CN114075413A - Method for manufacturing protective film forming sheet roll - Google Patents
Method for manufacturing protective film forming sheet roll Download PDFInfo
- Publication number
- CN114075413A CN114075413A CN202110737442.4A CN202110737442A CN114075413A CN 114075413 A CN114075413 A CN 114075413A CN 202110737442 A CN202110737442 A CN 202110737442A CN 114075413 A CN114075413 A CN 114075413A
- Authority
- CN
- China
- Prior art keywords
- protective film
- film
- forming
- release
- sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000003860 storage Methods 0.000 claims abstract description 23
- 206010040844 Skin exfoliation Diseases 0.000 claims description 36
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Images
Classifications
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- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- 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
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/0007—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/06—Interconnection of layers permitting easy separation
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- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/02—Wrappers or flexible covers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
-
- 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
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- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/06—Non-macromolecular additives organic
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/068—Copolymers with monomers not covered by C09J133/06 containing glycidyl groups
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- 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
- C09J7/10—Adhesives in the form of films or foils without carriers
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- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
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- 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 subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/52—Mounting semiconductor bodies in containers
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- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/6835—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
- H01L21/6836—Wafer tapes, e.g. grinding or dicing support tapes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C09J2483/00—Presence of polysiloxane
- C09J2483/005—Presence of polysiloxane in the release coating
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- Quality & Reliability (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Dicing (AREA)
Abstract
The invention provides a method for manufacturing a sheet roll for forming a protective film, which is not easy to generate marks due to winding of a protective film forming film which brings marks to the protective film. The method for manufacturing the sheet roll for forming the protective film comprises the following steps: a step of storing a sheet roll, which is formed by winding a long sheet having a protective film forming film, a first release film provided on one surface of the protective film forming film, and a second release film provided on the other surface of the protective film forming film, at a storage temperature of 10 ℃ or less for 25 days or more from 60 days after the sheet roll is formed, wherein a relation of F1 > F2 is satisfied where a peeling force for peeling the first release film from the protective film forming film is F1 and a peeling force for peeling the second release film from the protective film forming film is F2, and a loss tangent of the protective film forming film at 10 ℃ is tan δ10Of tan delta10Is 1.2 or less.
Description
Technical Field
The present invention relates to a method for manufacturing a roll for forming a protective film. In particular, the present invention relates to a method for manufacturing a roll of protective film forming sheet, in which a mark is not easily generated due to winding of the protective film forming film, which may cause a mark to the protective film.
Background
In recent years, semiconductor devices are being manufactured by a mounting method called flip chip bonding. In this mounting method, when a semiconductor chip having a circuit surface on which convex electrodes such as bumps (bumps) are formed is mounted, the circuit surface side of the semiconductor chip is turned over (face down) and bonded to the chip mounting portion. Therefore, the semiconductor device has a structure in which the back surface side of the semiconductor chip on which no circuit is formed is exposed.
Therefore, in order to protect the semiconductor chip from impact during transportation or the like, a hard protective film made of an organic material is often formed on the back surface side of the semiconductor chip. Such a protective film is formed by curing or in a non-cured state after a protective film forming film is attached to the back surface of a semiconductor wafer, for example.
The protective film forming film and a support film supporting the protective film forming film together constitute a long protective film forming sheet. Before forming a film using the protective film, the long strip-shaped sheet is generally wound into a sheet roll. When the protective film is used to form a film, a long protective film-forming sheet unwound from a roll is cut into substantially the same shape as the semiconductor wafer to which the sheet is attached, and then the cut sheet is attached to the semiconductor wafer.
Documents of the prior art
Patent document
Patent document 1: international publication No. 2017/145735
Disclosure of Invention
Technical problem to be solved by the invention
The manufactured long protective film forming sheet is fixed to the core by using the core fixing tape, and the long protective film forming sheet is wound by a winding device while applying a predetermined tension, thereby forming a protective film forming sheet roll. As a result, stress remains in the long protective film forming sheet (protective film forming sheet roll) after winding, and a winding pressure is generated in a direction toward the core. The take-up pressure tends to be large in the protective film forming sheet near the core, that is, the protective film forming sheet at the start of winding, and small in the protective film forming sheet on the outer peripheral side of the sheet roll.
Further, there are a strongly pressed position and a slightly pressed position even in the same roll of the sheet for forming the protective film due to variations in tension at the time of winding, and there are cases where a mark (a winding mark) due to winding is formed in the sheet for forming the protective film at the strongly pressed position for a long time after winding. In particular, the take-up pressure is high at the position where the protective film forming sheet starts to be wound, and the take-up pressure tends to vary from one position to another in the width direction after winding. Further, since a step difference occurs due to the thickness of the core fixing tape and the protective film forming sheet, the take-up pressure due to the step difference becomes large, or variation in the take-up pressure is likely to occur in the width direction. Therefore, after winding, a roll mark due to a partially strong pressing is more likely to be generated in the protective film forming sheet near the core than in the protective film forming sheet on the outer peripheral side of the sheet roll. If such a roll mark occurs, a roll mark also occurs in the protective film forming film constituting the protective film forming sheet. As a result, when the protective film forming film is attached to a workpiece to form a protective film, a curl mark remains, and appearance of the protective film is deteriorated.
However, there is a problem that even if the setting conditions of the winding device are adjusted when forming the sheet roll, it is difficult to completely suppress the winding mark accompanying the deviation of the winding pressure and the like.
The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for manufacturing a roll of protective film forming sheet in which a mark is not easily generated due to winding of the protective film forming film which causes a mark to the protective film.
Means for solving the problems
The scheme of the invention is as follows.
[1] A method for manufacturing a roll of protective film-forming sheet, comprising: a step of storing a sheet roll, which is formed by winding a long sheet having a protective film forming film, a first release film provided on one surface of the protective film forming film, and a second release film provided on the other surface of the protective film forming film, at a storage temperature of 10 ℃ or lower for 25 days or longer, from 60 days after the sheet roll is formed,
when the peeling force for peeling the first peeling film from the protective film forming film is F1 and the peeling force for peeling the second peeling film from the protective film forming film is F2, the relationship of F1 > F2 is satisfied,
the loss tangent of the protective film forming film at 10 ℃ was set to tan delta10Of tan delta10Is 1.2 or less.
[2] The method for producing a roll for forming a protective film according to [1], wherein the step of storing at a storage temperature of 10 ℃ or lower is started within 10 days after the roll is formed.
[3] The method for producing a roll of protective film-forming sheet according to [1] or [2], wherein the storage temperature is-10 ℃ or higher.
[4] The method for manufacturing a roll of protective film-forming sheet according to any one of [1] to [3], wherein a surface of the first release film and/or the second release film that is not in contact with the protective film-forming film is subjected to a peeling treatment.
[5]According to [1]～[4]The method for producing a roll of protective film-forming sheet according to any one of the above claims, wherein tan δ10Is 0.04 or more.
Effects of the invention
According to the present invention, it is possible to provide a method for manufacturing a roll of protective film forming sheet in which a mark due to winding of the protective film forming film that may mark the protective film is less likely to occur.
Drawings
Fig. 1A is a schematic perspective view of an example of a roll of protective film forming sheet according to the present embodiment.
Fig. 1B is an enlarged cross-sectional view of part IB of fig. 1A.
Fig. 2 is a schematic cross-sectional view of one example of the protective film-forming sheet of the present embodiment.
Fig. 3 is a schematic cross-sectional view showing that the first and second release films have the first and second release agent layers.
Fig. 4 is a perspective view schematically showing a slit-formed long sheet unwound from a protective film-forming sheet roll according to the present embodiment.
Fig. 5A is a schematic cross-sectional view illustrating attachment of a stacked body of the protective film forming film and the first release film to the workpiece.
Fig. 5B is a schematic cross-sectional view showing that the protective film attached to the workpiece is formed into a protective film.
Description of the reference numerals
100: a protective film-forming sheet roll; 1: a protective film-forming sheet; 10: forming a film by the protective film; 20: a first release film; 21: a substrate; 22. 23: a first release agent layer; 30: a second release film; 31: a substrate; 32: a second release agent layer; 70: a core; 80: and (5) fixing the tool.
Detailed Description
Hereinafter, the present invention will be described in detail based on specific embodiments with reference to the accompanying drawings.
First, main terms used in the present specification will be described.
The workpiece is a plate-shaped body which is attached with a protective film to form a film and is to be processed. Examples of the workpiece include a wafer and a panel. Specifically, a semiconductor wafer and a semiconductor panel are exemplified. Examples of the workpiece to be processed include a wafer (single wafer) and a chip obtained by singulating the wafer. Specifically, a semiconductor wafer is singulated to obtain semiconductor chips. At this time, the protective film is formed on the back surface side of the wafer.
The "front surface" of the workpiece refers to a surface on which a circuit, a convex electrode such as a bump, or the like is formed, and the "back surface" refers to a surface on which no circuit or the like is formed.
In the present specification, for example, "(meth) acrylate" is used as a term indicating both "acrylate" and "methacrylate", and other similar terms are also used.
In the present specification, the weight ratio of the components constituting each composition is expressed as a solid content ratio.
(1. roll of protective film-forming sheet)
(1.1 form of roll for Forming protective film)
Fig. 1A shows an example of a roll of protective film-forming sheet manufactured by the manufacturing method of the present embodiment. In fig. 1A, a sheet roll 100 for forming a protective film is a roll obtained by winding a long sheet 1 for forming a protective film.
(1.2 protective film-forming sheet)
First, the long sheet will be explained. The protective film-forming sheet 1 as a long sheet is used for attaching a protective film-forming film to a workpiece. As shown in fig. 2, the protective film forming sheet 1 has a structure in which the first release film 20 is disposed on one main surface 10a of the protective film forming film 10 and the second release film 30 is disposed on the other main surface 10 b. Hereinafter, the long sheet 1 is also sometimes referred to as a protective film-forming sheet 1.
The protective film-forming sheet 1 is wound into a roll and then stored before use. The protective film forming film is supported by the first release film and the second release film formed on both main surfaces during storage.
When the protective film forming device is used, the protective film forming sheet is unwound from the protective film forming sheet roll, and the protective film forming film is cut into a predetermined shape. After the second stripping film is stripped, the protective film forming film is attached to the back of the workpiece, and the protective film is formed after the first stripping film is stripped. The protective film protects the workpiece or the workpiece to be processed.
Hereinafter, a protective film forming film, a first release film, and a second release film constituting the protective film forming sheet will be described.
(1.3 protective film Forming film)
As described above, the protective film forming film is attached to the workpiece and then formed into a protective film, thereby forming a protective film for protecting the workpiece or the workpiece to be processed.
The "protective film formation" refers to a state in which a protective film is formed to have sufficient characteristics for protecting a workpiece or a processed object of the workpiece. Specifically, when the protective film forming film is curable, "forming a protective film" means forming an uncured protective film forming film into a cured product. In other words, the protective film formed into a protective film is a cured product of the protective film forming film, which is different from the protective film forming film.
After the work is laminated on the curable protective film forming film, the protective film can be firmly adhered to the work by curing the protective film forming film, and a protective film having durability can be formed.
On the other hand, when the protective film forming film does not contain a curable component and is used in an uncured state, the protective film is formed into a protective film at the time when the protective film forming film is attached to a workpiece. In other words, the protective film forming film formed into a protective film is the same as the protective film forming film.
When high protective performance is not required, it is not necessary to cure the protective film forming film, and therefore the protective film forming film is easy to use.
In the present embodiment, the protective film forming film is preferably curable. Therefore, the protective film is preferably a cured product. Examples of the cured product include a thermal cured product and an energy ray cured product. In the present embodiment, the protective film is more preferably a thermoset.
Further, the protective film forming film preferably has adhesiveness at normal temperature (23 ℃) or exhibits adhesiveness by heating. Thus, the protective film forming film and the workpiece can be bonded together when the workpiece is stacked thereon. Therefore, positioning can be performed with certainty before curing the protective film-forming film.
The protective film forming film may be composed of one layer (single layer) or may be composed of a plurality of layers of two or more layers. When the protective film forming film has a plurality of layers, the plurality of layers may be the same as or different from each other, and the combination of the layers constituting the plurality of layers is not particularly limited.
In the present embodiment, the protective film forming film is preferably one layer (single layer). The protective film forming film of one layer can be obtained with high precision in thickness and is therefore easy to produce. Further, if the protective film forming film is composed of a plurality of layers, it is necessary to consider the adhesiveness between the layers and the stretchability of each layer, and there is a risk that peeling from the adherend occurs due to this. When the protective film is formed as one layer, the above risk can be reduced, and the degree of freedom of design can be improved.
The thickness of the protective film-forming film is not particularly limited, but is preferably less than 100 μm, 70 μm or less, 45 μm or less, and 30 μm or less. By setting the upper limit value of the thickness of the protective film forming film to the above value, the step difference due to the thickness of the protective film forming sheet at the position where winding starts can be reduced.
The thickness of the protective film forming film is preferably 5 μm or more, 10 μm or more, and 15 μm or more. When the lower limit value of the thickness of the protective film forming film is set to the above value, the performance of protecting the work is easily obtained as the protective film, and further, in the protective film forming sheet roll, the protective film forming film acts as a stress relief, and the length from the core portion at which the roll mark starts to appear can be further shortened.
The thickness of the protective film forming film is the thickness of the entire protective film forming film. For example, the thickness of the protective film forming film composed of a plurality of layers means the total thickness of all the layers constituting the protective film forming film.
(loss tangent of protective film formation film at 1.3.110 ℃ C.)
In the present embodiment, the loss tangent (tan. delta.) of the protective film forming film at 10 ℃10) Is 1.2 or less. The loss tangent is defined as "loss modulus/storage modulus" and is measured from the response to a stress applied to an object by a dynamic viscoelasticity measuring apparatusThe value of (c). When the loss tangent of the protective film forming film is within the above range at 10 ℃, the components constituting the protective film forming film become slightly elastic, and the protective film forming film is less likely to be deformed, so that there is a tendency that the roll mark is less likely to occur even when the take-up pressure of the sheet roll is high. Therefore, the present embodiment controls the loss tangent of the protective film forming film at 10 ℃.
Loss tangent (tan. delta.) of protective film forming film at 10 DEG C10) Preferably 1.0 or less, more preferably 0.9 or less, and still more preferably 0.8 or less. Further, the loss tangent (tan. delta.) of the protective film forming film at 10 ℃10) Preferably 0.04 or more, more preferably 0.1 or more, further preferably 0.2 or more, and particularly preferably 0.3 or more. By setting the lower limit value of the loss tangent of the protective film forming film at 10 ℃ to the above value, the phenomenon that the protective film forming film bent in the roll is cracked at 10 ℃ can be prevented.
Loss tangent (tan. delta.) of protective film forming film at 10 DEG C10) The measurement may be carried out by a known method. For example, a film forming the protective film may be formed into a sample having a predetermined size, a strain may be applied to the sample at a predetermined frequency in a predetermined temperature range by a dynamic viscoelasticity measuring apparatus, the elastic modulus may be measured, and the loss tangent (tan δ) at 10 ℃ may be calculated from the measured elastic modulus10). The specific measurement method will be described in detail in the examples below.
(1.4 first Release film)
The first release film is a film capable of supporting the protective film forming film in a peelable manner. In this embodiment, it is preferable that the first release film is peeled from the protective film forming film after attaching the protective film forming film to the workpiece.
The second release film may be composed of one layer (single layer) or two or more layers of the base material, and the surface of the base material may be subjected to a release treatment from the viewpoint of controlling releasability. That is, the surface of the base material may be modified, or a material not derived from the base material may be formed on the surface of the base material.
The thickness of the first release film is not particularly limited, but is preferably 30 μm to 100 μm. The thickness of the first release film is more preferably 40 μm or more, and still more preferably 45 μm or more. The thickness of the first release film is more preferably 80 μm or less, and still more preferably 70 μm or less.
When the lower limit of the thickness of the first release film is set to the above value, when a cut reaching a part of the first release film is formed using a dicing blade described later, the dicing blade can be prevented from penetrating the first release film and cutting the first release film. Further, in the sheet roll for forming a protective film, the first release film acts as a stress relief, and the length from the core portion at which the roll mark starts to appear can be further shortened.
In addition, when the protective film forming sheet is passed through a roller such as a guide roller in the apparatus before the protective film forming sheet is unwound and the protective film forming film is cut out and conveyed to the next step, the upper limit of the thickness of the first release film is set to the above value, whereby the protective film forming film can be prevented from being peeled from the first release film. Further, the step difference due to the thickness of the protective film forming sheet at the position where winding starts can be reduced.
The thickness of the first release film is the thickness of the entire first release film. For example, the thickness of the first release film composed of a plurality of layers means the total thickness of all the layers constituting the first release film.
In this embodiment, the first release film preferably has a base material and a first release agent layer. By having the first release agent layer, the physical properties of the surface of the first release film on which the first release agent layer is formed can be easily controlled.
In the protective film forming sheet of this embodiment, when the peeling force with which the first peeling film is peeled off from the protective film forming film is F1 and the peeling force with which the second peeling film is peeled off from the protective film forming film, which will be described later, is F2, F1 and F2 satisfy the relationship of F1 > F2. By satisfying such a relationship, when the second release film is removed from the protective film forming sheet, the protective film forming film 10 to be left is not removed together with the second release film, and the protective film forming film 10 is easily left on the first release film.
Thus, the first release film is a heavy release film and the second release film is a light release film.
In the present embodiment, F1 and F2 are load values measured using a tensile tester. The specific measurement method will be described in detail in the examples below.
(1.4.1 base Material)
The base material of the first release film is not particularly limited as long as it can support the protective film forming film before the protective film forming film is stuck to the workpiece, and is generally composed of a film (hereinafter referred to as "resin film") mainly made of a resin-based material.
As specific examples of the resin film, a polyethylene film, a polypropylene film, a polybutylene film, a polybutadiene film, a polymethylpentene film, a polyvinyl chloride film, a vinyl chloride copolymer film, a polyethylene terephthalate film, a polyethylene naphthalate film, a polybutylene terephthalate film, a polyurethane film, an ethylene vinyl acetate copolymer film, an ionomer resin film, an ethylene- (meth) acrylic acid copolymer film, an ethylene- (meth) acrylate copolymer film, a polystyrene film, a polycarbonate film, a polyimide film, a fluororesin film, and the like can be used. In addition, crosslinked films of these films may also be used. Further, a laminated film of these films is also possible. In the present embodiment, a polyethylene terephthalate film is preferable from the viewpoint of environmental safety, cost, and the like, and from the viewpoint of suppressing the winding-up accompanying the stretching of the base material.
The base material may contain various additives such as a colorant, a flame retardant, a plasticizer, an antistatic agent, a lubricant, and a filler in the resin film.
The thickness of the base material is not particularly limited, and is within the range of the thickness of the first release film, which can function appropriately in each step using the protective film-forming sheet. The thickness of the substrate is preferably 30 μm to 100 μm. The thickness of the base material is more preferably 40 μm or more, and still more preferably 45 μm or more. The thickness of the base material is more preferably 80 μm or less, and still more preferably 70 μm or less.
(1.4.2 first Release agent layer)
The first release agent layer imparts releasability to the first release film from the protective film forming film. The first release agent layer is not particularly limited as long as it is made of a material that can impart releasability. In this embodiment, the first release agent layer can be obtained by curing a composition for a first release agent layer containing a release agent.
In the first release film, the first release agent layer is preferably formed directly on the surface of the base material. By forming the first release agent layer directly on the surface of the substrate, the production of the first release film becomes easy, and therefore, cost reduction can be achieved.
The thickness of the first release agent layer is not particularly limited, but is preferably 30nm to 200 nm. The thickness of the first release agent layer is more preferably 50nm or more, and still more preferably 80nm or more. Further, the thickness of the first release agent layer is more preferably 180nm or less.
When the thickness of the first release agent layer is within the above range, stable release performance can be exhibited when the protective film-forming film is attached to a workpiece.
In this embodiment, it is preferable that the first release agent layer is formed on the surface of the first release film on the side of the protective film forming film, and the first release agent layer is also formed on the surface on the opposite side. That is, as shown in fig. 3, in the protective film forming sheet 1, the first release film 20 includes a base 21 and first release agent layers 22 and 23 formed on both main surfaces of the base 21. The main surface 20b of the first release film (the main surface 20b of the first release agent layer 22) is in contact with the main surface 10a of the protective film formation film. The first release agent layer 22 and the first release agent layer 23 may be composed of the same composition or different compositions.
In the sheet roll, since the long sheets 1 are stacked in the radial direction, the surface 20a of the first release film 20 not in contact with the protective film forming film 10 and the surface 30b of the second release film 30 not in contact with the protective film forming film 10 are in contact with each other. Therefore, in the first release film 20, by subjecting the surface 20a not in contact with the protective film forming film 10 to the release treatment (by forming the first release agent layer 23), the long pieces in contact are easily slid, and therefore, stabilization of the take-up pressure described later can be promoted.
(1.5 second Release film)
The second release film is a film capable of supporting the protective film forming film in a releasable manner. In the present embodiment, the second release film is preferably peeled from the protective film forming film before attaching the protective film forming film to the workpiece.
The second release film may be composed of one layer (single layer) or two or more layers of the base material, as in the first release film, and the surface of the base material may be subjected to a release treatment from the viewpoint of controlling the releasability. That is, the surface of the base material may be modified, or a material not derived from the base material may be formed on the surface of the base material.
The thickness of the second release film is not particularly limited, but is preferably 10 μm to 75 μm. The thickness of the second release film is more preferably 18 μm or more, and still more preferably 24 μm or more. The thickness of the second release film is more preferably 60 μm or less, and still more preferably 45 μm or less. From the viewpoint of making the peel force F2 and the peel force F1F 1 > F2 as described above, the thickness of the second release film is preferably equal to or less than the thickness of the first release film, and more preferably smaller than the thickness of the first release film.
The thickness of the second release film is the thickness of the entire second release film. For example, the thickness of the second release film composed of a plurality of layers means the total thickness of all the layers constituting the second release film.
In this embodiment, the second release film preferably has a base material and a second release agent layer. By having the second release agent layer, the physical properties of the surface of the second release film on which the second release agent layer is formed can be easily controlled.
(1.5.1 base Material)
The base material of the second release film can be appropriately selected from the materials exemplified as the base material of the first release film.
(1.5.2 second Release agent layer)
When the second release film has a second release agent layer, the second release agent layer is not particularly limited as long as it is made of a material capable of imparting releasability. For example, the second release agent layer can be obtained by curing a composition for the second release agent layer containing a silicone release agent, as in the first release agent layer.
In the second release film, the second release agent layer is preferably formed directly on the surface of the substrate, as in the first release film. By forming the second release agent layer directly on the surface of the substrate, production of the second release film becomes easy, and therefore cost reduction can be achieved.
In this embodiment, the second release agent layer is formed on the surface of the second release film on the protective film formation film side. That is, as shown in fig. 3, in the protective film-forming sheet 1, the second release film 30 has a base material 31 and a second release agent layer 32 formed on the surface of the base material 31 on the protective film-forming film side. The main surface 30a of the second release film 30 (the main surface 30a of the second release agent layer 32) is in contact with the main surface 10b of the protective film formation film 10. In addition, in addition to the second release agent layer formed on the surface of the second release film 30 on the protective film-forming film side, a second release agent layer may be formed on the surface 30b on the opposite side.
In addition, when the second release agent layer is formed on both main surfaces of the substrate, the second release agent layer may be formed by applying a coating agent containing a composition for the second release agent layer, which will be described later, to both main surfaces of the substrate, or the second release agent layer may be formed on a main surface not coated with the coating agent by applying a coating agent containing a composition for the second release agent layer to one main surface of the substrate, winding the substrate into a roll, and transferring a component of the composition for the second release agent layer from the main surface coated with the coating agent to the main surface not coated with the coating agent (transfer phenomenon).
(2. method for producing protective film-forming sheet roll)
In the method of manufacturing a roll of protective film forming sheet according to this embodiment, first, the protective film forming sheet having the protective film forming film, the first release film, and the second release film is manufactured as a long sheet having a length in the longitudinal direction that is much longer than a length in the short direction. The long sheet may be produced by a known method, and a specific method is as described below.
Then, the long sheet is wound by a winding device with a predetermined tension while both sides in the width direction are cut to adjust the dimension in the width direction according to the dimension of a work to which the protective film forming film is to be attached, thereby producing a protective film forming sheet roll.
Further, when the width of the work is 150mm, the length in the width direction after cutting is preferably in the range of 155 to 194mm, when the width of the work is 200mm, the length in the width direction after cutting is preferably in the range of 205 to 250mm, when the width of the work is 300mm, the length in the width direction after cutting is preferably in the range of 305 to 350mm, and when the width of the work is 450mm, the length in the width direction after cutting is preferably in the range of 455 to 500 mm.
As shown in fig. 1B, the strip sheet 1 is fixed to the core 70 via a fixing tool 80 such as a core fixing tape, and the strip sheet 1 is wound around the core 70 by a winding device while applying a predetermined tension to the strip sheet 1, thereby forming the sheet roll 100. As described above, in the wound sheet roll, a deviation in winding pressure occurs, and particularly, a winding mark of the protective film forming film, which may mark the protective film, is easily formed at a position strongly pressed in the long sheet near the core.
On the other hand, it is estimated that after the sheet roll is formed, that is, after the winding is completed, the winding pressure at a position where the winding pressure is high gradually becomes lower and approaches the winding pressure at a position where the winding pressure is low as time passes. In other words, it is estimated that the deviation of the winding pressure is eliminated with the lapse of time, and the winding pressure in the sheet roll is stabilized (averaged). Therefore, although the deviation of the winding pressure in the sheet roll is largely eliminated eventually, the winding mark formed before the deviation of the winding pressure is eliminated remains in the protective film forming film even after the deviation of the winding pressure is eliminated.
However, in the case where the loss tangent of the protective film forming film is low and the protective film forming film is not easily deformed, even if a deviation in take-up pressure occurs and there is a position strongly pressed, a take-up mark is not easily formed on the protective film forming film. Further, when the temperature is lowered, the loss tangent of the protective film formation film is easily maintained low. Further, as described above, the winding pressure in the sheet roll tends to be stabilized with the passage of time.
(2.1 storage step)
Therefore, in the present embodiment, the sheet roll immediately after winding is stored for a predetermined time until the take-up pressure is stabilized while maintaining the loss tangent of the protective film forming film within the above range.
Specifically, the method for manufacturing a roll for forming a protective film according to the present embodiment includes the steps of: loss tangent (tan delta) from formation of protective film formation film having 10 DEG C10) The sheet roll having a protective film formed of a film of 1.2 or less is wound up and stored for 60 days, and the sheet roll is stored at a storage temperature of 10 ℃ or less for 25 days or more out of 60 days.
Loss tangent (tan delta) for a protective film forming film having a temperature of 10 DEG C10) The sheet roll of the protective film forming film having a thickness of 1.2 or less is stored at a temperature of 10 ℃ or less until the take-up pressure of the sheet roll is stabilized, so that the protective film forming film easily attains a loss tangent in the above range, and therefore, the formation of a roll mark on the protective film forming film in the sheet roll can be suppressed.
The storage period of the sheet roll at a storage temperature of 10 ℃ or lower is preferably 30 days or longer, 35 days or longer, 40 days or longer, or 45 days or longer. On the other hand, the period is preferably 60 days or less and 59 days or less.
Further, the storage at the storage temperature of 10 ℃ or less is preferably started within 10 days, more preferably within 7 days, and still more preferably within 4 days after the formation of the sheet roll. Since the sheet roll immediately after winding tends to have a large variation in take-up pressure, the formation of a lap mark on the protective film forming film in the sheet roll can be further suppressed by maintaining the loss tangent of the protective film forming film at a low value.
The storage temperature is preferably-10 ℃ or higher, more preferably-5 ℃ or higher, and still more preferably 0 ℃ or higher. When the lower limit of the storage temperature is set to the above value, the elastic modulus of the protective film forming film can be suppressed from becoming too high, and peeling can be suppressed from occurring between the protective film forming film and the release film, particularly between the protective film forming film and the second release film.
Through the above-described storage step, the protective film forming sheet roll of the present embodiment can be obtained. The loss tangent tan delta at 10 ℃ is obtained by storing the protective film forming film in the above-mentioned storage step10The protective film forming sheet is 1.2 or less, and even if the protective film forming sheet is unwound from the protective film forming sheet roll, the formation of a roll mark on the protective film forming film up to the protective film forming sheet on the core side can be suppressed. Therefore, the appearance failure of the protective film is suppressed, and the roll of protective film forming sheet of the present embodiment can be used up without waste.
(2.2 method for producing Long sheet)
The method for producing the roll for forming a protective film according to the present embodiment may be a method for producing a long sheet having the above-described configuration by a known method. In this embodiment, a case where the first release film has the above-described base material and first release agent layer, and the second release film has the above-described base material and second release agent layer will be described.
The protective film forming film is formed using the composition for a protective film forming film, the first release agent layer is formed using the composition for a first release agent layer, and the second release agent layer is formed using the composition for a second release agent layer.
Hereinafter, the composition for forming a protective film, the composition for a first release agent layer, and the composition for a second release agent layer will be described.
(2.2.1 composition for Forming protective film)
The composition of the protective film forming film is not particularly limited as long as the protective film forming film has the above physical properties. In the present embodiment, the composition constituting the protective film-forming film (the composition for forming a protective film) is preferably a resin composition containing at least the polymer component (a), the curable component (B), and the filler (E). The polymer component can be considered as a component formed by a polymerization reaction of a polymerizable compound. The curable component is a component capable of undergoing a curing (polymerization) reaction. The polymerization reaction in the present invention also includes a polycondensation reaction.
Further, components contained in the polymer component may be a curable component. In the present embodiment, when the composition for forming a protective film contains such a component that belongs to both the polymer component and the curable component, it is regarded that the composition for forming a protective film contains both the polymer component and the curable component.
(2.2.1.1 Polymer component)
The polymer component (a) imparts film formability (film formability) to the protective film-forming film and provides appropriate viscosity, thereby reliably and uniformly adhering the protective film-forming film to the workpiece. The weight average molecular weight of the polymer component is usually in the range of 5 to 200 ten thousand, preferably 10 to 150 ten thousand, and particularly preferably 20 to 100 ten thousand. As such a polymer component, for example, an acrylic resin, a urethane (urethane) resin, a phenoxy resin, a silicone resin, a saturated polyester resin, or the like can be used, and an acrylic resin is particularly preferably used.
In addition, in the present specification, unless otherwise specified, "weight average molecular weight" means a polystyrene equivalent value measured by a Gel Permeation Chromatography (GPC) method. The measurement based on this method can be performed, for example, in the following manner: a high performance chromatographic column "TSK guard column H" was connected in sequence in a high performance GPC apparatus "HLC-8120 GPC" manufactured by TOSOH CORPORATIONXL-H”、“TSK Gel GMHXL”、“TSK Gel G2000 HXL"(all manufactured by TOSOH CORPORATION) at a column temperature: 40 ℃ and liquid inlet speed: under the condition of 1.0 mL/min, the detector was set as a differential refractometer.
Examples of the acrylic resin include (meth) acrylate copolymers composed of a (meth) acrylate monomer and a structural unit derived from a (meth) acrylic acid derivative. The (meth) acrylate monomer preferably includes an alkyl (meth) acrylate having an alkyl group with 1 to 18 carbon atoms, and specifically includes methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, and the like. Examples of the (meth) acrylic acid derivative include (meth) acrylic acid, glycidyl (meth) acrylate, and hydroxyethyl (meth) acrylate.
In the present embodiment, glycidyl groups are preferably introduced into the acrylic resin using glycidyl methacrylate or the like. The acrylic resin having a glycidyl group introduced therein has improved compatibility with an epoxy resin as a thermosetting component described later, and tends to easily form a protective film having stable properties. In the present embodiment, it is preferable to introduce a hydroxyl group into an acrylic resin using hydroxyethyl acrylate or the like in order to control adhesiveness to a work or adhesive properties.
The glass transition temperature of the acrylic resin is preferably-70-40 ℃, 35-35 ℃, 20-30 ℃, 10-25 ℃ and 5-20 ℃. By setting the lower limit of the glass transition temperature of the acrylic resin to the above value, tan δ of the protective film forming film can be easily reduced10. When the upper limit value of the glass transition temperature of the acrylic resin is set to the above value, the adhesion of the protective film forming film to the work is suitably improved, and the adhesion of the protective film to the work is suitably improved.
When the acrylic resin has m kinds of structural units (m is an integer of 2 or more), the glass transition temperature of the acrylic resin can be calculated as follows. That is, when m kinds of monomers from which the structural units in the acrylic resin are derived are sequentially assigned with numbers that do not overlap from 1 to m, and are named as "monomers m", the glass transition temperature (Tg) of the acrylic resin can be calculated using the Fox equation shown below.
[ mathematical formula 1]
Wherein Tg is the glass transition temperature of the acrylic resin; m is an integer of 2 or more; tgk is the glass transition temperature of a homopolymer of monomer m; wk is the mass fraction of a structural unit m derived from a monomer m in the acrylic resin, wherein Wk satisfies the following formula.
[ mathematical formula 2]
Wherein m and Wk are the same as those described above.
As Tgk, the values described in the Polymer data manual (polymers データ and ハンドブック), the adhesion manual (adhesion ハンドブック), or Polymer Handbook, etc. can be used. For example, a homopolymer of methyl acrylate is Tgk deg.C, a homopolymer of n-butyl acrylate is Tgk deg.C-54 deg.C, a homopolymer of methyl methacrylate is Tgk deg.C-105 deg.C, a homopolymer of 2-hydroxyethyl acrylate is Tgk deg.C-15 deg.C, a homopolymer of glycidyl methacrylate is Tgk deg.C 41 deg.C, and a homopolymer of 2-ethylhexyl acrylate is Tgk deg.C-70 deg.C.
The content of the polymer component is preferably 5 to 80 parts by mass, 8 to 70 parts by mass, 10 to 60 parts by mass, 12 to 55 parts by mass, 14 to 50 parts by mass, or 15 to 45 parts by mass, based on 100 parts by mass of the total weight of the composition for forming a protective film. When the content of the polymer component is in the above range, the viscosity of the protective film forming film is appropriately increased, and the adhesion between the protective film forming film and the work is appropriately increased. In addition, the occurrence of the curl mark tends to be easily suppressed.
(2.2.1.2 thermosetting Components)
The curable component (B) forms a hard coating by curing the coating film-forming film. As the curable component, a thermosetting component, an energy ray curable component, or a mixture thereof can be used. When the protective film is cured by irradiation with energy rays, the protective film contains a filler, a coloring material, and the like described later, and thus light transmittance is reduced. Therefore, for example, when the thickness of the protective film forming film is increased, the energy ray curing is likely to be insufficient.
On the other hand, a thermosetting protective film-forming film can be sufficiently cured by heating even if the film is thick, and therefore a protective film having high protective performance can be formed. Further, by using a general heating apparatus such as a heating oven, a plurality of protective film forming films can be collectively heated to be thermally cured.
Therefore, in the present embodiment, it is desirable that the curable component be thermosetting. That is, the protective film forming film is preferably thermosetting.
Whether or not the protective film forming film is thermosetting can be judged in the following manner. First, a normal temperature (23 ℃) protective film forming film is heated to a temperature exceeding the normal temperature, and then cooled to the normal temperature, to prepare a heated and cooled protective film forming film. Next, when the hardness of the heated and cooled protective film forming film is compared with the hardness of the protective film forming film before heating at the same temperature, the case where the heated and cooled protective film forming film is harder is judged as the protective film forming film being thermosetting.
As the thermosetting component, for example, epoxy resin, thermosetting polyimide resin, unsaturated polyester resin, and a mixture thereof are preferably used. The thermosetting polyimide resin is a generic name of a polyimide precursor and a thermosetting polyimide which can be thermally cured to form a polyimide resin.
An epoxy resin as a thermosetting component has a property of forming a three-dimensional network structure and forming a firm coating film when heated. As such an epoxy resin, various known epoxy resins can be used. In the present embodiment, the molecular weight (formula weight) of the epoxy resin is preferably 300 or more and less than 50000, 300 or more and less than 10000, 300 or more and less than 5000, 300 or more and less than 3000. In addition, the epoxy equivalent of the epoxy resin is preferably 50 to 5000g/eq, more preferably 100 to 2000g/eq, and further preferably 150 to 1000 g/eq.
Specific examples of the epoxy resin include glycidyl ethers of phenols such as bisphenol a, bisphenol F, resorcinol, phenyl novolac (phenyl novolac), and cresol novolac; glycidyl ethers of alcohols such as butanediol, polyethylene glycol, and polypropylene glycol; glycidyl ethers of carboxylic acids such as phthalic acid, isophthalic acid, and tetrahydrophthalic acid; glycidyl-type or alkylglycidyl-type epoxy resins obtained by substituting active hydrogen bonded to a nitrogen atom such as aniline isocyanurate (aniline isocyanurate) with a glycidyl group; vinylcyclohexane diepoxide, 3, 4-epoxycyclohexylmethyl-3, 4-bicyclohexane carboxylate, 2- (3, 4-epoxy) cyclohexyl-5, 5-spiro (3, 4-epoxy) cyclohexane-m-dioxane, and the like, so-called alicyclic epoxy oxides in which an epoxy group is introduced by, for example, oxidation or the like of a carbon-carbon double bond in a molecule. Further, an epoxy resin having a biphenyl skeleton, a dicyclohexyldiene skeleton, a naphthalene skeleton, or the like can also be used.
When a thermosetting component is used as the curable component (B), it is preferable to use the curing agent (C) together as an auxiliary. As the curing agent for epoxy resin, a heat-active latent epoxy resin curing agent is preferable. The "thermally active latent epoxy resin curing agent" refers to a type of curing agent which is not easily reacted with an epoxy resin at normal temperature (23 ℃) and is activated by heating at a certain temperature or higher to react with the epoxy resin. As a method for activating a heat-active latent epoxy resin curing agent, there are: a method of generating active species (anion, cation) using a chemical reaction based on heating; a method of stably dispersing in an epoxy resin at around normal temperature, compatibly-dissolving with the epoxy resin at high temperature and starting a curing reaction; a method of starting a curing reaction after dissolving out a molecular sieve-encapsulated type curing agent at a high temperature; microcapsule-based methods, and the like.
Among the above-mentioned methods, a method of stably dispersing in an epoxy resin at around room temperature, and starting a curing reaction by being compatible with and dissolved in the epoxy resin at high temperature is preferable.
Specific examples of the thermally active latent epoxy resin curing agent include various onium salts, dibasic acid dihydrazide compounds, dicyandiamide, amine adduct curing agents, high-melting-point active hydrogen compounds such as imidazole compounds, and the like. These heat-reactive latent epoxy resin curing agents may be used singly or in combination of two or more. Dicyandiamide is particularly preferred in this embodiment.
Further, as a curing agent for the epoxy resin, a phenol resin is also preferable. As the phenol resin, there can be used, without particular limitation, a polycondensate of a phenol such as an alkylphenol, a polyphenol, or naphthol, and an aldehyde. Specifically, phenol novolac resin, o-cresol novolac resin, p-cresol novolac resin, t-butylphenol novolac resin, dicyclopentadiene cresol resin, poly-p-vinylphenol resin, bisphenol a-type novolac resin, modified products thereof, and the like can be used.
The phenolic hydroxyl group contained in these phenolic resins can be easily subjected to addition reaction with the epoxy group of the epoxy resin by heating, and a cured product having high impact resistance can be formed.
The content of the curing agent (C) is preferably 0.01 to 30 parts by mass, 0.1 to 20 parts by mass, 0.2 to 15 parts by mass, or 0.3 to 10 parts by mass, based on 100 parts by mass of the epoxy resin. When the content of the curing agent (C) is in the above range, the protective film can easily provide the performance of protecting the work.
When dicyandiamide is used as the curing agent (C), it is more preferable to use the curing accelerator (D) together. As the curing accelerator, imidazoles (imidazoles in which one or more hydrogen atoms are substituted with a group other than a hydrogen atom) such as 2-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 2-phenyl-4-dimethyloimidazole, 2-phenyl-4, 5-dimethyloimidazole and 2-phenyl-4-methyl-5-hydroxymethylimidazole are preferable. Among them, 2-phenyl-4, 5-dimethylol imidazole is particularly preferable.
The content of the curing accelerator is preferably 0.01 to 30 parts by mass, 0.1 to 20 parts by mass, 0.2 to 15 parts by mass, or 0.3 to 10 parts by mass, based on 100 parts by mass of the epoxy resin. When the content of the curing accelerator (D) is within the above range, the protective film can easily provide the performance of protecting a workpiece.
The total content of the thermosetting component and the curing agent is preferably 3 to 80 parts by mass, 5 to 60 parts by mass, 7 to 50 parts by mass, 9 to 40 parts by mass, or 10 to 30 parts by mass, based on 100 parts by mass of the total weight of the protective film forming composition. When the thermosetting component and the curing agent are blended in such a ratio, the performance of protecting the work as a protective film can be easily obtained.
(2.2.1.3 energy ray-curable component)
When the curable component (B) is an energy ray-curable component, the energy ray-curable component is preferably uncured, preferably adhesive, and more preferably uncured and adhesive.
The energy ray-curable component is a component that is cured by irradiation with an energy ray, and is a component for imparting film formability, flexibility, and the like to the protective film.
As the energy ray-curable component, for example, a compound having an energy ray-curable group is preferable. Examples of such a compound include known compounds.
(2.2.1.4 Filler)
By incorporating the filler (E) into the protective film forming film, the thermal expansion coefficient of the protective film obtained by forming the protective film forming film into a protective film can be easily adjusted. By making the thermal expansion coefficient close to that of the workpiece, the adhesion reliability with the workpiece is further improved. Further, by incorporating the filler (E) into the protective film forming film, a hard protective film can be easily obtained to obtain a performance of protecting a work, and the moisture absorption rate of the protective film can be reduced.
The filler (E) may be either an organic filler or an inorganic filler, and is preferably an inorganic filler in view of shape stability at a high temperature such as 260 ℃.
Examples of preferable inorganic fillers include powders of silica, alumina, talc, calcium carbonate, red iron oxide, silicon carbide, boron nitride, and the like; beads obtained by spheroidizing these inorganic fillers; surface modifications of these inorganic filler materials; single crystal fibers of these inorganic filler materials; glass fibers, and the like. Among them, silica and surface-modified silica are preferable. The surface-modified silica is preferably surface-modified with a coupling agent, and more preferably surface-modified with a silane coupling agent.
The average particle size of the filler is preferably 0.02 to 10 μm, 0.05 to 5 μm, or 0.10 to 3 μm.
When the average particle diameter of the filler is in the above range, the workability of the composition for forming a protective film is improved. As a result, the composition for forming a protective film and the quality of the protective film-forming film are easily stabilized.
In addition, unless otherwise specified, "average particle diameter" in the present specification means a value of a particle diameter (D50) at a cumulative value of 50% in a particle size distribution curve obtained by a laser diffraction scattering method.
The content of the filler is preferably 15 to 80 parts by mass, 30 to 75 parts by mass, 40 to 70 parts by mass, or 45 to 65 parts by mass, based on 100 parts by mass of the total weight of the composition for forming a protective film.
By setting the lower limit of the content of the filler to the above value, tan δ which is easy to reduce the formation of the protective film can be obtained10The tendency of (c). When the upper limit of the content of the filler is set to the above value, the adhesion between the protective film forming film and the work tends to be improved, and the adhesion between the protective film and the work tends to be appropriately improved.
(2.2.1.5 coupling agent)
The protective film-forming film preferably contains a coupling agent (F). By containing the coupling agent, after the protective film forming film is cured, the adhesion between the protective film and the work can be improved without impairing the heat resistance of the protective film, and the water resistance (moist heat resistance) can be improved. As the coupling agent, a silane coupling agent is preferable from the viewpoint of its versatility and cost advantage.
Examples of the silane coupling agent include gamma-glycidyloxypropyltrimethoxysilane, gamma-glycidyloxypropylmethyldiethoxysilane, beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, gamma- (methacryloyloxypropyl) trimethoxysilane, gamma-aminopropyltrimethoxysilane, N-6- (aminoethyl) -gamma-aminopropylmethyldiethoxysilane, N-phenyl-gamma-aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane, gamma-mercaptopropyltrimethoxysilane, gamma-mercaptopropylmethyldimethoxysilane, bis (3-triethoxysilylpropyl) tetrasulfide, gamma-glycidyloxypropyltrimethoxysilane, gamma-glycidyloxypropylmethyldimethoxysilane, gamma-glycidyloxypropyltrimethoxysilane, gamma-hydroxysilane, beta-hydroxysilane, and the like-hydroxysilane, Methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriacetoxysilane, imidazolesilane and the like. These silane coupling agents may be used singly or in combination of two or more.
(2.2.1.6 colorant)
The protective film forming film preferably contains a colorant (G). Therefore, the back surface of the workpiece such as a chip can be shielded, various electromagnetic waves generated in the electronic device can be blocked, and the malfunction of the workpiece such as a chip can be reduced.
As the colorant (G), for example, known pigments such as inorganic pigments, organic pigments, and organic dyes can be used. In the present embodiment, inorganic pigments are preferable.
Examples of the inorganic pigments include carbon black, cobalt pigments, iron pigments, chromium pigments, titanium pigments, vanadium pigments, zirconium pigments, molybdenum pigments, ruthenium pigments, platinum pigments, ITO (indium tin oxide) pigments, ATO (antimony tin oxide) pigments, and the like. Among them, carbon black is particularly preferably used. In the case of carbon black, electromagnetic waves in a wide wavelength range can be blocked.
The amount of the colorant (particularly carbon black) to be blended in the protective film-forming film may vary depending on the thickness of the protective film-forming film, and when the thickness of the protective film-forming film is 20 μm, for example, the amount of the colorant to be blended is preferably 0.01 to 10 mass%, 0.04 to 7 mass%, or 0.07 to 4 mass% with respect to the total mass of the protective film-forming film. When the amount of the colorant is within the above range, the trace of the protective film due to the rolling mark of the roll of the protective film-forming sheet tends to be inconspicuous in appearance.
The average particle diameter of the colorant (especially carbon black) is preferably 1 to 500nm, particularly preferably 3 to 100nm, and further preferably 5 to 50 nm. When the average particle diameter of the colorant is within the above range, the light transmittance can be easily controlled to a desired range.
(2.2.1.7 other additives)
The protective film-forming composition may further contain, for example, a photopolymerization initiator, a crosslinking agent, a plasticizer, an antistatic agent, an antioxidant, a gettering agent, a tackifier, a release agent, and the like as other additives within a range not to impair the effects of the present invention.
(2.2.2 composition for first Release agent layer)
In the present embodiment, the composition for the first release agent layer may contain, for example, an alkyd-based release agent, a silicone-based release agent, a fluorine-based release agent, an unsaturated polyester-based release agent, a polyolefin-based release agent, and a wax-based release agent, and among them, a silicone-based release agent is preferably contained. When the composition for the first release agent layer contains a silicone release agent, the composition preferably contains a silicone release agent and a heavy release additive.
(2.2.2.1 Silicone-based Release agent)
As the silicone-based mold release agent, a silicone mold release agent in which silicone having dimethylpolysiloxane as a basic skeleton is blended can be used.
The content of the silicone composed of dimethylpolysiloxane is preferably less than 100 parts by mass, less than 90 parts by mass, less than 80 parts by mass, or less than 70 parts by mass, based on 100 parts by mass of the total weight of the composition for the first release agent layer (excluding a catalyst described later).
The silicone may be any of an addition reaction type, a polycondensation reaction type, and an energy ray curing type such as an ultraviolet curing type and an electron beam curing type, and is preferably an addition reaction type silicone. Addition reaction type silicone has high reactivity and excellent productivity, and has advantages such as less change in peeling force after production and no curing shrinkage as compared with polycondensation type silicone.
Specific examples of the addition reaction type silicone include organopolysiloxanes having 2 or more alkenyl groups having 2 to 10 carbon atoms such as vinyl, allyl, propenyl, and hexenyl groups at the end and/or side chain of the molecule.
When such an addition reaction type silicone is used, it is preferable to use a crosslinking agent and a catalyst together.
Examples of the crosslinking agent include an organopolysiloxane having at least 2 hydrogen atoms bonded to silicon atoms in 1 molecule.
Specific examples of the crosslinking agent include dimethylhydrogensiloxy end-blocked dimethylsiloxane-methylhydrogensiloxane copolymer, trimethylsiloxy end-blocked methylhydrogensiloxane, poly (hydrogensilsesquioxane), and the like.
Examples of the catalyst include platinum group metal compounds such as fine particulate platinum, fine particulate platinum adsorbed on a carbon powder carrier, chloroplatinic acid, alcohol-modified chloroplatinic acid, olefin complexes of chloroplatinic acid, palladium, and rhodium.
By using the catalyst, the curing reaction of the composition for the first release agent layer can be more effectively performed.
From the viewpoint of the peeling force F1 being within the above range, the content of the silicone-based release agent is preferably 30 to 100 parts by mass, and 50 to 100 parts by mass, based on 100 parts by mass of the total weight of the composition for the first release agent layer (excluding the catalyst).
(2.2.2.2.2 heavy Release additives)
The heavy release additive is used to increase the release force F1 of the first release film from the protective film forming film. Examples of the heavy release additive include organic silanes such as silicone resins and silane coupling agents, and among them, silicone resins are preferably used.
As the silicone resin, for example, those containing siloxane units [ R ] as monofunctional groups are preferably used3SiO1/2]With as tetrafunctional siloxane units [ SiO ]4/2]The MQ resin of Q unit of (1). In addition, 3R in the M unit each independently represent a hydrogen atom, a hydroxyl group, or an organic group. From the viewpoint of easily suppressing the silicone transfer, 1 or more of 3R in the M unit is preferably a hydroxyl group or a vinyl group, and more preferably a vinyl group.
The content of the heavy release additive is preferably 0 to 50 parts by mass, 5 to 45 parts by mass, or 10 to 40 parts by mass, based on 100 parts by mass of the total weight of the composition for a first release agent layer (excluding the catalyst).
In addition, when the first release agent layer is formed on both main surfaces of the substrate, the first release agent layer may be formed by applying a coating agent containing a composition for the first release agent layer, which will be described later, to both main surfaces of the substrate, or the first release agent layer may be formed on a main surface to which the coating agent is not applied by utilizing a phenomenon (transfer phenomenon) in which a component of the composition for the first release agent layer is transferred from a main surface to which the coating agent is applied to a main surface to which the coating agent is not applied by winding the substrate to form a roll after applying the coating agent containing the composition for the first release agent layer to one main surface of the substrate.
In the first release film, whether or not the substrate has been subjected to the release treatment can be determined, for example, as described below. When the first release agent layer contains the silicone-based release agent described above, both main surfaces of the first release film are subjected to surface analysis by X-ray photoelectron spectroscopy (XPS), the ratio of silicon atoms is calculated from the obtained spectrum, and if the ratio is equal to or greater than a predetermined value, it is determined that the release treatment has been performed. The specific measurement method will be described in detail in the examples below.
When the substrate is made of a polyethylene terephthalate film, contact angles of water are measured with respect to both main surfaces of the first release film, and when the contact angles are equal to or larger than a predetermined value, it is determined that the peeling treatment has been performed. The specific measurement method will be described in detail in the examples below.
(2.2.3 composition for second Release agent layer)
The second composition for a release agent layer can be selected from the materials exemplified in the first composition for a release agent layer, as long as the relationship between F1 and F2 is satisfied. Among them, the content of the material exemplified as the heavy release additive is preferably less than the content in the composition for the first release agent layer or is not contained.
In addition, the composition for the first release agent layer and the composition for the second release agent layer may contain a commonly used additive in the release agent layer within a range not to impair the effects of the present invention. Examples of such additives include dyes and dispersants.
Further, from the viewpoint of adjusting the peeling force to be low and the viewpoint of making it easier to form the release agent layer utilizing the transfer phenomenon, silicone oil may be added to the composition for a release agent layer (composition for a first release agent layer and composition for a second release agent layer).
(2.2.4 Process for producing Long sheet)
When the long sheet is produced, first, the composition for forming the protective film, the composition for the first release agent layer, and the composition for the second release agent layer are prepared. In the present embodiment, it is preferable to prepare a coating agent in which the composition for forming a protective film and the composition for a release agent layer, each containing the above components, are diluted with a diluent solvent from the viewpoint of adjusting the viscosity and improving the coatability.
Examples of the diluting solvent include aromatic hydrocarbons such as toluene, fatty acid esters such as ethyl acetate, ketones such as methyl ethyl ketone, and organic solvents such as aliphatic hydrocarbons such as hexane and heptane. These diluting solvents may be used alone or in combination of two or more.
The solid content concentration of the coating agent comprising the composition for forming a protective film is preferably 20 to 80% by mass, and more preferably 30 to 70% by mass. On the other hand, the coating agent containing the composition for the first release agent layer and the composition for the second release agent layer preferably has a solid content concentration of 0.3 to 10% by mass, more preferably 0.5 to 5% by mass, and still more preferably 0.5 to 3% by mass.
In this embodiment, a coating agent containing the composition for the first release agent layer is applied to one surface of the base material by a known method, and then the coating film is dried and cured to form the first release agent layer. Thereby obtaining a first release film. The second release film can also be produced in the same manner.
When the release agent layer is formed on both main surfaces of the substrate, a coating agent of the composition for the release agent layer may be applied to the other surface of the substrate. Alternatively, it may be formed in the following manner: the first release film formed by applying the coating agent of the composition for a release agent layer is wound into a roll, and during storage at 30 ℃ for 7 days or the like, for example, the components of the composition for a release agent layer are transferred to the other surface by utilizing the transfer phenomenon described above.
In this embodiment, a coating agent containing the composition for forming a protective film is applied to the first release agent layer of the first release film or the second release agent layer of the second release film by a known method, and then heated and dried to form a coating film. Next, a second release agent layer of a second release film or a first release agent layer of a first release film is laminated on the coating film, thereby producing a protective film-forming sheet (strip sheet). In the present embodiment, from the viewpoint of making the peeling force F1 within the above range and from the viewpoint of making F1 > F2, it is preferable that the coating agent comprising the composition for forming a protective film is applied to the first release agent layer of the first release film, not to the second release agent layer.
Examples of the coating method of the coating agent containing each composition include spin coating, spray coating, bar coating, blade coating, roll blade coating, die coating, and gravure coating.
(3. method for manufacturing device)
As an example of a method for manufacturing an apparatus using a roll of protective film-forming sheet manufactured by the method of the present embodiment, a method for manufacturing a chip with a protective film obtained by processing a wafer on which a protective film-forming film is attached will be described.
First, as shown in fig. 4, the strip sheet 1 is unwound from the protective film forming roll 100, and a slit 40 that penetrates the second release film 30 and the protective film forming film 10 and reaches a part of the first release film 20 is formed in the strip sheet by using a dicing blade 50. By removing the second release film and the unnecessary protective film forming film from the long sheet in which the slits 40 are formed, a circular protective film forming film can be obtained.
Next, as shown in fig. 5A, the circular protective film forming film 11 is attached to the back surface 60B of the wafer 60 as a workpiece, and as shown in fig. 5B, the first release film 20 is peeled from the laminate and the protective film forming film 11 is formed into a protective film to form the protective film 15. Then, the wafer with the protective film is singulated to obtain chips with the protective film. In addition, the wafer may be singulated and then subjected to protective film formation.
Since the formation of the curl mark on the protective film formation film can be suppressed, the mark is also suppressed on the surface of the protective film. Therefore, the chip with the protective film can be obtained, wherein appearance defects of the protective film are suppressed.
(4. modification)
Fig. 3 shows the following constitution: in the first release film 20, the first release agent layer 23 is formed on the surface 20a not in contact with the protective film forming film 10, and in the second release film 30, the second release agent layer is not formed on the surface 30b not in contact with the protective film forming film 10, but the present embodiment is not limited to this configuration.
For example, the following configuration is also possible: in the first release film, a first release agent layer is formed on a surface not in contact with the protective film forming film, and in the second release film, a second release agent layer is formed on a surface not in contact with the protective film forming film. Further, the following configuration is also possible: in the first release film, the first release agent layer is not formed on the surface not in contact with the protective film forming film, and in the second release film, the second release agent layer is formed on the surface not in contact with the protective film forming film.
In fig. 4, the slit for forming the protective film forming film to be attached to the workpiece is circular, but may have another shape as long as it is a closed shape. Examples of the other shapes include a polygon such as a triangle, and an ellipse. Further, it is preferable that the closed shape corresponds to the shape of the workpiece.
While the embodiments of the present invention have been described above, the present invention is not limited to the above embodiments and can be modified in various ways within the scope of the present invention.
Examples
The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples.
(preparation of first Release film)
First, in order to prepare the composition for the first release agent layer, the following ingredients were prepared.
(alpha) silicone release agent
[ alpha ] -1 ] Silicone-based mold release agent containing organopolysiloxane having vinyl groups and organopolysiloxane having hydrosilyl groups (manufactured BY Dow Corning Toray Co., Ltd., BY24-561, solid content 30 mass%)
(alpha-2) Dimethylpolysiloxane (manufactured by Shin-Etsu Chemical Co., Ltd., trade name: X-62-1387, weight average molecular weight: 2000)
(beta) Silicone resins
MQ resin having vinyl group (SD-7292, manufactured by Dow Corning Toray Co., Ltd., solid content 71 mass%)
(gamma) catalyst
Platinum (Pt) catalyst (manufactured by Dow Corning Toray Co., Ltd., SRX-212, solid content 100% by mass)
Next, 67.5 parts by mass (solid content ratio) (. alpha. -1), 2.5 parts by mass (solid content ratio) (. alpha. -2), 30 parts by mass (solid content ratio) (. beta.) and 6.7 parts by mass (solid content ratio) (. gamma.) were blended and mixed, and diluted with a mixed solvent of toluene and methyl ethyl ketone (toluene/methyl ethyl ketone: 1/1 (mass ratio)) so that the solid content concentration was 2% by mass, to prepare a coating agent including the first stripper layer composition.
A coating agent containing the prepared composition for forming a first release agent layer was applied to both main surfaces of a PET film (product name: DIAFOIL (registered trademark) T-100, thickness: 50 μm, manufactured by Mitsubishi Chemical Corporation) as a substrate so that the film thickness after heating and drying was 0.15 μm, and a first release agent layer was formed on both main surfaces of the PET film to prepare a first release film.
(preparation of second Release film)
As the second release film, a film having one surface of a PET film subjected to a release treatment ("SP-PET 381031" manufactured by Lintec Corporation, 38 μm in thickness) was used.
(production of protective film Forming film)
The following components were mixed at the blending ratios (in terms of solid content) shown in table 1, and diluted with methyl ethyl ketone so that the solid content concentration was 50 mass%, to prepare a coating agent containing the composition for forming a protective film.
(A) Polymer component
(A-1) A (meth) acrylic ester copolymer (weight-average molecular weight: 80 ten thousand, glass transition temperature: -28 ℃ C.) obtained by copolymerizing 55 parts by mass of n-butyl acrylate, 10 parts by mass of methyl acrylate, 20 parts by mass of glycidyl methacrylate, and 15 parts by mass of 2-hydroxyethyl acrylate
(A-2) a (meth) acrylic ester copolymer (weight-average molecular weight: 50 ten thousand, glass transition temperature: -9 ℃ C.) obtained by copolymerizing 27 parts by mass of n-butyl acrylate, 38 parts by mass of methyl acrylate, 20 parts by mass of glycidyl methacrylate, and 15 parts by mass of 2-hydroxyethyl acrylate
(B) Curing component (thermosetting component)
(B-1) bisphenol A epoxy resin (manufactured by Mitsubishi Chemical Corporation, jER828, epoxy equivalent 184 to 194g/eq)
(B-2) acrylate rubber Fine particles dispersed bisphenol A type liquid epoxy resin (NIPPON SHOKUBAI CO., LTD., manufactured by BPA328, epoxy equivalent 230g/eq, acrylate rubber content 20phr)
(B-3) Dicyclopentadiene-based epoxy resin (EPICLON HP-7200HH, softening point 88-98 ℃ C., epoxy equivalent 255-260 g/eq)
(C) Curing agent: dicyandiamide (manufactured by Mitsubishi Chemical Corporation, DICY7)
(D) Curing accelerator: 2-phenyl-4, 5-dimethylol imidazole (manufactured by SHIKOKU CHEMICALS CORPORATION, CURIZOL 2PHZ)
(E) Filling materials: epoxy-modified spherical silica Filler (SC 2050MA, average particle diameter 0.5 μm, manufactured by Admatechs Co., Ltd.)
(F) Silane coupling agent: gamma-glycidyl Ether oxypropyltrimethoxysilane (Shin-Etsu Chemical Co., Ltd., KBM403, methoxy equivalent 12.7mmol/g, molecular weight 236.3)
(G) Colorant: carbon black (manufactured by Mitsubishi Chemical Corporation, MA600B, average particle diameter 28nm)
The coating agent containing the prepared composition for forming a protective film was applied to the surface of the first release film on which the first release agent layer was formed, and dried at 100 ℃ for 2 minutes to form a protective film forming film having a thickness of 20 μm. Next, the surface of the prepared second release film on which the second release agent layer is formed is attached to the protective film forming film, thereby obtaining a protective film forming sheet (a structure of first release film/protective film forming film/second release film) in which the first release film is formed on one main surface of the protective film forming film and the second release film is formed on the other main surface. The attaching conditions were 60 ℃ temperature, 0.4MPa pressure, and 1 m/min speed.
(preparation of roll sheet)
The obtained sheet for forming a protective film was cut into a width of 320mm by using a biaxial winding slitter (manufactured by TOIZAKI BUSSAN co., ltd.) while the cut sheet for forming a protective film was wound in a roll shape on a hollow plastic core (core) having a width (320mm) equal to the width of the cut sheet for forming a protective film and a diameter of 3 inches via a core fixing tape having a width of 5mm and a thickness of 40 μm. The winding condition is a condition that an ammeter of a magnetic particle brake for controlling tension at the time of winding shows 0.25A. The length of the wound sheet for forming a protective film was 50 m. The cutting speed was 5 m/min.
The wound sheet for forming a protective film (examples 1 to 3 and comparative examples 1 to 2) was stored under the following storage conditions (modes 1 to 4), thereby obtaining a roll of the sheet for forming a protective film.
In mode 1, after being left to stand at 23 ℃ for 3 days after winding, it was left to stand at 5. + -. 4 ℃ for 40 days, and then left to stand at 23 ℃ for 17 days again (example 1 and comparative example 1). In mode 2, after being left to stand at 23 ℃ for 3 days from the time of winding, it was left to stand at 5. + -. 4 ℃ for 50 days, and then left to stand at 23 ℃ for 7 days again (example 2). In mode 3, after being left to stand at 23 ℃ for 3 days from the time of winding, it was left to stand at 5. + -. 4 ℃ for 30 days and then left to stand at 23 ℃ for 27 days again (example 3). In mode 4, the sheet was left standing at 23 ℃ for 60 days from the time of winding (comparative example 4).
Subsequently, the following measurement and evaluation were performed.
(loss tangent tan. delta. of protective film formation film at 10 ℃10)
The first release film and the second release film were peeled from the prepared protective film-forming sheet, and a plurality of protective film-forming films were laminated to form a laminate of protective film-forming films having a thickness of 200 μm ± 20 μm. The laminate was cut to a width of 4mm to obtain a measurement sample.
With respect to the above-mentioned measurement sample, tan. delta. of the measurement sample at-20 ℃ to 50 ℃ was measured in a tensile mode under the measurement conditions of a frequency of 11Hz, an inter-chuck distance of 15mm and a temperature rise rate of 3 ℃/min using a viscoelasticity measuring apparatus ("RHEOVBRON DDV-01 FP" manufactured by Ltd., Ltd.), and from these values, loss tangent tan. delta. at 10 ℃ was calculated10. The measurement results of the samples of examples 1 to 3 and comparative examples 1 and 2 are shown in table 1.
(evaluation of Presence or absence of peeling treatment of peeling film)
From the obtained sheet roll, the protective film-forming sheet was unwound, and 3 portions of 50mm × 50mm of the protective film-forming sheet were cut in the width direction at a position 1m from the initial portion of the protective film-forming sheet fixed to the plastic core by the core fixing tape.
The first release film and the second release film were peeled from the cut protective film-forming sheet, and XPS measurement was performed on the surface of the first release film that was not bonded to the protective film-forming film under the following conditions. Similarly, XPS measurement was performed on the surface of the second release film not bonded to the protective film formation film under the following conditions. XPS measurements were performed 1 time for each of 3 first release films and 3 second release films obtained by cutting the protective film-forming sheet.
XPS device: QuanteraSXM manufactured by ULVAC-PHI, INCORPORATED
X-ray: AlK alpha (1486.6eV)
Taking out the angle: 45 degree
And (3) measuring elements: silicon (Si), carbon (C), oxygen atom (O)
From the obtained measurement results, the following silicon atom ratios were calculated from the amounts of the respective measurement elements (XPS counts) of the first release film and the second release film, respectively, and the average values thereof were calculated.
Silicon atom ratio (% by atom) [ (amount of Si element)/[ (amount of C element) + (amount of O element) + (amount of Si element) ] ] × 100
Based on the obtained average value, evaluation was performed using the following criteria. The cases of determination a and determination B were determined to have undergone the peeling process. The measurement results of the samples of examples 1 to 3 and comparative examples 1 and 2 are shown in table 1.
And (3) judging A: at least one of the first and second release films has an average value of 1.0 atomic% or more
And B, judgment: not satisfying the determination A, and the average value of at least one of the first and second release films is 0.1 atomic% or more and less than 1.0 atomic%
And C, judgment: the average value of the first and second release films is less than 0.1 atom%
A first release film before coating of a coating agent containing the protective film forming film composition was prepared, and 3 cuts were made in the width direction from the first release film in a size of 50mm × 50 mm. Using the XPS apparatus, the presence or absence of the peeling treatment was evaluated under the same conditions as described above on the surface of the first release film on which the coating agent containing the composition for forming a protective film was to be applied, out of the two main surfaces. As a result, it was confirmed that the average value of the silicon atom ratio at 3 points was 1.0 atomic% or more for the sample of the first release film.
A second release film before being attached to the protective film forming film was prepared, and 3 portions were cut out in the width direction from the second release film in a size of 50mm × 50 mm. Using the XPS apparatus, the presence or absence of the peeling treatment was evaluated on the surface to be bonded to the protective film formation film of the two main surfaces of the second peeling film under the same conditions as described above. As a result, it was confirmed that the average value of the silicon atom ratio at 3 points was 1.0 atomic% or more for the sample of the second release film.
(evaluation of Water contact Angle of Release film)
From the obtained sheet roll, the protective film-forming sheet was unwound, and 3 portions of 50mm × 50mm of the protective film-forming sheet were cut in the width direction at a position 1m from the initial portion of the protective film-forming sheet fixed to the plastic core by the core fixing tape.
The first release film and the second release film were peeled from the cut protective film-forming sheet, and the contact angle of water was measured under the following conditions for the surface of the first release film that was not bonded to the protective film-forming film. Similarly, the contact angle of water was measured for the surface of the second release film that was not bonded to the protective film formation film under the following conditions. The contact angle of water was measured 5 times for each of 3 first release films and 3 second release films obtained by cutting the protective film-forming sheet.
Contact angle measuring apparatus: fully automatic contact Angle apparatus DM-701 manufactured by Kyowa Interface Science, Inc
The dropping amount is as follows: 2 μ L
Environment: the temperature is 23 ℃ and the humidity is 50%
The average value of the measurement results obtained for each of the first release film and the second release film was calculated. Based on the obtained average value, evaluation was performed using the following criteria. The case of determination a is determined to have undergone the peeling process. The measurement results of the samples of examples 1 to 3 and comparative examples 1 and 2 are shown in table 1.
And (3) judging A: at least one of the first and second release films has an average value of 78 or more
And C, judgment: the average value of the first and second release films is 77 or less
(peeling force F1 for peeling the first release film from the protective film-forming film)
The second release film was peeled from the obtained protective film-forming sheet. A laminate sample was produced by attaching a good adhesive surface of a good adhesive PET (TOYOBO co., ltd., PET25A-4100) having a thickness of 25 μm to the surface of the protective film forming film exposed by peeling, by heat lamination (70 ℃, 1 m/min). The laminate sample was cut into a width of 100mm to prepare a sample for measurement. The back surface of the first release film of the measurement sample was fixed to the hard support plate with a double-sided tape.
The protective film-forming film/well-bonded PET composite (integrated type) body was peeled from the first release film at a measurement distance of 100mm, a peel angle of 180 °, and a peel speed of 1 m/min using a universal type tensile tester (manufactured by Shimadzu Corporation, product name "AUTOGRAPH (registered trademark) AG-IS"), and the load at this time was measured. The average value of the loads between 80mm excluding the first 10mm load and the last 10mm load of the measurement distance among the measured loads was taken as the peel force F1.
(peeling force for peeling the second peeling film from the protective film forming film F2)
The obtained protective film-forming sheet was cut into a width of 100mm to prepare a sample for measurement. The back surface of the first release film of the measurement sample was fixed to the hard support plate with a double-sided tape.
The second release film was peeled from the sample for measurement at a measurement distance of 100mm, a peel angle of 180 ° and a peel speed of 1 m/min using a universal type tensile tester (manufactured by Shimadzu Corporation, product name "AUTOGRAPH (registered trademark) AG-IS"), and the load at this time was measured. The average value of the loads between 80mm excluding the first 10mm load and the last 10mm load of the measurement distance among the measured loads was taken as the peel force F2.
The obtained peel forces F1 and F2 were compared, and it was confirmed that F1 was larger than F2 in all the samples.
(evaluation of curl marks)
The long sheet was unwound from the outermost layer at a speed of 3 m/min from a roll of protective film-forming sheet after 60 days of storage, and the "length from the core" at which the occurrence of a curl mark outside the allowable range was started was measured. Whether the roll mark is outside the allowable range is checked by 5 judges with the naked eye, and if the roll mark is outside the allowable range, the roll mark is judged to be outside the allowable range. The evaluation results of the samples of examples 1 to 3 and comparative examples 1 and 2 are shown in Table 1.
And (3) judging A: more than 0m and less than 4m
And B, judgment: more than 4m and less than 6 m
And C, judgment: more than 6 m and less than 8 m
And D, judgment: over 8 m and less than 10m
And E, judgment: over 10m
[ Table 1]
From table 1, it was confirmed that the loss tangent (tan δ) of the protective film forming film at 10 ℃10) When the storage condition of the rolled sheet roll for forming the protective film is 1.2 or less and the above condition is satisfied, the formation of a roll mark on the protective film forming film in the sheet roll for forming the protective film is suppressed.
Claims (5)
1. A method for manufacturing a roll of protective film-forming sheet, comprising: a step of storing a sheet roll, which is formed by winding a long sheet having a protective film forming film, a first release film provided on one surface of the protective film forming film, and a second release film provided on the other surface of the protective film forming film, at a storage temperature of 10 ℃ or lower for 25 days or longer, in 60 days from the formation of the sheet roll,
a relationship of F1 > F2 is satisfied where F1 is a peeling force for peeling the first release film from the protective film forming film and F2 is a peeling force for peeling the second release film from the protective film forming film,
the loss tangent of the protective film forming film at 10 ℃ is set to tan delta10Of tan delta10Is 1.2 or less.
2. The method for manufacturing a protective film-forming sheet roll according to claim 1, wherein the step of storing the sheet roll at a storage temperature of 10 ℃ or lower is performed within 10 days after the sheet roll is formed.
3. The method for manufacturing a roll of protective film-forming sheet according to claim 1 or 2, wherein the storage temperature is-10 ℃ or higher.
4. The method for manufacturing a roll of protective film-forming sheet according to any one of claims 1 to 3, wherein a surface of the first release film and/or the second release film that is not in contact with the protective film-forming film is subjected to a peeling treatment.
5. A method for producing a roll of protective film-forming sheet according to any one of claims 1 to 4, wherein tan δ10Is 0.04 or more.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2020-136455 | 2020-08-12 | ||
| JP2020136455A JP7448442B2 (en) | 2020-08-12 | 2020-08-12 | Manufacturing method of sheet roll for forming protective film |
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| CN114075413A true CN114075413A (en) | 2022-02-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110737442.4A Pending CN114075413A (en) | 2020-08-12 | 2021-06-30 | Method for manufacturing protective film forming sheet roll |
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| JP (1) | JP7448442B2 (en) |
| KR (1) | KR20220020769A (en) |
| CN (1) | CN114075413A (en) |
| TW (1) | TW202218868A (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009256458A (en) | 2008-04-16 | 2009-11-05 | Hitachi Chem Co Ltd | Pressure-sensitive adhesive sheet and method for manufacturing semiconductor device |
| JP4956560B2 (en) | 2009-01-14 | 2012-06-20 | 古河電気工業株式会社 | Wafer processing tape roll packaging method |
| JP2012044193A (en) | 2011-09-15 | 2012-03-01 | Toray Ind Inc | Adhesive sheet for semiconductor device, component for semiconductor device and semiconductor device using the same |
| JP2016111165A (en) | 2014-12-04 | 2016-06-20 | 古河電気工業株式会社 | Tape for wafer processing |
| JP2017145735A (en) | 2016-02-17 | 2017-08-24 | 日立オートモティブシステムズ株式会社 | Control device for internal combustion engine and warming-up method for exhaust emission control catalyst |
| MY186890A (en) | 2016-02-24 | 2021-08-26 | Lintec Corp | Adhesive sheet and usage method therefor |
| JP6852030B2 (en) | 2018-09-25 | 2021-03-31 | 古河電気工業株式会社 | Electronic device packaging tape |
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2020
- 2020-08-12 JP JP2020136455A patent/JP7448442B2/en active Active
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| Publication number | Publication date |
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| JP7448442B2 (en) | 2024-03-12 |
| JP2022032572A (en) | 2022-02-25 |
| TW202218868A (en) | 2022-05-16 |
| KR20220020769A (en) | 2022-02-21 |
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