WO2005021258A1 - 表面保護フィルム及びその製造方法 - Google Patents
表面保護フィルム及びその製造方法 Download PDFInfo
- Publication number
- WO2005021258A1 WO2005021258A1 PCT/JP2004/012529 JP2004012529W WO2005021258A1 WO 2005021258 A1 WO2005021258 A1 WO 2005021258A1 JP 2004012529 W JP2004012529 W JP 2004012529W WO 2005021258 A1 WO2005021258 A1 WO 2005021258A1
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- WIPO (PCT)
- Prior art keywords
- polysulfone
- silicone rubber
- protective film
- surface protective
- rubber layer
- Prior art date
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Definitions
- the present invention relates to a surface protective film and a method for producing the same, and more particularly, to a method for easily peeling off an adhesive silicone rubber layer from an adhesive silicone rubber layer and improving the adhesiveness of the adhesive silicone rubber layer to a semiconductor chip or a semiconductor chip mounting portion.
- the present invention relates to a surface protective film which does not adversely affect the surface flatness of an adhesive silicone rubber layer, and a method for producing the same, which does not adversely affect the surface flatness of an adhesive silicone rubber layer.
- a semiconductor device is a package in which a semiconductor chip is wrapped in a package, and is also called a semiconductor element. And arithmetic circuits.
- FIG. 1 A semiconductor chip 1 (also referred to as a silicon wafer), which is an IC or LIC, is centered, and its lower surface is bonded to the upper surface of the adhesive silicone rubber layer 2.
- the lower surface of the adhesive silicone rubber layer 2 is bonded to the upper surface of the semiconductor chip mounting portion 3 [In this state, in the present invention, the semiconductor chip 1 is attached to the semiconductor chip via the adhesive silicone rubber layer 2. It is sometimes described as bonded (synonymous with attachment) to part 3. Ko.
- the adhesive silicone rubber layer has a role of bonding the semiconductor chip 1 and the semiconductor chip mounting portion 3 and relieving stress between the semiconductor chip 1 and the semiconductor chip mounting portion 3.
- the semiconductor chip 1 and the circuit wiring 4 are connected by bonding wires 5, and the blocks of the semiconductor chip 1, the adhesive silicone rubber layer 2, the semiconductor chip mounting portion 3 and the circuit wiring 4 are sealed with an epoxy resin. It is sealed with a blocking agent to protect it from dust, dust, moisture, impact, etc. in the outside air, and to radiate the heat generated inside to the outside.
- a liquid crosslinkable (synonymous with curable) silicone composition such as a paste-like crosslinkable silicone composition
- a system adhesive was used.
- Such silicone-based adhesives include an organopolysiloxane having at least two silicon-bonded alkenyl groups in one molecule, and an organopolysiloxane having at least two silicon-bonded hydrogen atoms in one molecule. And a catalyst for hydrosilylation reaction are used, and a silicone atom-bonded alkoxy group, a silicon atom-bonded alkenyl group or a silicon atom-bonded group in one molecule is used as an adhesion promoter.
- a crosslinkable silicone composition comprising an organopolysiloxane having at least one atom-bonded hydrogen atom has been used (for example, see Patent Document 1).
- such a crosslinkable silicone composition has a problem in that low-viscosity silicone oil oozes out of the composition during crosslinking, and contaminates the surroundings of the composition.
- This low-viscosity silicone oil is a low-polymerization degree organopolysiloxane contained in the main component organopolysiloxane, or a low-polymerization degree organopolysiloxane contained in an onoleganopolysiloxane added as an adhesion promoter. Because of the siloxane, it was very difficult to completely remove them. For this reason, after bonding the semiconductor chip and the chip mounting portion using such a crosslinkable (curable) silicone composition, the wire bondability between the bonding pad and the bonding wire or beam lead on the chip is reduced. And the reliability of the obtained semiconductor device becomes poor.
- Adhesive silicone rubber layer (which is synonymous with sheet and may be used hereafter) and particularly good adhesiveness in such an adhesive silicone rubber layer.
- a semiconductor device having excellent characteristics has been proposed (for example, see Patent Document 2).
- Films such as fluororesin, polyethylene resin, polypropylene resin, polyimide resin, polyester resin, polyether resin, polyethersulfone resin, epoxy resin, and phenol resin are used as the surface protection film (for example, See Patent Document 24
- Polyethylene resin sheets (synonymous with films, layers, etc.) and polypropylene resin sheets are inexpensive, but the melting point is lower than the crosslinking temperature of the silicone rubber composition. If it is difficult to form a thick adhesive silicone rubber layer, there is a problem.
- Polyimide resin sheets are extremely excellent in heat resistance, dimensional stability, etc., but are expensive, and have some problems in releasability from the adhesive silicone rubber layer.
- Polyester resin (eg, polyethylene terephthalate) sheets have poor releasability from the adhesive silicone rubber layer.
- Polyether resin sheets are expensive and have very poor releasability from the adhesive silicone rubber layer.
- Polyethersulfone (PES) resin sheet is most used as a surface protection film because of its good releasability from the adhesive silicone rubber layer.
- PES Polyethersulfone
- Epoxy resin sheets are not used because they have very poor releasability from the adhesive silicone rubber layer.
- the phenolic resin sheet is not used because of poor flexibility.
- a general release film (separator) whose surface has been subjected to a silicone release treatment has an adhesive property to the adherend (semiconductor chip ⁇ the chip mounting portion) of the adhesive silicone rubber layer after the release film is peeled off. There is a problem of lowering.
- a strong polar inert liquid [DMSO (dimethyl sulfoxide), DMF (dimethylformamide)] is used as a solvent. It has been proposed to use a mixed solvent mainly composed of a cycloaliphatic ketone and a highly volatile aliphatic ketone (for example, see Patent Document 5).
- the polysulfone dimer and the like crystallize and the solution becomes turbid, and when the turbid polysulfone-based resin solution is formed into a film and formed into a film, the haze increases.
- the resulting film has a large surface roughness. Therefore, prior to the film forming process, filtration with a filter and heat treatment at 80 ° C or higher are performed (for example, see Patent Documents 6 to 8).
- the filtration step lowers the productivity, and the heat treatment requires the use of a high-boiling solvent, so that the drying step requires a high temperature or a long time, and there is a problem in productivity. And, with these measures, sufficient surface smoothness has not yet been obtained.
- Patent Document 1 Japanese Patent Application Laid-Open No. 3-157474 (Claims, etc.)
- Patent Document 2 JP-A-11-12546 (Claims, page 4, etc.)
- Patent Document 3 JP-A-2000-80335 (Claims, page 4, etc.)
- Patent Document 4 JP 2001-19933 A (Claims, page 11, etc.)
- Patent Document 5 JP-A-49-110725 (Claims, etc.)
- Patent Document 6 JP-A-5-329857 (Claims, etc.)
- Patent Document 7 Japanese Patent Application Laid-Open No. 7-233265 (Claims, etc.)
- Patent Document 8 JP-A-7-268104 (Claims, etc.)
- an object of the present invention is to easily peel off the adhesive silicone rubber layer, and to adversely affect the adhesiveness of the adhesive silicone rubber layer to a semiconductor chip or a semiconductor chip mounting portion.
- Surface protective film having excellent surface smoothness of the surface protective film itself without containing any residual organic solvent and having no adverse effect on the thickness uniformity and surface flatness of the adhesive silicone rubber layer, and a method for producing the same. It is to provide
- the present inventors prototyped a surface protection film made of various plastic films and a laminate composed of the surface protection film and an adhesive silicone rubber layer. Numerous experiments have been conducted on the effects of peelability and adhesive silicone rubber layer on the adhesiveness of semiconductor chips and semiconductor chip mounting parts, the effect of adhesive silicone rubber layer on surface flatness, and the surface smoothness of the surface protection film itself. As a result, a surface obtained by laminating a polysulfone-based resin layer (B) formed by using a polysulfone-based resin solution composition using a specific combination of mixed solvents on at least one surface of the base film was obtained. Protective film found good results for peelability, adhesion, surface flatness, surface smoothness, etc. This has led to the completion of the present invention.
- an adhesive silicone rubber layer (C) comprising a polysulfone resin layer (B) laminated on at least one surface of a base film (A)
- the polysulfone resin layer (B) has a boiling point of at least one of ratatones (a) or aromatic ketones (b) and a cyclic ketone (c).
- a surface protective film characterized by being formed of a polysulfone-based resin solution composition obtained by dissolving at least one polysulfone-based resin in a mixed solvent comprising an aliphatic ketone (d) at 150 ° C or lower. Is done.
- a diameter of 50 mm Provided is a surface protective film characterized by having a circular unevenness force of ⁇ ⁇ or more and SI or less.
- the adhesive strength between the base film (A) and the polysulfone-based resin layer (B) is not less than N / m.
- a surface protection film is provided.
- the surface protective film according to the first aspect wherein the base film (A) is a polyethylene terephthalate film.
- the surface protective film according to the first aspect wherein the amount of the mixed solvent contained in the surface protective film is 1000 mg / m 2 or less. You.
- the thickness of the base film (A) is O—200 ⁇ m
- the thickness of the polysulfone-based resin layer (B) is 0.
- a surface protective film having a thickness of 1 to 50 ⁇ m.
- the surface protective film according to the first aspect wherein the peel strength with the adhesive silicone rubber layer (C) is 4 N / m or less. .
- a polysulfone-based resin layer (B) is formed by applying a polysulfone-based resin dope on at least one surface of the base film (A) and drying it.
- the present invention provides a method for protecting an adhesive silicone rubber layer (C) formed by laminating a polysulfone resin layer (B) on at least one surface of a base film (A) as described above.
- the surface protective film wherein the polysulfone resin layer (B) is composed of at least one of ratatones (a) or aromatic ketones (b) and cyclic ketones (c) and a fat having a boiling point of 150 ° C or less.
- the present invention relates to a surface protective film or the like characterized by being formed from a system resin solution composition. Preferred embodiments thereof include the following.
- the mixing ratio (parts by volume) of the solvent in the mixed solvent must satisfy the following expressions (1)-(4) simultaneously based on 100 parts by volume of the total mixed solvent.
- a surface protection film characterized by the following.
- the blending amount of the polysulfone resin in the polysulfone resin solution composition is 1 to 30 parts by weight with respect to 100 parts by weight of the mixed solvent. .
- the polysulfone resin is a polysulfone resin (PSF), a polyethersulfone resin (PES), or a polyphenylsulfone resin (PPSU).
- PSF polysulfone resin
- PES polyethersulfone resin
- PPSU polyphenylsulfone resin
- the dope is composed of at least one of a radione (a) or an aromatic ketone (b), a cyclic ketone (c) and an aliphatic having a boiling point of 150 ° C or less.
- a method for producing a surface protective film which is a polysulfone-based resin solution obtained by dissolving at least one polysulfone-based resin in a mixed solvent comprising a ketone (d).
- the crosslinkable silicone which is a raw material of the adhesive silicone rubber layer (C) is used.
- the corn rubber composition comprises (a) an organopolysiloxane having at least two silicon-bonded alkenyl groups in one molecule, and (a) an organopolysiloxane having at least two silicon-bonded hydrogen atoms in one molecule.
- a laminate comprising siloxane, (c) an adhesion promoter, and (2) a catalyst for a hydrosilinolelation reaction.
- the surface protective film of the present invention can be easily peeled off from the adhesive silicone rubber layer and contains a residual solvent that adversely affects the adhesiveness of the adhesive silicone rubber layer to the semiconductor chip and the semiconductor chip mounting portion.
- the surface protection film itself has excellent surface smoothness, there is an effect that the surface flatness of the adhesive silicone rubber layer is not adversely affected.
- the force between the surface protective film of the present invention and the adhesive silicone rubber layer can be easily peeled off, and the adhesiveness between the adhesive silicone rubber layer and the semiconductor chip or the semiconductor chip mounting portion is extremely low. It is excellent and has an effect that a highly reliable semiconductor device can be manufactured.
- FIG. 1 is a cross-sectional view showing an example of a semiconductor device (hybrid IC) to which the laminate of the present invention is applied.
- FIG. 2 is a cross-sectional view showing one example of a semiconductor device (LSI) to which the laminate of the present invention is applied.
- LSI semiconductor device
- FIG. 3 is a diagram showing the composition of three components constituting a mixed solvent used in the polysulfone-based resin solution composition according to the present invention.
- FIG. 4 is a cross-sectional view showing one example of the surface protective film of the present invention.
- FIG. 5 is a cross-sectional view of a laminate composed of A / B / C / B / A, which is an example of the use of the surface protective film of the present invention.
- Circuit board made of epoxy resin
- Circuit board made of epoxy resin
- the surface protective film of the present invention has a surface for protecting an adhesive silicone rubber layer (C) formed by laminating a polysulfone-based resin layer (B) on at least one surface of a base film (A).
- the polysulfone resin layer (B), which is a protective film comprises at least one of ratatones (a) or aromatic ketones (b), a cyclic ketone (c) and an aliphatic ketone having a boiling point of 150 ° C or lower. It is characterized by being formed from a polysulfone-based resin solution composition obtained by dissolving at least one kind of polysulfone-based resin in a mixed solvent which is strong with ketone (d).
- the base film (A) is a film that serves as a base material of the surface protective film of the present invention and bears the mechanical strength of the surface protective film. At least one of the surfaces is a polysulfone-based film.
- the resin layer (B) is laminated.
- the raw material resin of the base finolem (sheets) made of
- the base film (A) has an adhesion strength with the polysulfone resin layer (B) of 5 NZm or more, preferably 7 N / m m or more, more preferably 10 N / m or more.
- those satisfying the above requirements are excellent in adhesion to polyethylene terephthalate film and polysulfone resin layer (B), and can be laminated with an adhesion strength of 5 NZm or more. It is the most preferred substrate film because it has excellent handleability due to its unevenness in thickness and thinness and its stiffness.
- the peel strength of the adhesive silicone rubber layer (C) from the surface protective film may be lower. If the adhesive strength is lower than 5 NZm, the surface protective film may be bonded to the adhesive silicone rubber layer (C). ) Cannot be peeled off from the surface, and the base film (A) and the polysulfone-based resin layer (B) peel off, so that the object of the present invention cannot be achieved.
- the thickness of the base film (A) is not particularly limited, but is, for example, 10 to 200 / im, preferably 30 to 150 Pm, and more preferably 40 to 100 Pm. If the thickness is less than 10 ⁇ m, the film is not stiff and the handleability is poor.On the other hand, if the thickness exceeds 200 / im, the stiffness is too strong and it is difficult to wind up the rolls. It becomes up and is not desirable.
- the base film (A) may be added with an antioxidant, a heat stabilizer, a lubricant, a pigment, an ultraviolet ray inhibitor and the like, if necessary.
- the base film (A) may be subjected to a corona discharge treatment or an undercoat treatment.
- the adhesive silicone rubber layer Since the polysulfone-based resin layer (B) used in the present invention forms an interface with the adhesive silicone rubber layer (C), the adhesive silicone rubber layer has good releasability from the adhesive silicone rubber layer (C). Poor adhesion performance of layer (C) to semiconductor chip or semiconductor chip mounting part It is necessary not to contain any influencing components.
- polysulfone-based resins such as polyethersulfone resins are most used as surface protective films because of their good releasability from the adhesive silicone rubber layer as described above.
- a polysulfone-based resin sheet is used as the surface protective film
- a thread-shaped (or beard-shaped) cutting residue is formed. Because of the large number of occurrences, there is a problem in that poor adhesion between the adhesive silicone rubber layer (C) and the semiconductor chip or the semiconductor chip mounting portion occurs due to the mixing of the punched residue.
- the surface protective film is characterized in that a polysulfone-based resin layer (B) is laminated on at least one surface of the base film (A).
- the thickness of the polysulfone-based resin layer (B) is not particularly limited, but is, for example, 0.150 x m, preferably 0.520 x m, and more preferably 13 / im. When the thickness is less than 0.1 ⁇ , it is difficult to form the polysulfone-based resin layer (B). On the other hand, when the thickness is more than 50 / m, the amount of punched waste increases, which is not preferable.
- polysulfone-based resins are also used for coating materials, paints, adhesives, and the like.When manufacturing them, usually, polysulfone-based resins are dissolved in a solvent, a solution composition is prepared, and the solution is used as it is or The product is applied to the surface of the base material and dried to produce a product.
- the polysulfone-based resin layer (B) is composed of at least one of ratatones (a) or aromatic ketones (b) and cyclic ketones (c) and an aliphatic having a boiling point of 150 ° C. or lower. It is formed of a polysulfone-based resin solution composition obtained by dissolving at least one polysulfone-based resin in a mixed solvent comprising ketone (d).
- the polysulfone-based resin is uniformly dissolved in the polysulfone-based resin solution composition.
- the polysulfone-based resin solution composition is applied and dried to form the polysulfone-based resin layer (B)
- the polysulfone-based resin layer (B) has excellent surface smoothness.
- a mixed solvent refers to It is a mixed organic solvent that can produce a rufone-based resin solution.
- the mixed solvent according to the present invention comprises at least one of radians (a) or aromatic ketones (b), a cyclic ketone (c), and a fat having a boiling point of 150 ° C or less. It is necessary that the mixture ratio (volume part) in the mixed solvent (100 vol. Part) satisfies the following equations (1)-(4) at the same time.
- a mixed solvent outside of these specific ranges that is, a solvent that does not simultaneously satisfy the formulas (1) and (4), cannot dissolve the polysulfone resin or only swells and gels the polysulfone resin. Absent.
- a binary mixed solvent of two selected from the species that is, excellent surface smoothness cannot be achieved, and even if a three-component mixed solvent is used, Those in a range not satisfying the formulas (1) and (4) cannot similarly achieve the object of the present invention, and are therefore not preferred.
- ratatones (a) or the aromatic ketones (b) one or more kinds may be used from the group of solvents described in detail below.
- Ratatatones (a) are cyclic compounds having an ester group (1 C ⁇ _ ⁇ 1) in the ring, for example, / 3-propiolatatatone (boiling point: 100 102 ° C), ⁇ _butyrolataton (boiling point) : 206.C), ⁇ _ valero lataton (boiling point: 206-207.C), ⁇ -valero lataton (boiling point: 218 220 ° C), ⁇ -force prolatatone (boiling point: 233.3.C), ethylene carbonate (boiling point: 238 ° C), propylene carbonate (boiling point: 90 ° C, @ 5 mmHg), hinokitiol (boiling point: 140 141 ° C, @ 10 mmHg), diketene (boiling point: 127 ⁇ 4 ° C) and the like.
- the values in Kakko are boiling points at 103.3
- the aromatic ketone (b) is a ketone having an aromatic ring group.
- the cyclic ketones (c) are cyclic compounds having a ketone group (one CO—) in the ring, such as cyclobutanone (boiling point: 100 to 102 ° C), cyclopentanone (boiling point: 130 ° C), Cyclohexanone (boiling point: 156.7 ° C), heptanone (boiling point: 179-18C), methylcyclohexanone (boiling point: 165-166 ° C), cyclooctanone (boiling point: 74 ° C, @ 1.6kPa) ), Cyclononanone (boiling point: 93-95.C, @ 1.6 kPa), cyclodecanone (boiling point: 107 ° C, @ 1.7 kPa), cycloundecanone (boiling point: 108.C, @ 1.6 kPa), cyclododecanone (Bo
- the aliphatic ketone (d) is an aliphatic ketone having a boiling point of 150 ° C. or less, for example, acetone (boiling point: 100 102.C), methylethyl ketone (boiling point: 100-102.C).
- Methyl propyl ketone (boiling point: 100 102 ° C), methyl isobutyl ketone (boiling point: 100 102.C), methyl n-butyl ketone (boiling point: 100 102 ° C)), methyl sec-butyl ketone (boiling point) : 100-102 ° C), diisobutyl ketone (boiling point: 100-102 ° C), pinacolone (boiling point: 106.4 ° C), methyl isoamyl ketone (boiling point: 144-9 ° C), getyl ketone (boiling point: 101 ⁇ 8 ° C), diisopropyl ketone (boiling point: 1250 ° C), ethyl ketone pill ketone (boiling point: 123.2 ° C),
- butyl acetyl ketone (boiling point: 147.3 ° C.).
- a polysulfone resin is a thermoplastic resin having an aromatic ring group in its main chain and a sulfone group as a bonding group thereof, and is roughly classified into a polysulfone resin, a polyethersulfone resin, and a polyphenylsulfone resin. Is done.
- a polysulfone resin (sometimes referred to as PSF) is a polymer having a structure represented by the following chemical formula (5), and was released from Union Carbide in the United States in 1965. is there.
- the polymer represented by the above chemical formula (5) is obtained by using, as raw materials, an alkali metal salt of bisphenol A (Na salt) and a chlorinated compound of bisphenol S (4,4 'dichloromouth diphenyl sulfone).
- a polyether sulfone resin (sometimes abbreviated as PES) is typically a polymer having a structure represented by the following chemical formula (14).
- PES is obtained by the Friedel-Crafts reaction of diphenyl ether chlorosulfone.
- PES includes Ultrason E (registered trademark, manufactured by BASF, Germany and imported and sold by Mitsui Chemicals, Inc.), Radel (registered trademark) A [produced by Amoco, USA, and Tijin Amoco Engineering Import and sales by Sumitomo Chemical Co., Ltd.] and Sumikaetacell (registered trademark, manufactured and sold by Sumitomo Chemical Co., Ltd.) are available as commercial products.
- the polyphenylsulfone resin (also referred to as PPSU) is typically a polymer having a structure represented by the following chemical formula (15).
- the polysulfone-based resin solution composition refers to at least one of ratatones (a) or aromatic ketones (b), cyclic ketones (c), and aliphatic ketones having a boiling point of 150 ° C or less.
- the blending amount of the polysulfone-based resin in the polysulfone-based resin solution composition is 1 to 30 parts by weight, preferably 5 to 20 parts by weight, based on 100 parts by weight of the mixed solvent. If the compounding amount is less than 1 part by weight, the viscosity becomes low and application becomes easy, and the life of the solution composition is prolonged, but the thickness of the polysulfone-based resin layer (coating film) is 0.1 ⁇ m. If it exceeds 30 parts by weight, the viscosity becomes so high that a polysulfone-based resin layer (coating) having a uniform thickness cannot be obtained, and the life of the solution composition becomes short, which is not desirable.
- the polysulfone-based resin solution composition includes an antioxidant, an ultraviolet absorber, and an antistatic agent. If necessary, a blocking agent, a flame retardant, a dye, a pigment, a lubricant, a fungicide, an antibacterial agent, a leveling agent, and the like can be added.
- a leveling agent include calcium perfluoroalkyl sulfonate, potassium perfluoroalkyl sulfonate, ammonium perfluoroalkyl sulfonate, perfluoroalkyl ethylenoxide, and perfluoroalkyl alkylene sulfonate. Trimethyl ammonium salt, fluorinated alkyl ester and the like can be mentioned.
- the polysulfone-based resin layer (B) is composed of a dope, ie, at least one of ratatones (a) or aromatic ketones (b), a cyclic ketone (c) and an aliphatic ketone having a boiling point of 150 ° C or less.
- a polysulfone-based resin solution obtained by dissolving at least one polysulfone-based resin in the mixed solvent consisting of (d) and a thin film of 0.150 xm, preferably 13 x
- the substrate film (A) preferably a polyethylene terephthalate film, and a high quality surface protective film can be provided at low cost.
- the surface smoothness of the polysulfone-based resin layer (B) is determined by the Nomarski differential interference microscopy. It is characterized by having one or less circular irregularities with a diameter of 50 ⁇ or more in the field of view lmm 2 when observed, and in particular, has excellent surface smoothness of the polysulfone resin layer (B) itself. It can be.
- the field lmm 2 in diameter 50 zm or more circular uneven force ⁇ pieces less is meant, when the surface protective film of the present invention is used, the surface is excellent in flat lubricity, to have sufficient gloss Or high transparency.
- the adhesive silicone rubber layer (C) since the surface of the surface protective film of the present invention has a smooth surface, problems such as entrapment of air bubbles occur. Absent.
- the surface smoothness of the polysulfone-based resin layer is poor, gloss is poor, transparency is low, etc. There is a problem.
- air bubbles are entrapped in the uneven portion, and it becomes difficult to produce a good laminate.
- the surface protective film of the present invention is obtained by laminating the polysulfone-based resin layer (B) on at least one surface of the base film (A), and adheres to a product to be adhered such as a semiconductor device. It is used to protect the adhesive silicone rubber layer (C) used for this purpose.
- the substrate film (A) is preferably a polyethylene terephthalate film, and the substrate film (A) and the polysulfone-based resin layer (B) are laminated with an adhesive strength of at least 5 N / m. Must not be peeled off.
- the peel strength between the surface protective film and the adhesive silicone rubber layer (C) is 4 NZm or less, preferably 3 NZm or less, and more preferably 2 N / m or less. Accordingly, the object of the present invention, which has no influence on the adhesive performance of the adhesive silicone rubber layer (C), can be achieved.
- the surface protective film of the present invention comprises a base film (A) having a thickness of 10-200 / im, on at least one side of which a polysulfone-based resin dope, ie, the above-mentioned polysulfone-based resin solution is coated. After the application, a drying process is performed, and a polysulfone-based resin layer (B) having a thickness of 0.1 to 50 / im, preferably 0.5 to 20 / im, more preferably 13 to 13 / m is laminated. Can be manufactured by the power S.
- the coating method can be used as the coating method.
- the application method by wire bar coating can precisely control the amount of the solution composition to be applied, and can improve the surface smoothness of the applied film. As a result, a surface protective film with excellent surface smoothness can be obtained. It is preferable because it can be obtained.
- the solution temperature at the time of applying the polysulfone-based resin solution composition onto the base film is preferably 20 to 50 ° C. in terms of production cost.
- the drying method is as follows: first, at 25-40 ° C, relative humidity 70, 100% RH for 2-10 minutes, then at next 150, 150 ° C, relative humidity 30-70% RH at 0.1. It is preferable to dry for 5 minutes Good.
- the amount of the mixed solvent used for forming the polysulfone-based resin layer (B) remaining on the surface protective film that is, the total residual solvent amount of the surface protective film, in other words, the mixed solvent contained in the surface protective film.
- the amount is less than 1000 mg / m 2 , preferably less than 800 mg / m 2, more preferably less than 500 mg / m 2 . If the total residual solvent amount exceeds 1000 mg / m 2 , the adhesion of the adhesive silicone rubber layer (C) is hindered, and the quality of the product to be bonded, for example, the operation of the semiconductor chip is adversely affected, which is not preferable.
- the solvent at least one of the above-mentioned radians (a) or aromatic ketones (b), a cyclic ketone (c) and an aliphatic ketone having a boiling point of 150 ° C or less (
- the polysulfone-based resin solution composition is applied to the base film, and N ⁇ ⁇ x, SOx, salt It is not possible to generate a dagger.
- an organic solvent containing nitrogen such as N-methyl-2-pyrrolidone or N, N-dimethylformamide, an organic solvent containing sulfur such as thiophene or dimethyl sulfoxide, or an organic solvent containing halogen such as dichloromethane or chloroform is used.
- N ⁇ x, S ⁇ x, and chloride may be generated during combustion for disposal of the solvent component that evaporates when the resin solution composition is applied and dried. Environmentally unfavorable.
- the analysis of the total amount of the residual solvent can be easily performed by gas chromatography (GC) or gas chromatography mass spectrometry (GC-MS).
- the surface protective film of the present invention is mainly for protecting the adhesive silicone rubber layer (C) used for bonding the semiconductor chip to the semiconductor chip mounting portion with dust power. It needs to be peeled off.
- the surface protective film of the present invention has a peel strength of the surface protective film with respect to the adhesive silicone rubber layer (C) when the surface protective film is adhered to both sides of the adhesive silicone rubber layer (C).
- Each is preferably 4N / m or less.
- Adhesive silicone rubber layer (C) If the peel strength of the surface protective film to the adhesive silicone rubber layer (C) exceeds 4 N / m, the adhesive silicone rubber layer (C) may be damaged when the surface protective film is peeled off. Because. [0068] 4. Adhesive silicone rubber layer (C)
- the adhesive silicone rubber layer (C) is mainly used for bonding a semiconductor chip and a semiconductor chip mounting portion.
- a polysulfone resin layer is provided between two surface protection films.
- An adhesive silicone rubber layer (C) is laminated via (B) to form an intermediate layer.
- the adhesive silicone rubber layer (C) is already cross-linked (cured) or semi-cross-linked (semi-cured)
- the raw material is a silicone rubber composition that has not been crosslinked (cured) or semi-crosslinked (semi-cured) as described in detail below.
- This silicone rubber composition has not yet been crosslinked, but is sometimes referred to as a crosslinkable silicone rubber composition with the meaning that it can be crosslinked.
- the raw material is referred to as a crosslinkable silicone rubber composition to distinguish it from the adhesive silicone rubber layer (C).
- examples of the crosslinkable silicone rubber composition include those that are crosslinked by a hydrosilylation reaction, those that are crosslinked by a condensation reaction, those that are crosslinked by an organic peroxide, and those that are crosslinked by ultraviolet light. Preferably, they are crosslinked by a hydrosilylation reaction.
- the hydrosilylation reaction-crosslinkable silicone composition includes, for example, (a) an organopolysiloxane having at least two silicon-bonded alkenyl groups in one molecule, and (a) at least two organopolysiloxanes in one molecule.
- Onoreganopolysiloxane having a silicon atom-bonded hydrogen atom (c) an adhesion promoter and (2) a catalyst for a hydrosilylide reaction.
- the component (i) is a main component of the composition, and is an organopolysiloxane having at least two silicon atom-bonded alkenyl groups in one molecule.
- the molecular structure of the component (a) include a straight-chain structure, a partially branched straight-chain structure, a branched chain structure, and a network structure.
- the alkenyl group bonded to a silicon atom in the component (a) include a butyl group, an aryl group, a butenyl group, a pentyl group and a hexenyl group, and a butyl group is particularly preferable.
- the bonding position of the alkenyl group examples include a molecular chain terminal and / or a molecular chain side chain.
- the group bonded to a silicon atom other than the alkenyl group in the component (ii) includes alkyl groups such as methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group and heptyl group.
- Aryl groups such as phenyl group, tolyl group, xylyl group and naphthyl group; aralkyl groups such as benzyl group and phenethyl group; chloromethyl group, 3_chloropropyl group, 3,3,3_trifluoropropyl group And substituted or unsubstituted monovalent hydrocarbon groups such as halogenated alkyl groups, etc., and particularly preferred are a methyl group and a phenyl group.
- the obtained silicone-based adhesive sheet has excellent cold resistance, and the reliability of a semiconductor device manufactured using this silicone-based adhesive sheet is further improved.
- the content of the phenyl group with respect to the organic group bonded to the silicon atom is not less than ⁇ mol%, more preferably, it is within the range of 116 mol%. It is particularly preferred that it is in the range of mol%.
- the viscosity of the component (a) is not particularly limited, but the viscosity at 25 ° C. is preferably within the range of 100-1, 000, OOOmPa's (cP).
- the (port) component is a cross-linking agent for the cross-linkable silicone rubber composition, and is an onoleganopolysiloxane having at least two silicon-bonded hydrogen atoms in one molecule.
- the molecular structure of the (mouth) component include a straight chain, a partially branched straight chain, a branched chain, a ring, and a network.
- the bonding position of the hydrogen atom bonded to the silicon atom in the (mouth) component include a molecular chain terminal and / or a molecular chain side chain.
- Examples of the group bonded to a silicon atom other than a hydrogen atom in the (mouth) component include an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group, and a heptyl group.
- alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group, and a heptyl group.
- aryl groups such as phenyl, tolyl, xylyl, and naphthyl
- aralkyl groups such as benzyl and phenethyl
- chloromethyl 3_chloropropyl, 3,3,3_trifluorophenol, etc.
- a substituted or unsubstituted monovalent hydrocarbon group such as a halogenated alkyl group, and a methyl group and a phenyl group are particularly preferable.
- the viscosity of the (mouth) component is not particularly limited, but the viscosity at 25 ° C. is preferably in the range of 1-100, OOOmPa's (cP).
- the content of the (mouth) component in the crosslinkable silicone rubber composition is an amount sufficient to crosslink (cure) the composition, and this is the amount of the alkenyl group bonded to the silicon atom in the composition.
- Mo It is preferred that the amount of silicon-bonded hydrogen atoms to the metal be in the range of 0.5 to 10 moles, and it is particularly preferable that this amount be in the range of 115 moles.
- the component (c) is a component for improving the adhesion of a crosslinked product of the composition, and includes the following silatrane derivative, a functional group-containing silicone compound, and an organopolysiloxane. Examples are siloxane oligomers.
- JP-A-2001-19933 (the aforementioned Patent Document 4), JP-A-2000-265063, JP-A-2000-302977, JP-A-2001-19933, and JP-A-2001-261963 And JP-A-2002-38014, JP-A-2002-97273 and the like, and among these compounds, typical ones are shown below.
- burtriethoxysilane burtris (2-methoxyethoxy) silane, 3-glycidoxypropyltrimethoxysilane, 2_ (3,4-epoxycyclo) Xinole) ethinoletrimethoxysilane, vinylinoletrimethoxysilane, 3-meta
- Examples of the above onoreganosiloxane oligomer include the following compounds. [0084]
- the content of the component (c) in the crosslinkable silicone rubber composition is an amount sufficient to impart good adhesiveness to the adhesive silicone rubber layer (C). 0.01 to 20 parts by weight is preferred for 100 parts by weight. 0.1 to 10 parts by weight is particularly preferred.
- the component (2) is a catalyst for accelerating the crosslinking of the crosslinkable silicone rubber composition by the hydrosilylation reaction, and is a well-known catalyst such as a platinum catalyst, a rhodium catalyst, and a palladium catalyst.
- Platinum-based catalysts such as complexes and platinum carbonyl complexes are preferred because of their good reaction rates.
- the content of the component (2) in the crosslinkable silicone rubber composition is an amount sufficient to promote the crosslinking of the composition.
- the amount of platinum metal in this catalyst should be within 0.01-1-1, OOOppm by weight. It is particularly preferred that this amount be in the range of 0.1-500 ppm. This is because a composition in which the content of the component (2) is less than the lower limit of the above range tends to have a remarkably low cross-linking rate, whereas the composition exceeds the upper limit of the above range. This is because the crosslinking speed is not so improved, but rather, there is a possibility that a problem such as coloring of the crosslinked product may occur.
- the crosslinkable silicone rubber composition preferably contains a hydrosilylation reaction inhibitor in order to adjust the rate of the hydrosilylation reaction.
- the hydrosilylation reaction inhibitor include alkyne alcohols such as 3-methinole_1-butyn-13_ol, 3,5-dimethinole_1-hexin-3-one, phenylbutynol, and the like; 3-methynole_3_pentene_1 Enyne compounds such as _in, 3,5-dimethyl-3-hexene-11-in; 1,3,5,7-tetramethyl-1,3,5,7-tetravininolecyclotetrasiloxane, 1,3,5 , 7-tetramethinole-1,3,5,7-tetrahexenylcyclotetrasiloxane and benzotriazole are exemplified.
- the content of the hydrosilylation reaction inhibitor varies depending on the crosslinking conditions of the composition. In practice, the content is within the range of 0.000001 to 5 parts by weight based on 100 parts by weight of the component (a). Is preferred.
- the above-mentioned composition may further contain, as optional components, precipitated silica, wet silica, fumed silica, calcined silica, titanium oxide, alumina, glass, quartz, aluminoic acid, iron oxide, zinc oxide, calcium carbonate, Inorganic fillers such as carbon black, silicon carbide, silicon nitride, and boron nitride; and inorganic fillers obtained by treating these fillers with organic silicon compounds such as organohalosilanes, organoalkoxysilanes, and organosilazanes; Organic resin fine powder such as resin, epoxy resin and fluororesin; filler such as conductive metal powder such as silver and copper; dyes, pigments, flame retardants and solvents.
- precipitated silica, wet silica, fumed silica calcined silica, titanium oxide, alumina, glass, quartz, aluminoic acid, iron oxide, zinc oxide, calcium carbonate
- Inorganic fillers such as carbon
- a polysulfone resin layer (B) is formed on at least one surface of the base film (A) (see FIG. 4) to protect the adhesive silicone rubber layer (C).
- Used to The surface protective film and the adhesive silicone rubber layer (C) are joined via a polysulfone-based resin layer (B) to form a laminate.
- the layer configuration of the entire laminate be in the order of AZB / C / B / A (see FIG. 5).
- the upper r page number is a typical one.
- the order may be ⁇ .
- the lower surface protective film layer (BZA) of the laminate composed of AZBZCZB / A was peeled off, and the lower surface of the exposed adhesive silicone rubber layer (C) was placed on the upper surface of the semiconductor chip mounting portion.
- the surface protective finolem layer (A / B) on the upper side of the remaining AZBZC laminate is peeled off, and the upper surface of the exposed adhesive silicone rubber layer (C) is placed under the semiconductor chip. Then, the semiconductor device shown in FIG. 1 or FIG. 2 is manufactured, for example.
- the obtained sample was subjected to a tensile test in the opposite direction, and the ratio of the area in which the adhesive silicone rubber layer was cohesively broken on the adherend was determined to be the cohesion failure rate (Q / o).
- the laminate was cut into strips of lcmW ⁇ 15 cmL, and the average stress when one surface protective film was peeled at a speed of 1000 mm / min by 180 ° using a tensile tester was taken as the peel strength. [0096] [Adhesion strength of polysulfone resin layer]
- Adhere cellophane tape (registered trademark) on the surface of the surface protection film, cut out into 2.5cmW x 15cmL strips, and measure the average stress when 180 ° peeling was performed at a speed of 1000mm / min using a tensile tester.
- the surface smoothness of the polysulfone-based resin layer when observed by Nomarski differential interference microscopy, circular irregularities of more than a diameter of 50 zm in view lmm 2 is evaluated by some number exists, S1 or less and the number force Was passed ().
- a 50 ml glass sample bottle was charged with a 5 mm square surface protection film (250 x 200 mm), and then 10 ml of closhol form was added and dissolved at room temperature for 24 hours. , the analysis by weight of the mixed solvent containing per lm 2 results from the surface protective film, i.e. the total residual solvent content of the surface protective film (MGZ m) into the threaded Mamoru.
- polysulfone-based resin layer (B) “Sumikaetacell PES5200G” manufactured by Sumitomo Chemical Co., Ltd., which is a polyethersulfone resin, was used.
- the crosslinkable silicone rubber composition was sandwiched between surface protective films, and the thickness of the crosslinkable silicone rubber composition was adjusted to 200 ⁇ m using two stainless steel rolls with adjusted clearance. In this state, the laminate was heated in a hot air circulating oven at 80 ° C for 30 minutes to cause a cross-linking reaction to prepare a laminate.
- the whole amount of the obtained reaction mixture was transferred to an eggplant type flask, and low boiling components were distilled off by a rotary evaporator to obtain 132 g of a pale yellow transparent liquid.
- PES polyethersulfone resins
- One side of a PET film [Toray “Noremirror QT32” (thickness: 50 / im)] is coated with a dope of the above-mentioned polyethersulfone resin solution composition using a reverse roll coater and dried to obtain a dry film thickness of the polysulfone resin.
- a coating film of ⁇ m was formed to prepare a surface protective film (1).
- the obtained surface protective film (1) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminate (1).
- Surface protection film (1) and laminate (1) have 100% adhesion, 0.9 N / m peel strength, 20 N / m adhesion strength, and surface smoothness is lmm 2 And less than 200 mg / m 2 in total residual solvent, and when the laminate (1) is punched with a Thomson punching machine, the generation of punched lint is reduced. It is of sufficient quality as a surface protection film and laminate.
- y- butyrate port Rataton 40 volume 0/0 a mixed solvent 100 parts by volume consisting of cyclohexanone 30% by volume of cyclohexane and methyl E chill ketone 3 0 vol%, polyethersulfone resins (PES) [Sumitomo “Sumika Etasel” (registered trademark) manufactured by Chemical Industry Co., Ltd. £ 35003?], And stirred for 24 hours to prepare a polyethersulfone resin solution composition.
- PES polyethersulfone resins
- a dope of the above polyethersulfone resin solution composition was applied to one side of a PET film [Tetron HS made by Teijin Dupont (thickness: 50 zm)] using a reverse roll coater and dried to obtain a dry film thickness of the polysulfone resin.
- a ⁇ m coating film was formed to produce a surface protective film (2).
- the obtained surface protective film (2) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminate (2).
- Surface protective film (2) and the laminate (2) is adhesive 100%, peel strength 1. 0N / m, the adhesion strength 25NZm, surface smoothness diameter 50 mu m or more circular irregularities in view lmm 2 1 Less than 200 mg / m 2 and the total amount of residual solvent is less than 200 mg / m 2 , and when the laminate (2) is punched by a Thomson punching machine, the surface protection with less generation of punching swarf (filamentous scallop) It is of sufficient quality as a film or laminate.
- PES polyethersulfone resins
- a dope of the above polyethersulfone resin solution composition was applied to one side of a PET film [Tetron HS made by Teijin Dupont (thickness: 50 zm)] using a reverse roll coater and dried to obtain a dry film thickness of the polysulfone resin.
- a ⁇ m coating film was formed to produce a surface protective film (3).
- the surface protection film (3) and the laminate (3) have 100% adhesiveness, 0.9 N / m peel strength, 20 N / m adhesion strength, and a surface unevenness of lmm 2 with a diameter of 50 ⁇ or more. And less than 200 mg / m 2 of total residual solvent, and when the laminate (3) is punched by a Thomson punching machine, the amount of thread-like whiskers and whisker-like punching residue generated is small. It is of sufficient quality as a surface protection film and laminate.
- y- butyrate port Rataton 30 volume 0/0 a mixed solvent 100 parts by volume consisting of cyclohexanone 30% by volume of cyclohexane and methyl E chill ketone 4 0 vol%, polyethersulfone resins (PES) [manufactured by Sumitomo Chemical Industry Co., , "Sumikaetacell” (registered trademark)? £ 35003?], And stirred for 24 hours to prepare a polyethersulfone resin solution composition.
- PES polyethersulfone resins
- a dope of the above polyethersulfone resin solution composition is applied to one side of a PET film [Tetron HS (manufactured by Teijin Dupont) (thickness: 50 / im)] using a reverse roll coater and dried to obtain a dry film thickness of the polysulfone resin.
- a coating film of 2 ⁇ m was formed to produce a surface protective film (4).
- the obtained surface protective film (4) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminate (4).
- Surface protective film (4) and the laminate (4) is adhesion of 100%, peel strength 0. 9N / m, the adhesion strength 20NZm, surface smoothness circular irregularities diameter of at least 50 mu m in view lmm 2 1 Less than 200 mg / m 2 and the total amount of residual solvent is less than 200 mg / m 2 , and when the laminated body (4) is punched by a Thomson punching machine, the surface protection with less occurrence of punching swarf in the form of thread and whiskers) It is of sufficient quality as a film or laminate.
- PET film [Toray “Noremirror QT32” (thickness 50 ⁇ m)] is used as the surface protection film (3). Prepared.
- the surface protective film (5) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminate (5).
- the surface protective film (5) and the laminate (5) have a large peel strength between the surface protective film and the adhesive silicone rubber layer. It is of insufficient quality as a laminate.
- the following PES film was prepared as a surface protection film (6).
- This surface protection film uses a PES film as a base material and has a single-layer structure.
- PES Huinolem was prepared by drying a Sumitomo Chemical Co., Ltd. PES resin "Sumikaetacell PES5200G” at 160 ° C for 8 hours to a water content of 0.08% by weight.
- the PES resin pellets were melt-extruded at 300 ° C from an extruder equipped with a T-die and cooled and solidified to produce a 75 ⁇ thick PES film.
- the surface protective film (6) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminated body (6).
- the surface protective film (6) and the laminate (6) had a peel strength of 1. IN / m and an adhesive property of 95%. There was no problem, but the laminate (6) was punched with a Thomson punching machine. In this case, the quality of the surface protection film and the laminate is insufficient for the generation of a large amount of punching swarf in the form of thread or whiskers.
- a dope of the above polyethersulfone resin solution composition was applied to one side of a PET film [Tetron HS made by Teijin Dupont (thickness: 50 zm)] using a reverse roll coater and dried to obtain a dry film thickness of the polysulfone resin.
- a ⁇ m coating film was formed to produce a surface protection film (7).
- the obtained surface protective film (7) was laminated on the adhesive silicone rubber layer (C) by the above-mentioned method to produce a laminate (7).
- the surface protective film (7) and the laminate (7) have an adhesiveness of 100%, a peel strength of 7 NZm, an adhesion strength of 13 NZm, and a surface smoothness of lmm 2 with four circular irregularities with a diameter of 50 ⁇ m or more.
- punched laminate (7) in Thomson punching machine the occurrence of scrap filamentous (or whisker-like) is small, a total residual solvent content 1200 mg / m 2, the surface protection film, It is of insufficient quality as a laminate.
- Base film 1 PET (Lumira-) PET (Tetron) PET (Tetron) ⁇ ( ⁇ tron) ET (Lumirror) PES PET (Tetron)
- the surface protective film of the present invention can be easily peeled off from the adhesive silicone rubber layer and contains no residual solvent which adversely affects the adhesiveness of the adhesive silicone rubber layer to the semiconductor chip or the semiconductor chip mounting portion.
- the excellent surface smoothness of the surface protection film itself does not adversely affect the surface flatness of the adhesive silicone rubber layer.
- the surface protective film of the present invention and the adhesive silicone rubber layer can be easily peeled off, and the adhesiveness between the adhesive silicone rubber layer and the semiconductor chip or semiconductor chip mounting portion is extremely low. It is capable of producing excellent and highly reliable semiconductor devices.
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- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
Claims
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US10/569,633 US20060251907A1 (en) | 2003-09-01 | 2004-08-31 | Surface protection film and method for producing the same |
JP2005513506A JPWO2005021258A1 (ja) | 2003-09-01 | 2004-08-31 | 表面保護フィルム及びその製造方法 |
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Cited By (2)
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JP2010018751A (ja) * | 2008-07-14 | 2010-01-28 | Dow Corning Toray Co Ltd | ヒドロシリル化反応により硬化してなるシリコーン層を備えた基材の製造方法および回収された有機溶媒を使用するシリコーン組成物 |
JPWO2011004756A1 (ja) * | 2009-07-06 | 2012-12-20 | 昭和電工株式会社 | 配線板の保護膜用熱硬化性組成物 |
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TW201406698A (zh) * | 2012-08-09 | 2014-02-16 | Hon Hai Prec Ind Co Ltd | 保護蓋及其加工方法 |
US9996173B2 (en) * | 2013-02-12 | 2018-06-12 | Illinois Tool Works, Inc. | Front panel overlay incorporating a logic circuit |
JP5852998B2 (ja) * | 2013-07-29 | 2016-02-09 | 藤森工業株式会社 | 表面保護フィルム、及びそれが貼合された光学部品 |
KR101943705B1 (ko) * | 2016-06-27 | 2019-01-29 | 삼성에스디아이 주식회사 | 점착필름, 이를 포함하는 광학부재 및 이를 포함하는 광학표시장치 |
CN107861180B (zh) * | 2017-10-31 | 2024-08-16 | 惠州市华隆工艺品有限公司 | 一种具有反光功能的硅胶贴及其制备方法 |
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