent Application Laid-Open No. H10-102-148081
• Patent Document 4 Japanese Patent Application Laid-Open No. H11-20110
• the object of the present invention is to solve the problems of the prior art and to solve the problems of the prior art, and to use the semiconductor wafer at a high temperature and a high humidity when used as a substrate of a back grinding tape or a substrate of a dicing tape.
• Excellent dimensional stability, smoothness, «strength, and! The purpose is to obtain a semiconductor film base film with good caroet aptitude. Further objects and advantages of the present invention will become apparent from the following description.
• the present invention is also achieved by the semiconductor wafer and the base film for processing according to the first aspect of the present invention, wherein the base film for processing a semiconductor wafer is for a pack grinding tape or a dicing tape.
• the above objects and advantages of the present invention are: Third, the amount of extracted oligomer in the film is 0.8% by weight or less, and the refractive index in the thickness direction of the film is 1.8%.
• the present invention is also attained by the base film for semiconductor wafers according to the first aspect of the present invention, which has a value of not less than 501 and not more than 1.515.
• a back grinding tape having an adhesive layer on one surface of the base film for a back grinding tape of the first or second invention, and an adhesive layer on one surface of the base film for a dicing tape of the first or second invention. This is achieved by at least one of the dicing tapes.
• a pack grind tape composite further comprising a release film on the pressure-sensitive adhesive layer of the pack grind tape of the fourth present invention, and a release further on the pressure-sensitive adhesive layer of the dicing tape of the fourth present invention This is achieved by at least one of the dicing tabs having a film.
• the base film for processing a semiconductor wafer of the present invention is excellent in dimensional stability, smoothness and mechanical strength under high temperature, especially under high humidity.
• it is suitable for semiconductor wafers, dicing tapes used for processing, or pad grinding tapes.
• the base film for semiconductor wafers is mainly composed of polyethylene-12,61-naphthalenedicarboxylate (hereinafter sometimes referred to as PEN), and may be a copolymer or a mixture.
• PEN polyethylene-12,61-naphthalenedicarboxylate
• the main dicarboxylic acid component is naphthalenedicarboxylic acid
• the main glycol component is ethylene glycolone.
• examples of the naphthalenedicarboxylic acid include 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 1,5-naphthalenedicarboxylic acid, and the like.
• —Naphthalenedicarboxylic acid is preferred.
• Mainly means that at least 80 mo 1% of the total repeating units are ethylene-1,2,6-naphthalenedicarboxylate, which is a component of the polymer which is a component of the film of the present invention. It is more preferably at least 90% mo, particularly preferably at least 95% mo. In other words, it is sufficient that the polyethylene-1,2,6-naphthalenedicarboxylate film of the present invention does not extremely lose its original properties and that dimensional stability and high strength can be ensured when used under high temperatures.
• a compound having two esteno-1 ⁇ functional groups in the molecule is used as the copolymerization component of the copolymer other than the main component ethylene-1,2,6-naphthalenedicanoleboxylate. be able to.
• Examples of such compounds include oxalic acid, adipic acid, phthalic acid, sebacic acid, dodecanedicarboxylic acid, isophthalic acid, terephthalic acid, 1,4-cyclohexanedicarboxylic acid, 4,4'-diphenyldicarboxylic acid, Dicarboxylic acids such as phenylindanedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, tetralindicarboxylic acid, decalindicarboxylic acid and diphenyletherdicarboxylic acid can be preferably used.
• oxycarboxylic acids such as p-oxybenzoic acid and p-oxochetoxybenzoic acid can also be preferably used.
• propylene glycol, trimethylene glycol, tetramethylene glycol, hexamethylene glycol, cyclohexanemethylene glycol, neopentyl glycol, ethylene oxide adduct of bisphenol sulfone, ethylene oxide adduct of bisphenol A, diethylene glycol And dihydric alcohols such as polyethylene oxide glycol are also preferably used.
• These compounds can be used alone or in combination of two or more.
• isophthalic acid, terephthalic acid, 4,4'-diphenyldicarboxylic acid, 2,7-naphthalenedicarboxylic acid, p-oxybenzoic acid 1S are used as the acid component, and tris are used as the glycolone component.
• Methylene glycolone, hexamethylene glycol neopentyl glycol and bisphenol sulfone ethylene oxide adducts are preferred.
• polyethylene 1,2,6-naphthalenedicarboxylate used in the present invention may partially or entirely block terminal hydroxyl groups and / or carboxyl groups with a monofunctional compound such as benzoic acid or methoxypolyalkylene glycol. It may be what you did.
• the polyethylene-1,2,6-naphthalenediole reoxyxylate used in the present invention can be used to obtain a substantially linear polymer with an extremely small amount of a trifunctional or higher functional esteno-forming compound such as glycerin or pentaerythritol. It may be copolymerized within the range.
• the film of the present invention may be a mixture of polyethylene-1,2,6-naphthalene dicarboxylate as a main component and other organic polymers.
• organic polymers include polyethylene terephthalate, polyethylene isophthalate, polytrimethylene terephthalate, polyethylene-1,4,4′-tetramethylenediphenyldicarboxylate, polyethylene-1,2,7-naphthalenedicarboxylate, polytrimethylene-1,2, Examples include 6-naphthalenedicarboxylate, polyneopentylene-1,2,6-naphthalenedicarboxylate, and poly (bis (4-ethylenoxyphenyl) sulfone) -1,2,6-naphthalenedicarboxylate.
• polyethylene isophthalate polytrimethylene terephthalate, polytrimethylene-1,2,6-naphthalenedicarboxylate, poly (bis (4-ethyleneoxyphen-nore) sunolefon) 1,2,6-naphthalenedicarbonate ⁇ boxylate
• polyethylene isophthalate polytrimethylene terephthalate
• polytrimethylene-1,2,6-naphthalenedicarboxylate polytrimethylene-1,2,6-naphthalenedicarboxylate
• poly (bis (4-ethyleneoxyphen-nore) sunolefon) 1,2,6-naphthalenedicarbonate ⁇ boxylate is preferred.
• the organic polymer mixed with these PENs may be used alone or in combination of two or more.
• the proportion of the organic polymer mixed with PEN is at most 20 mo 1%, preferably at most 10 mo 1%, particularly preferably at most 5 mo 1%, in the repeating unit of the polymer. You.
• the production of such a mixture can be carried out by a generally known method for producing a polyester fiber.
• the polyester used in the present invention can be obtained by a conventionally known method.
• a method of directly obtaining a low-polymerization degree polyester by a reaction of dicarboxylic acid and dalicol, or a method of subjecting a lower alkyl ester of dicarboxylic acid and glycol to a transesterification reaction using a known transesterification catalyst The polymerization reaction may be carried out in the presence of a heavy vehicle.
• the ester exchange reaction catalyst include compounds containing sodium, potassium, magnesium, calcium, dumbbell, strontium, titanium, zirconium, manganese, and konoleto, and these may be used alone or in combination of two or more. .
• Antimony trioxide, antimony tetroxide, antimony pentoxide, antimony trichloride, antimony tribromide, antimony glycolate, antimony acetate, antimony compounds such as antimony trioxide, antimony acetate, and germanium dioxide are typical examples of heavy insect media. Titanium compounds such as germanium compounds, tetraethino retitanate, tetrapropyl titanate, tetraphenyl titanate or partial hydrochloride thereof, titanium-noreammonium oxalate, titanium potassium oxalate, and titanium trisacetyl acetate Can be Among the above polymerization catalysts, germanium conjugates are particularly preferably used.
• the resulting transesterification product is added to the obtained transesterification reaction product in a ffi state.
• the germanium compound used for the polycondensation reaction catalyst for example, (a) amorphous germanium oxide (mouth) fine crystalline germanium oxide (c) a solution in which germanium oxide is dissolved in water can be preferably used. .
• germanium oxides such as crystalline germanium dioxide, amorphous germanium dioxide, germanium tetraethoxide, and germanium tetra-n-butoxide can be preferably used.
• Germanium dioxide and amorphous germanium dioxide can be preferably used.
• Germanium metal remaining in the metal The element is preferably from 10 to 100 ppm by weight, more preferably from 10 to 500 ppm by weight, and still more preferably from 10 to 200 ppm by weight.
• concentration of germanium in the metal element was determined by setting the dried sample on a scanning electron microscope (SEM, trade name “S570” manufactured by Hitachi Measuring Instruments Service Co., Ltd.) and connecting the energy to it. It is a value obtained by quantitative analysis using a dispersive X-ray microanalyzer (XMA, trade name: AX-700, manufactured by HORIBA, Ltd.).
• ⁇ preferably contains a phosphorus compound for the purpose of deactivating the transesterification catalyst before the polymerization reaction.
• phosphorus compounds include phosphoric acid, phosphorous acid, phosphonic acid, phosphonate compounds and derivatives thereof, and these may be used in battle insects or in combination of two or more.
• a phosphonate compound represented by the following formula (I) is preferable as the phosphorus compound.
• R 1 and R 2 are an alkyl group having 1 to 4 carbon atoms
• X is one CH 2 — or one CH (Y) ⁇ (Y represents a phenyl group).
• R 1 and R 2 may be the same or different.
• Particularly preferred phosphorus compounds are carbomethoxymethanephosphonic acid, carbethoxymethanephosphonic acid, canolevopropoxymethanephosphonic acid, phenolic olevobutoxymethanephosphonic acid, carpomethoxy-phosphonopheninoleacetic acid, and canolevoethoxyphosphono Dimethylacetate, carbopropoxy-phosphonophenylacetate, and carbopoxy-phosphonophene / lexanoic acid dimethyl / leestenole, jetty / leestene / le, dipropinole ester and dibutyl ester.
• the reason why these phosphonate compounds are preferable is that the reaction with the metal compound proceeds relatively slowly as compared with the phosphorus compound which is usually used as a stabilizer. Long contact time of the compound As a result, the amount of catalyst added to the polyester can be reduced, and even if a large amount of stabilizer is added to the catalyst, the thermal stability of the polyester is impaired! / This is for you.
• the timing of the recommendation of these phosphorus compounds may be any time after the transesterification reaction is substantially completed, for example, under atmospheric pressure before the start of the polycondensation reaction, under reduced pressure after the start of the polycondensation reaction. At the end of polycondensation reaction or after completion of polycondensation reaction, ie polymer You may add after obtaining.
• the content of the phosphorus compound is preferably 20 to: L 00 weight ppm in polyethylene mono 2,6-naphthalenedicarboxylate as the phosphorus element in the phosphorus compound.
• the polyethylene-1,2,6-naphthalenedicarboxylate used in the present invention may be prepared by using 2,6-naphthalenedicarboxylic acid and ethylene glycol as raw materials, and may be 2,6-naphthalenedicarboxylate represented by 2,6-dimethylnaphthalate. Esteno W ⁇ -forming derivatives of acid and ethylene dalicol may be used as raw materials.
• the transesterification reaction is carried out under a pressure of not less than 0.05 MPa and not more than 0.2 OMPa, so that the amount of the metal compound added can be further reduced.
• polyester used in the present invention can be formed into chips after melt polymerization, and then subjected to solid-phase polymerization under calorific heat or in an inert gas stream such as nitrogen.
• solid-state polymerization is also preferably performed in the present invention.
• the intrinsic viscosity of the polymer containing polyethylene-1,6-naphthalenedicarboxylate as a main component is 0.40 (preferably not less than 1 1 / ⁇ and not more than 0.90 dl Zg).
• the intrinsic viscosity is a value (unit: d1 / g) measured at 25 ° C using o-chlorophenol as a solvent.
• the base particles for processing semiconductor wafers of the present invention have a small percentage of inert particles in order to impart slipperiness to the film.
• inert particles for example, particles such as spherical silica, porous silica, calcium carbonate, alumina, titanium dioxide, potassium chloride, barium sulfate, zeolite, or organic particles such as silicone resin particles and cross-linked polystyrene particles Can be mentioned.
• the inorganic particles are synthetic products rather than natural products because the particle size is uniform.
• the crystal morphology, hardness, specific gravity, and color of the particles are not particularly limited, and can be used according to the purpose.
• calcium carbonate examples include calcium carbonate, porous silica, spherical silica, and chao. Phosphorus, talc, magnesium carbonate, palladium carbonate, calcium sulfate, calcium sulfate, potassium sulfate, lithium phosphate, canolecum phosphate, magnesium phosphate, aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, lithium fluoride, etc. be able to.
• calcium carbonate particles spherical silica particles, porous silica particles, and plate-like aluminum silicate are particularly preferred.
• organic particles examples include organic particles and crosslinked polymer particles.
• organic salt particles include, for example, terephthalates such as calcium phosphate, calcium, norium, zinc, manganese, and magnesium.
• crosslinked polymer particle examples include an insect or copolymer of a vinyl monomer such as dibienolebenzene, styrene, acryloleic acid or methacrylic acid.
• fine particles such as polytetrafluoroethylene, a silicone resin, a benzoguanamine resin, a thermosetting epoxy resin, an unsaturated polyester resin, a hydrophobizable urea resin, and a hydrophobizable phenol resin are also preferably exemplified.
• silicone resin particles and crosslinked polystyrene particles are particularly preferred.
• the average particle size of each type of particles is preferably 0.05 to 5 ⁇ , and 0.08 ⁇ to 3.5. ⁇ am is more preferable, and it is particularly preferable that it is 0.10 m or more and 3 m or less. Further, the total amount of inert particles contained in the film is preferably 0.05% by weight or more and 3% by weight or less, more preferably 0.08% by weight or more and 2.0% by weight or less. It is particularly preferred that the content be 0.1% by weight or more and 1.0% by weight or less. ,
• the inert particles to be added to the film may be a single component selected from those exemplified above, or may be a multicomponent containing two or more components.
• a single component: ⁇ may contain two or more types of particles with different average particle sizes!
• the average of inert particles is determined by using a CP-50 centrifugal particle size analyzer (Centrifugal P a • rticle Size Ann a 1 yzer) j manufactured by Shimadzu Corporation. From the integrated curve of particles of each particle size and their abundance calculated based on the centrifugal sedimentation curve obtained from the measurement. This is a value obtained by reading the particle size corresponding to 0% by weight (see “Particle Size Measurement Technology”, published by Nikkan Kogyo Shimbun, p. 1979, p. '
• calcium carbonate particles having an average particle size of 0.3 to 111 or more and 0.8 zm or less are contained in an amount of 0.05 to 0.4% by weight and / or an average particle size of 0 to 0.4% by weight.
• Spherical particles having a particle size of 1 ⁇ m or more and 0.6 m or less are used in an amount of 0.3% by weight or more and 0.5% by weight or less, and the Z or average vertical diameter is 0.1 Zm or more and 0.6 ⁇ m.
• particles of the same type of inert particles having different particle sizes may be simultaneously contained.
• the film of the present invention may contain a nucleating agent, an antioxidant, a heat stabilizer, a lubricant, a flame retardant, an antistatic agent, a polysiloxane, etc., depending on the use.
• the addition time of the inert particles and other additives is not particularly limited as long as it is a stage before the film formation of polyethylene 1,261-naphthalenedicarboxylate. It can also be added during film formation. From the viewpoint of uniform dispersion, it is preferable to add inactive particles and other additives to ethylene glycol and add them at a high concentration during polymerization to form a master chip, and dilute the obtained master chip with an additive-free chip. Good.
• the semiconductor wafer and the base film for processing according to the present invention are biaxially oriented films containing the above-mentioned polyethylene-12,61-naphthalenedicarboxylate as a main component.
• the base film (which may be abbreviated as a film) in the present invention may be a single layer or a plurality of layers of two or more layers. It is preferable for achieving both flatness of the surface and winding property of the base film.
• a co-extrusion method, an extrusion laminating method, a coating method, and the like can be used, and are not particularly limited. It is preferable to form a plurality of layers by a co-extrusion method in which each resin is extruded from a plurality of extruders using 6-naphthalene dicanolepoxylate.
• the base film for processing a semiconductor wafer of the present invention is used for back grinding tape. Or preferably for dicing tape! / ,.
• the film of the present invention has a heat shrinkage of not more than 1.0% in both the film forming direction and the width direction when subjected to heat treatment at 200 for 10 minutes.
• the heat shrinkage of the film of the present invention is more preferably from ⁇ 0.20% to 0.80%, particularly preferably from 0.10% to 0.60%.
• the film forming direction is a traveling direction when a film is formed, and may be referred to as a longitudinal direction, a longitudinal direction, a continuous direction, a film direction or an MD direction of the film.
• the width direction is a direction orthogonal to the film forming direction in the in-plane direction of the film, and may be referred to as a lateral direction or TD.
• the heat shrinkage ratio after heat treatment at 200 ° C for 10 minutes exceeds 1.0%, the dimensional shrinkage of the base film will increase when the temperature rises in the semiconductor wafer processing process. On the other hand, since the wafer thermally expands, the wafer may fall off the adhesive of the tape during the processing process, or in some cases, the thickness of the wafer may be too thin.
• the heat shrinkage is less than 0.20%: ⁇ , that is, when the thermal expansion occurs, the thermal expansion of the base film becomes larger than the thermal expansion of the wafer. May move to the wafer surface from the part.
• any of the 8 8 ⁇ in which the shrinkage or expansion of the film is large beyond the scope of the present invention is not preferable because the semiconductor wafer mounted on the tape warps due to the difference from the expansion coefficient of the wafer. Also, if the expansion coefficient of the film is larger than the expansion coefficient of the semiconductor wafer, it warps with the wafer side inward and causes chips to stick together, so that the expansion of the film, that is, the heat shrinkage rate becomes negative. Direction must be suppressed as much as possible.
• the oligomer extraction amount of the film of the present invention is preferably 0.8% by weight or less under the condition of extracting with chloroform for 24 hours. It is more preferably 0.6% by weight or less, particularly preferably 0.5% by weight. / 0 or less. Oligomer extraction is 0.8 It exceeds weight 0/0 when the semiconductor Ueno, was used as a working base film: ⁇ a, your a processing temperature environment or a pressure-sensitive adhesive layer Coating process in step! / Polyolomer may precipitate on the surface of the base film, causing problems such as contamination in the processing step and a decrease in the adhesive strength between the pressure-sensitive adhesive layer and the base film.
• the most effective way to suppress the precipitation of oligomers on the film surface is to reduce the amount of oligomers contained in the film, and it is preferable to reduce the amount of oligomer extracted for this application.
• the intrinsic viscosity of polyethylene-2,6-naphthalenedicarboxylate be 0.45 dl / g or more and 0.90 dlZg or less. It is more preferably from 0.48 to 0.85 d1 / g, particularly preferably from 0.50 to 0.80 d1 / g. If the intrinsic viscosity of poly (1,6-naphthalenedicanolepoxylate) is less than the lower limit, the amount of finolem extracted oligomer will be too large, but will exceed the upper limit; ⁇ indicates excessive load in the polymerization and film forming process May be required.
• the intrinsic viscosity of the film is preferably 0.40 to 0.90 d1 / g.
• the intrinsic viscosity is a value (unit: d1 / g) measured at 25 ° C using o-chlorophenol as a solvent. Refractive index in the thickness direction>
• the refractive index (nz) in the thickness direction of the film of the present invention is preferably from 1.501 to 1.515. It is more preferably 1.503 or more and 1.513 or less, particularly preferably 1.504 or more and 1.52 or less.
• the refractive index in the thickness direction is less than 1.501, the laminating property of the film is degraded, so that burrs are generated on the cut end surface of the film.
• the refractive index in the thickness direction exceeds 1.515, the film becomes brittle, and when the tape is used as a base film for pack grind tape or dicing tape, the film tears when peeling. Sometimes.
• the variation in the thickness of the film of the present invention is preferably 15% or less, more preferably 10% or less, and particularly preferably 8% or less based on the average thickness of the film.
• the smaller the variation in film thickness the more uniform the bonding strength between the back grinding tape and the semiconductor wafer and the bonding surface between the dicing chip and the semiconductor wafer, and stable taping becomes possible.
• Back grinding and dicing can be performed, and a chip suitable for high definition and high density can be supplied.
• the Young's modulus of the film of the present invention is preferably 540 OMPa or more and 690 OMPa or less in both the film forming direction and the width direction of the film. OMPa or less, particularly preferably 560 OMPa or more and 670 OMPa or less. The difference between the Young's moduli in both directions is preferably 100 OMPa or less.
• the Young's modulus is less than 540 OMPa, the rigidity of the film will be insufficient, and it will be difficult to reduce the thickness of the base film for semiconductor wafer processing utilizing the high elastic modulus of polyethylene-2,61-naphthalenedicarboxylate film. Sometimes. On the other hand, if the Young's modulus exceeds 690 OMPa, a large amount of chips tend to be generated when cutting the film, which may contaminate processing in a clean state. Furthermore, when picking up each cut chip, it is difficult to push up the chip from the expanding tape side of the tape, which reduces production efficiency.
• the center line average surface roughness (Ra) on at least one side of the film of the present invention is preferably 3 nm or more and 80 nm or less, more preferably 5 nm or more and 60 nm or less, and particularly preferably 7 nm or more and 5 Onm or less. It is. Further, the film is preferably composed of two or more layers, and the sum of Ra on both surfaces of the film is preferably 10 nm or more, and more preferably 14 nm or more.
• the center line average roughness (R a) is determined by the method specified in JISB-0601, the cutoff is 0.25 mm, and the measurement probe is 3 ⁇ ⁇ .
• Ra Ra is less than 3 nm, the film will not slide easily, and the film surface will be abraded when transported during film production or when the film is wound, or the film will be in a whirl state. When the film is wound, it is difficult for air trapped between the film and the film to escape, and the air traps generated may impair the flatness of the film. On the other hand, if Ra exceeds 80 nm, the film slips too much, so that misalignment may frequently occur when winding the film or winding it after applying an adhesive layer on the film surface to form a tape. There is.
• the density of the film of the present invention is preferably 1.356 gZcm 3 or more and 1.364 gZcm 3 or less. More preferably, 1.357 ⁇ . It is not less than 111 3 and not more than 1.36 2 gZcm 3 . If the density is less than 1.356 gZ cm 3 , the crystallinity of the film is low; the semiconductor wafer may have insufficient dimensional stability in the processing step. If the density exceeds 1.364 gZ cm 3 , the crystallinity will be too high and the toughness of the film will be lost. Become.
• the density of the film is a value measured by the floatation method at 25 ° C during a density gradient using an aqueous solution of calcium nitrate as a solvent.
• the average thickness of the film of the invention is preferably from 9 in to 150 ⁇ , more preferably from 9 m to 125 m, and particularly preferably from 12 ⁇ m to 100; If the average thickness of the film is less than 9 m, there will be an age at which the strength of Nada, Ueno, and surface humidification as a support in Uenoka will be insufficient. On the other hand, if the average thickness of the film exceeds 150 ⁇ , the stiffness of the film becomes extremely strong, and even if the adhesive strength of the tape is slightly strong: In the case of ⁇ , the wafer may be damaged when the tape is peeled off, or dicing may occur. Later, the force to expand the film may be too great.
• the film of the present invention preferably has a coefficient of dynamic friction ( ⁇ d) between the films of 0.5 or less. If the number of friction ( ⁇ d) exceeds 0.5, the handleability during the film forming process and during the application of the adhesive layer will deteriorate, for example, when running on a roll in the process. Or, when wound up in a roll, drawbacks such as scratches may occur.
• ⁇ d coefficient of dynamic friction
• the heat shrinkage of the film was determined by calculating the heat shrinkage (SMD) in the film forming direction and the thermal TO ratio (S TD) in the width direction. It is preferable that the absolute value of the difference (
• SMD heat shrinkage
• S TD thermal TO ratio
• the back grinding tape in the present invention has an adhesive layer on the above-mentioned base for back grinding tape-one side of the film.
• a silicon wafer is stabilized by using a back grinding tape in which an adhesive layer is laminated on one side of a base film for a pack grinding tape for fixing the silicon wafer. It can be fixed in a state.
• the dicing tape in the present invention has the single-sided pressure-sensitive adhesive layer of the above-mentioned base film for dicing tape.
• a dicing tape in which an adhesive layer is laminated on one surface of a base film for dicing tape is used for fixing silicon wafers, and silicon wafers are fixed. Can be fixed in a stable state.
• the base film for a back grinding tape or a dicing tape of the present invention may be provided with a coating layer on at least one surface thereof for the purpose of improving the adhesiveness with an adhesive.
• the coating layer is preferably made of at least one water-soluble or water-dispersible polymer resin selected from a polyester resin, a urethane resin, an acryl resin, and a butyl resin, and particularly contains both a polyester resin and an attaryl resin. Power S preferred ,.
• the polyester resin of the coating layer used in the present invention has a glass transition point (T g) of 0 to: L 00 ° C, more preferably 10 to 90 ° C.
• the polyester resin is soluble in water. Or, a dispersible polyester / resin is preferred, but it may contain some organic solvent.
• the powerful polyester resin includes a polybasic acid or an ester / ester derivative thereof and a polyol or an estero conductor thereof as described below.
• polybasic acid components include terephthalenic acid, isophthalenic acid, phthalenic acid, phthalic anhydride, 2,6-naphthalenedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid, adipic acid, sepasic acid, trimellitic acid, Examples include melitic acid, dimer acid, and 5-sodium sulfonic acid.
• a copolymerized polyester resin is synthesized using two or more of these acid components.
• an unsaturated polycarboxylic acid such as maleic acid, itaconic acid and the like, and hydroxycarboxylic acids such as p-hydroxybenzoic acid.
• the polyol components include ethylene glycol, 1,4-butanediol, diethylene glycol, dipropylene glycol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, xylene glycolone, and dimethylolone.
• the acryl resin of the coating layer used in the present invention has a glass transition point (Tg) of 150 to 50 ° C, more preferably 150 to 25 ° C.
• Tg glass transition point
• the acryl resin is preferably water-soluble or dispersible acryl, but may contain some organic solvent.
• Such an acryl resin can be copolymerized from the following acrylic monomers.
• the acrylic monomer include alkyl acrylate, alkyl methacrylate (alkyl groups include methyl, ethyl, n-propyl, isopropyl, n-butynole, isobutyl, t-butynole, and 2-ethylhexyl). Group, cyclohexyl group, etc.); hydroxy such as 2-hydroxyethyl acrylate, 2-hydroxyethynolemethacrylate, 2-hydroxypropinolate tallate, 2-hydroxypropyl / methacrylate, etc.
• the composition used in the present invention is preferably used in the form of a water-based coating solution such as a watery night, an aqueous dispersion, or an emulsion in order to form a fine grain.
• a water-based coating solution such as a watery night, an aqueous dispersion, or an emulsion in order to form a fine grain.
• other resins other than the above composition for example, a polymer having an oxazoline group, a crosslinking agent such as melamine, epoxy, and aziridine, an antistatic agent, a coloring agent, a surfactant, ⁇ ]
• a strong lubricant may be added as necessary for the purpose of improving the slipperiness or blocking resistance of the film.
• the solid content concentration of the aqueous coating solution is usually 20% by weight or less, and preferably 1 to 10% by weight. If the proportion is less than 1% by weight, the coatability on the polyester film will be insufficient, while if it exceeds 20% by weight, the stability of the coating and the coating property may be degraded.
• the coating layer is applied firmly to the unstretched film or uniaxially stretched film by applying the aqueous coating solution, and then stretched in two or one direction and thermally fixed. Can be opened.
• a coating method a roll coat method, a gravure coat method, a roll brush method, a spray method, an air knife coat method, an impregnation method, a curtain coat method, or the like can be used or in combination.
• the pressure-sensitive adhesive constituting the back-grinding tape and the dicing tape of the present invention known pressure-sensitive adhesives can be widely used, but an ataryl-based pressure-sensitive adhesive is preferred.
• the ataryl adhesive specifically, copolymers with acryl-based polymers and other functional monomers selected from combat insect polymers and copolymers having an acrylic acid ester as a main structural unit. Combinations and mixtures of these polymers are used.
• acrylic acid esters of alkyl alcohols having 1 to 10 carbon atoms, methacryloleic acid esters of alkyl alcohols having 1 to 10 carbon atoms, vinyl esters of acetic acid, acrylonitrile, and butyl alkyl ether can be preferably used.
• the above acrylic copolymers can be used alone or in combination of two or more! / You can.
• the functional monomer for example, atalylic acid, methacrylic acid, maleic acid, 2-hydroxyxethynoleate tallate, 2-hydroxyethyl methacrylate, and the like are used.
• a cross-linking agent examples include a polyvalent isocyanate compound, a polyvalent epoxy compound, a polyvalent aziridine compound, and a chelate compound.
• polyvalent isocyanate compounds include toluylene diisocyanate, diphene / lemethane diisocyanate, hexamethylene diisocyanate, and isophorone diisocyanate. Etc. are used.
• polyepoxy compound include ethylene glycol diglycidyl ether, terephthalic acid diglycidyl ester atalylate, and the like.
• polyvalent aziridine compound specifically, tris-2,4,6-((1-aziridinole)-1,3,5-triazine, tris [1-1 (2-methinole) -aziridininole] phosphinoxide, hexa [ 11- (2-Methinole) -aziridininole] Triphosphatriazine or the like is used.
• the chelate compound include ethyl acetoacetate aluminum diisopropylate, aluminum tris (ethyl acetoacetate), and the like.
• the molecular weight of the acrylic copolymer obtained by polymerizing these monomers is 1.0 X 10 5 to: 10.0 X 10 5 , preferably 4.0 X 10 5 to 8.5. 0 X 1 0 5.
• a pressure-sensitive adhesive layer which can be hardened by irradiating a UV ray to reduce the adhesive force at the time of pickup can be used.
• a pressure-sensitive adhesive containing the above acrylonitrile-based copolymer as a main component and a radiation-polymerizable compound.
• Such radiation-polymerizable compounds are disclosed, for example, in JP-A-60-196,956 and JP-A-60-223,139.
• low molecular weight compounds having at least two or more photopolymerizable carbon-carbon double bonds in a molecule that can be three-dimensionally reticulated by light irradiation are widely used, specifically, trimethylol propane triatalylate, and tetramethylol.
• a polyurethane acrylate oligomer can be used in addition to the above-mentioned atalylate compound.
• the urethane atalylate-based oligomer is composed of a polyester compound such as a polyester type or a polyethenolate type, and a polyvalent isocyanate compound such as 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, Hydroxyl groups are present in the terminal isocyanate urethane prepolymer obtained by reacting 3-xylylene diisocyanate, 1,4-xylylene diisocyanate, diphenylmethane 4,4-diisocyanate, etc.
• This urethane acrylate oligomer is a radiation polymerizable compound having at least one carbon-carbon double bond.
• Such a urethane acrylate copolymer has a molecular weight of 300 to If a wafer having a size of 300,000, preferably 300,000 to 100,000, and more preferably 400,000 to 800, is used, the wafer chip can be used even for semiconductor wafers and rough surfaces. This is preferable because the adhesive does not adhere to the chip surface during the pick-up. Further, in order to use a urethane acrylate oligomer as a radiation polymerizable compound, at least a photopolymerizable single-carbon double bond must be included in the molecule as disclosed in JP-A-60-196,956.
• an extremely excellent pressure-sensitive adhesive sheet can be obtained.
• the adhesive force of the adhesive sheet before irradiation with the ultraviolet ray is sufficiently large, and the adhesive force after irradiation is sufficiently reduced so that the adhesive does not remain on the chip surface when picking up the wafer chip.
• the pressure-sensitive adhesive layer may contain, in addition to the pressure-sensitive adhesive and the crosslinkable polymerizable compound as described above, a compound that is colored by irradiation with radiation.
• a compound to be colored to the adhesive layer by such Nada line irradiation, the sheet is colored after the adhesive sheet is irradiated with radiation, and therefore, the wafer sensor is detected by an optical sensor. In this case, the detection accuracy is improved, and no malfunction occurs when picking up a wafer chip. Further, an effect is obtained that whether or not radiation has been applied to the pressure-sensitive adhesive sheet can be immediately determined visually.
• the compound colored by irradiation with the thigh line include leuco dye.
• leuco dye triphenylenomethane type, phenololean type, phenothiazine type, auramine type and spiropyran type dyes for poor use are preferably used.
• Developers preferably used with these leuco dyes include conventionally used electron acceptors such as phenol formalin resin prepolymers, aromatic carboxylic acid derivatives, and activated clay, and the like.
• Various known color formers can be used in combination.
• Such a compound that is colored by irradiation with X-rays may be included in the adhesive layer after being dissolved in an organic solvent or the like, or may be included in the adhesive layer in the form of fine powder. .
• This compound is present in the pressure-sensitive adhesive layer in an amount of 0.01 to 10% by weight, preferably 0.5 to 5% by weight. Desirable, used in an amount of / 0 .
• the back-grinding tape is usually stored in the form of a back-grid tape in which the surface of the pressure-sensitive adhesive layer is protected by a release film;
• the release film is peeled off and used in the Indian process. That is, the back grinding tape composite of the present invention further has a release film on the adhesive layer of the back grinding tape.
• Such a release film is obtained by laminating a silicone release layer on one side of a base film made of polyester, and bonding the silicone release layer surface to the adhesive layer surface of the pack grind tape to form a back grind tape.
• a silicone release layer is obtained by laminating a silicone release layer on one side of a base film made of polyester, and bonding the silicone release layer surface to the adhesive layer surface of the pack grind tape to form a back grind tape.
• the release film may further have a primer layer between the silicone release layer and the base film made of polyester.
• the dicing tape is usually stored in the state of a dicing tape composite in which the surface of the pressure-sensitive adhesive layer is protected by a release film, and the release film is peeled and removed in the dicing process. That is, the dicing tape composite of the present invention further has a release film on the adhesive layer of the dicing tape.
• a strong release film is made by laminating a silicone release layer on one side of a base film made of polyester.
• the silicone release layer surface and the adhesive layer surface of the dicing tape are bonded together to form a dicing tape: I do.
• the release film may further have a primer layer between the silicone release layer and the base film made of polyester.
• the polyester base film constituting the release film of the present invention may be composed of the same polyester as the base finolem for processing a semiconductor wafer of the present invention, or may be composed of a different polyester.
• Preferable examples of such polyesters include polyesters containing polyethylene terephthalate and polyethylene_2,6-naphthalenedicarboxylate as main components.
• “mainly” means that at least 8% of Omo 1% of the repeating unit in the polymer component is ethylene terephthalate or ethylene-1,6-naphthalenedicarboxylate, and more preferably 90%. mo 1% or more, particularly preferably 95 mo 1% or more.
• the polyester base film which constitutes the release film, is hardened by UV irradiation after curing, dicing, and curing.
• the light transmittance of the base film is preferably 85% or more.
• the silicone release layer constituting the release film of the present invention can be formed by applying a coating liquid containing, for example, a curable silicone resin to one surface of a polyester base film, followed by drying and curing.
• a curable silicone resin include a condensation reaction system, an addition reaction system, an ultraviolet or electron beam curing system, and a reaction system with a deviation, and one or more of such curable silicone resins can be used.
• the method for producing the base film of the present invention will be described in detail.
• the polyethylene-2,6-naphthalenedicarboxylate film of the present invention can be obtained by, for example, melt-extruding a resin at a normal extrusion temperature, that is, at a temperature not lower than the melting point (hereinafter referred to as Tm) (Tm + 70 ° C).
• Tm melting point
• the obtained film-like melt is quenched on the surface of a rotary cooling drum to obtain an unstretched film having an intrinsic viscosity of 0.40 to 0.90 dl Zg.
• a static adhesion method of applying an electrostatic charge to the film-like melt is known.
• polyethylene 1,2,6-naphthalenedioxy propyloxylate has a high electrical resistance of a molten material, so that the above-mentioned electrostatic adhesion to the cooling drum may be insufficient.
• quaternary sulfonic acid with 0.1 to 10 mmo 1% of esteno-forming functional group based on all bifunctional carboxylic acid components of polyethylene 1,2,6-naphthalene dicanoleboxylate It is preferred to include phosphonium.
• the unstretched film thus obtained is stretched in the longitudinal direction by a factor of 2.8 to 3.5 times at a temperature of 120 to 170 ° (more preferably, a temperature of 130 to 160 ° C).
• the film is stretched at a draw ratio of 2.8 to 3.6 times at 120 to 150 ° C in the transverse direction at the next V, and becomes a biaxial film.
• the elongation ratio is preferably in the range of 0.90 to 1.15 times the longitudinal stretching ratio in order to keep the thickness variation of the film within a desired range.
• the biaxially oriented film thus obtained may have a biaxially oriented film of from 235 to 255 ° C, more preferably from 240 to 250 ° C.
• the polyester refinolem of the present invention is heat-treated after winding.
• the method of heat treatment after winding is not specified, but a hanging-type loosening treatment method is particularly preferable.
• the suspended fiber treatment method is as follows: the film to be processed is dropped downward by its own weight through a mouthpiece installed above, heated by calories in the middle, and then turned almost horizontally while being cooled by rollers below.
• winding is performed after the winding tension is cut off by an ep-mouth.
• the hanging distance is preferably about 2 to 10 m.
• the heat treatment after the film forming step is performed in the film forming step (relaxation treatment after heat setting) if the heat shrinkage at 200 ° C. of the obtained biaxially oriented polyester film is within a desired range. Even if it is performed, even if it is performed by a relaxation heat treatment after the film is formed and once wound up, the processing method is not particularly limited.
• a preferred heating method is infrared heat because the film can be immediately calo-heated.
• a preferred relaxation heat treatment is a treatment in which the film temperature is set to 200 to 240 ° C. If the film temperature is lower than 200 ° C, it is difficult to reduce the heat shrinkage at 200 ° C.
• the film temperature exceeds 240 ° C
• the flatness tends to be worse.
• ⁇ the oligomer may precipitate and the film may become white. This whitening depends on the pressure history. For example, if a hanging belt is transported over the film part of a film roll, it will be 200. Even if it is less than C, the belt and the infested part are whitened: ⁇ .
• the film fi3 ⁇ 4 can be measured using a non-inverting infrared spectrometer (eg, a Burns ⁇ n radiometer).
• the suspension relaxation heat treatment method is preferable to the heat treatment in the film forming process because the heat shrinkage in a wide range of buoy / REM can be suppressed more uniformly.
• polyester base films that make up release films have been known for some time. Or can be obtained by methods that are accumulated in the art. That is, the unstretched polyester film that has been melted and extruded is uniaxially stretched, then stretched in a direction perpendicular to the stretching direction, and further subjected to a heat setting treatment.
• ⁇ can be applied, for example, by applying a coating liquid containing a component of a release layer to a polyester base film and drying by heating.
• a known coating method can be applied as a 'coating liquid' coating method, and for example, a low / coater method or a blade coater method can be used.
• Each composite is obtained by laminating the release film obtained by the above method on a pack grind tape dicing tape.
• the film is held in an oven set at a temperature of 200 ° C without tension for 10 minutes, and the dimensional change before and after the heat treatment is calculated as the heat shrinkage S (%) by the following equation (1). . ⁇
• L. Distance between gauges before heat treatment
• L distance between gauges after heat treatment.
• the sample width is 20 mm and length is 200 mm
• the distance between gauge points before heat treatment is 150 mm.
• the heat shrinkage was determined by measuring in both the machine direction (MD) and width direction (TD) of the film.
• the oligomer deposition rate as a percentage of the total area occupied by oligomers (appearing as white spots) with respect to the total area of the photograph is evaluated.
• the refractive index in the thickness direction (z) of the film was determined at 25 ° C using a Na-D line.
• the measurement is performed in both the film forming direction (MD) and the width direction (TD) of the finolem, and the Young's modulus is calculated from the tangent at the top of the obtained load-elongation curve.
• the cut-off is 0.25 mm
• the measuring probe is 3 ⁇ .
• a surface roughness meter (trade name “Surfcom SE-3CK” manufactured by Tokyo Seimitsu Co., Ltd.) ) Measure at.
• Film thickness ⁇ ⁇ Using a micrometer (trade name “K-402B” manufactured by Anritsu Corporation), the film thickness is 10 cm in each of the film forming direction (MD) and width direction (TD). The film thickness is measured at a total of 300 locations. The average value of the film thickness at 300 locations was calculated and the average film thickness t was calculated. ( ⁇ ).
• the film was made in the J ⁇ direction (MD) and the width direction (MD) at a needle pressure of 30 g and a running speed of 25 mmsec.
• TD Measure over a length of 2m each, and get a chart.
• the maximum thickness t ( ⁇ ) and the minimum thickness t 2 ( ⁇ ) are read from this chart. Average thickness t of the film thus obtained.
• ( ⁇ ) and the maximum thickness ( ⁇ , the minimum thickness t 2 ( ⁇ m), and force), and calculate the thickness variation D (%) using the following equation (3): D t 2 ) / t. ] X 1 00... (3)
• a stack of two 75mm (width) x 10 Omm (length) cut huinolems (sampnoles), a weight of 200 g is placed as a load W (g), and the upper film is slid at a speed of 150 mmZ. Calculate the number of moving and shaking from the force F d (g) when sliding. The film is measured after conditioning for 24 hours at 23 ° C and 65% R ⁇ . Number of dynamics F d , W
• the film was held for 10 minutes in an oven set at a temperature of 200 ° C without tension, and before and after each heat treatment in the film forming direction (MD) and width direction (TD). From the dimensional change, (1)
• the heat shrinkage S (%) is calculated by the following equation (1), as in the case of the heat shrinkage, and the absolute value of the difference in the heat shrinkage in both directions is calculated.
• L0 distance between gauge points before heat treatment
• L distance between gauge points after heat treatment
• the density of the biaxially oriented polyethylene-1,6-naphthalenedicarboxylate film was measured according to JIS C2151.
• dicing depth 20 ⁇ from tape surface
• four push-up pins diameter of suction holder: 28 ⁇
• collet pyramid collet
• throw-up distance 2mm
• dicing size 8111111 It is 8111111.
• Polymer C a polyethylene-1,6-naphthalenediene ruboxylate polymer having an intrinsic viscosity of 0.62 dlZg (referred to as “Polymer C”) was obtained. 170 ° C of this polymer C After being dried for 6 hours in the extruder, it is melted at a temperature of 30 ° C and melted through a slit die with an opening of l mm. The surface finish is 0.3 S, and the rotating drum has a surface temperature of 50 ° C. This was extruded to obtain an unstretched film.
• the unstretched film thus obtained is stretched 3.3 times in the direction (orientation) at 144, and then stretched 3.4 times in the transverse direction (width direction) at 140 ° C. Further heat-setting at 243 ° C for 5 seconds ⁇ ⁇ Shrink 5% in the width direction (tow-in) and apply a biaxially oriented PEN film with a thickness of 16 ⁇ m and an intrinsic viscosity of 0.5 2 d 1 / g to 1 It was wound up into a 300-Om width in a 50-Omm width.
• the obtained biaxially oriented PEN film is dripped downward by its own weight via the nip roller installed above, and the infrared excitation filter is set so that the finolem ⁇ J becomes 2225 ° C on the way.
• the roller After heating with a heating device, the roller is turned almost horizontally while cooling with a roll roller located 4 m below the roller installed above, winding off the winding tension with a nip roller, and winding and relaxing heat treatment. went. Relaxation was performed by using the difference in speed between the upper nip roller and the nip roller that shuts off the winding tension.
• Example 1 shows the property evaluation results of the obtained film of Example 1.
• a good pick-up operation could be performed without causing a malfunction due to a malfunction of the diponder device due to a change in the thermal dimension of the film, a variation in the thickness of the film or the flatness of the film.
• the semiconductor layer in the adhesive layer coating process was not contaminated, and the processing process was not contaminated.Further, the film was not broken by peeling off the tape, and the processing performance in manufacturing semiconductor wafers was good. .
• Example 2 The same operation as in Example 1 was repeated except that the stretching ratio in the direction of »was changed to 2.9 times, the stretching ratio in the horizontal direction was changed to 3.1 times, and the suspension relaxation heat treatment was not performed. A 5 ⁇ m biaxially oriented PEN film was obtained.
• Table 1 shows the property evaluation results of the obtained film of Example 2.
• the film thickness and workability of the example film there was no failure due to the malfunction of the die bonder device due to the change in the thermal dimension of the film, the thickness variation of the film, the flatness of the film, etc. Was.
• the inside of the adhesive layer coating process and the semiconductor No dyeing was observed, and no film was broken by tape peeling, and the workability in the production of semiconductor wafers was good.
• Example 3 a two-layer film was formed as follows. First, add 0.03 parts of manganese acetate tetrahydrate to a mixture of 100 parts of dimethyl 2,6-naphthalenedicarboxylate and 60 parts of ethylene glycol, and gradually raise the temperature from 150 ° C to 240 ° C. The transesterification was carried out while performing the reaction. Way, the reaction of antimony trioxide was added 0.024 parts at which point 1 70 ° C, further average elevation diameter 0.5 0.1 5 wt carbonate Cal Shiumu particles ⁇ 0 /. Was added. And the reaction temperature is 220.
• each of these polymers After drying each of these polymers at 170 ° C for 6 hours, they are fed to two separate extruders, each melted at 300 ° C, and co-extruded to form slits with an opening of 1 mm.
• the mixture was extruded through a die onto a rotating drum having a surface finish of 0.3 S and a surface of ⁇ J at 50 ° C to obtain a two-layer unstretched film.
• This unstretched film was successively biaxially stretched in the same manner as in Example 1 and heat-set to obtain a film thickness of 16 ⁇ m (polymer A layer side: 10 ⁇ m, polymer B layer side: 6 ⁇ ⁇ ).
• a biaxially oriented PEN film having a viscosity of 0.54 d 1 / g was wound up in a roll shape of 300 Om with a width of 150 Omm.
• the obtained biaxially oriented PEN film was subjected to a relaxation treatment using the same suspension-type relaxation heat treatment apparatus.
• the biaxially oriented PEN film after the relaxation treatment thus obtained was used as Example 3.
• Table 1 shows the property evaluation results of the obtained films of the examples.
• the film and workability of these films there was no failure due to a malfunction of the die bonder unit due to a change in the thermal dimension of the film, a variation in the thickness of the film, or the flatness of the film, and a good pick-up operation was performed. Further, the inside of the adhesive layer coating step, the semiconductor wafer, and the processing step were not contaminated, and further, the film was not broken by tape peeling, and the workability in the production of the semiconductor wafer was good.
• a 50m film of "Kapton; Type H” manufactured by Toray DuPont was used.
• Table 1 shows the characteristics of the film. Although the thermal dimensional change of the film was excellent, the dimensional stability under high humidity was poor due to the high water absorption.
• This polymer was dried at 170 ° C for 3 hours, fed to an extruder, melted at 290 ° C, passed through a slit die with an opening of 1 mm, surface finish 0.3 S, surface It was extruded on a rotating drum at a temperature of 25 ° C to obtain an unstretched film.
• the unstretched film obtained in this way is increased 3.2 times in the longitudinal direction (film forming direction) at 90 ° C. Stretched, then stretched 3.8 times in the transverse direction (width direction) at 120 ° C, and heat-set at 210 ° C for 5 seconds.
• a biaxially oriented polyethylene terephthalate film having 16, ⁇ ⁇ and an intrinsic viscosity of 0.55 dl Zg was wound into a roll of 3500 m in width of 1500 mm. After that, the obtained biaxially oriented polyethylene terephthalate film is suspended downward by its own weight through a nip roller installed above, and the infrared heating device is set so that the film temperature becomes 180 ° C in the middle.
• Table 1 shows the property evaluation results of the obtained film of Comparative Example 2.
• the chip was misaligned due to the poor dimensional stability of the film, and malfunctions occurred due to malfunction of the diponder device.
• the amount of oligomer “a” contaminating the inside of the adhesive layer coating step and the inside of the semiconductor wafer processing step was found. Also, the oligomer precipitation rate on the film surface after heating was high.
• Example 3 As Comparative Example 3, the same operation as in Example 2 was repeated except that the stretching ratio in the longitudinal direction was changed to 3.6 times and the stretching ratio in the transverse direction was changed to 3.7 times. An axially oriented PEN film was obtained.
• Table 1 shows the results of evaluating the characteristics of the fi / rem of Comparative Example 3 obtained.
• the thermal dimensional change of the film exceeds 1.0% in both the vertical and horizontal directions of the film, resulting in wafer processability, chip displacement, etc., and failure due to malfunction of the diponder device. occured.
• Comparative Example 4 the same operation as in Example 1 was repeated except that the stretching ratio in the horizontal direction was changed to 3.6 times and the stretching ratio in the horizontal direction was changed to 3.9 times, and the suspension-type relaxation fiber treatment was performed. Thus, a biaxially oriented PEN film having a thickness of 20 m was obtained. Table 1 shows the results of the regeneration evaluation of the obtained film of Comparative Example 4. The change in the thermal dimension of the film exceeded 1.0% in the longitudinal direction of the film, and in the case of the wafer and the workability, the chip was misaligned and the die bonder device failed due to malfunction.
• Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Layer Configuration Single Layer Single Layer Two Layer Single Layer Single Layer Single Layer Single Layer Polymer Polymer C Polymer C Polymer AI Bolima B-One Polymer C Polymer C Added particles
• Type Spherical silica Spherical silica Calcium carbonate I Spherical silica-Spherical silica Spherical silica Spherical silica Particle size U m 0.4 0.4 0.5 0.1-0.4 0.4 0.4 Amount added% by weight 0.20 0.20 0.15 0.05 1 0.20 0.20 0.20 0.20 Longitudinal stretching magnification 3.3 2.9 3.3 ⁇ 3.2 3.6 3.6 imJ3 ⁇ 4. 145 145 145 1 90 145 145 Lateral stretching magnification ⁇ 3.4 3.1 3.1 ⁇ 3.8 3.7 3.9
• 2,6-Naphthalenediphenyl dimethyl sulfonate (100 parts) and ethylene glycol (60 parts) are mixed with 0.03 parts of manganese acetate tetrahydrate, and the temperature is gradually raised from 150 ° C to 240 ° C. While performing an estenole exchange reaction. During the reaction, when the reaction temperature reached 170 ° C, 0.024 parts of antimony trioxide was added, and spherical silica particles having an average particle diameter of 0.6 ⁇ m and a particle diameter ratio of 1.1 were added. 1% by weight was added.
• reaction temperature reached 220 ° C.
• 0.042 parts corresponding to 2 mmol% of 3,5-dicarboxybenzenesulfonic acid tetrabutylphosphonium salt was added.
• an ester exchange reaction was subsequently carried out, and after the transesterification reaction was completed, 0.023 parts of trimethinol phosphate was added.
• the reaction product was transferred to a polymerization reactor, heated to 290 ° C, and subjected to a polycondensation reaction under a high vacuum of 0.2 mmHg or less.
• Polyethylene-1,2,6-naphthalene di- ore-boxylate polymer (polymer D) with an intrinsic viscosity of 0.43 d1 / g measured at night and polyethylene-1,2,6 with an intrinsic viscosity of 0.69 dlZg —A naphthalenedicarboxylate polymer (Polymer E) was obtained.
• Polymer E was further solid-phase polymerized to have an intrinsic viscosity of 0.78 dlZg (Polymer F).
• Polymer E 170 After drying at C for 6 hours, it is fed to an extruder, melted at a melting temperature of 305 ° C, extruded through a slit die with an opening of lmm, onto a rotating drum with a surface finish of 0.3 S and a surface of 50 ° C. An unstretched film was obtained.
• the unstretched film thus obtained is stretched 3.0 times in the longitudinal direction (film forming direction) at 145 ° C, and then stretched 3.0 times in the transverse direction ( ⁇ ⁇ direction) at 140 ° C in the next step. Then heat-set at 246 ° C for 5 seconds. @ 3 ⁇ 4 ⁇ Shrink 4% in the width direction (tow-in) and apply a 30 ⁇ m thick, 0.59 d 1 / g biaxially oriented PEN film to the 1 It was wound up in a 50 Omm width and 300 Om mouth shape.
• the obtained biaxially oriented PEN film is dripped downward by its own weight via a roll-up roller installed at the top, and the infrared temperature is adjusted so that the film temperature becomes 225 ° C on the way.
• the nip roller was placed 4 m below the roller placed above, and the direction was changed almost horizontally while cooling with a nip roller. Winding tension was cut off by a nip roller, and then the film was wound and subjected to relaxation heat treatment. Relaxation cuts off the winding tension with the upper nip roller. I went there.
• Example 4 The biaxially oriented PAN film thus obtained after the relaxation treatment was used as Example 4.
• Table 2 shows the property evaluation results of the obtained film of Example 4.
• a good pick-up operation could be performed without a failure due to a malfunction of the die bonder device due to a change in the thermal dimension of the film, a variation in the thickness of the film or the flatness of the film.
• the semiconductor wafer and the processing step were not contaminated in the adhesive layer coating step, the film was not broken by tape peeling, and the workability in the production of the semiconductor wafer was good.
• Example 5 The same operation as in Example 4 was repeated except that polymer F was used in Example 4, to obtain a 50- ⁇ m-thick biaxially oriented PAN film.
• the biaxially oriented PEN film thus obtained was used as Example 5.
• Table 2 shows the property evaluation results of the obtained film of Example 5.
• the heat and workability of the film of the example there was no failure due to the malfunction of the diponder device due to the change in the thermal dimension of the film, the variation in the thickness of the film, the flatness of the film, and the like, and a good pick-up operation was performed.
• the inside of the adhesive layer coating process, the semiconductor coating, and the inside of the processing process were not contaminated, and further, the film was not broken by tape peeling, and the workability in the production of semiconductor wafers was good.
• Example 4 the same as Example 4, except that the film was stretched 3.3 times in the machine direction at 145 ° C, and then stretched 3.3 times in the direction at 140 ° C. The operation was repeated to obtain a biaxially oriented ⁇ ⁇ ⁇ film having a thickness of 30 ⁇ m.
• the biaxially-oriented film obtained in this manner was used as Example 6.
• Table 2 shows the property evaluation results of the obtained films of the examples.
• a good pick-up operation could be performed without causing a failure due to a malfunction of the diponder device due to a change in the thermal dimension of the film, a variation in the thickness of the film or the flatness of the film.
• the inside of the adhesive layer coating step, the semiconductor wafer, and the processing step were not contaminated, and the tape was not broken by peeling off the tape.
• the flexibility in the production of semiconductor wafers was good.
• Example 7 The same operation as in Example 4 was repeated except that Polymer D was used in Example 4, to obtain a biaxially oriented PAN film having a thickness of 50 ⁇ m.
• the biaxially oriented PEN finolem thus obtained was used as Example 7.
• Table 2 shows the property evaluation results of the obtained film of Example 7.
• a good pick-up operation was performed without any failure due to malfunction of the die bonder due to changes in the thermal dimensions of the film, variations in the thickness of the film, and flatness of the film.
• contamination in the process due to oligomer precipitation on the film surface occurred.
• Example 6 the same operation as in Example 6 was repeated except that the amount of the inert particles contained in the film was set to 0.01% by weight and the heat setting was set to 233 ° C. A 30 ⁇ m biaxially oriented PEN film was obtained. The biaxially oriented PEN film / rem obtained in this manner was used as Example 8.
• Table 2 shows the property evaluation results of the obtained film of Example 8.
• the thermal dimensional change of the film is small, the difference in the thermal shrinkage in the vertical and horizontal directions exceeds the desired range, so that there is a slight problem in the stability in the production of semiconductor wafers. It was hot.
• Example 4 except that the film was stretched 2.7 times in the ifc direction at 145 ° C, and stretched 2.7 times in the horizontal direction at 140 ° C in Example 4. The same operation as in 4 was repeated to obtain a biaxially oriented ⁇ ⁇ ⁇ film having a thickness of 30 ⁇ .
• the biaxially-oriented film obtained in this manner was referred to as Run # 9.
• Table 2 shows the property evaluation results of the obtained films of the examples. Deterioration of the film process, although the thermal dimensional change of the film is small, the refractive index in the film thickness direction is high, causing contamination in the process due to film chips, etc., and film tearing at the time of tape peeling. did. [Table 2]

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