TWI546532B - A method of selecting a separator and an adhesive sheet using the separator selected by the selected method - Google Patents
A method of selecting a separator and an adhesive sheet using the separator selected by the selected method Download PDFInfo
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- TWI546532B TWI546532B TW101121209A TW101121209A TWI546532B TW I546532 B TWI546532 B TW I546532B TW 101121209 A TW101121209 A TW 101121209A TW 101121209 A TW101121209 A TW 101121209A TW I546532 B TWI546532 B TW I546532B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/327—Layered products comprising a layer of synthetic resin comprising polyolefins comprising polyolefins obtained by a metallocene or single-site catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H41/00—Machines for separating superposed webs
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/10—Homopolymers or copolymers of propene
- C09J123/14—Copolymers of propene
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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
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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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
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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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
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/748—Releasability
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2405/00—Adhesive articles, e.g. adhesive 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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/10—Peculiar tacticity
- C08L2207/14—Amorphous or atactic polypropylene
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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
- C08L2314/00—Polymer mixtures characterised by way of preparation
- C08L2314/06—Metallocene or single site catalysts
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
-
- 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
- C09J2423/00—Presence of polyolefin
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
- Laminated Bodies (AREA)
Description
本發明係關於一種分隔片之選定方法及使用由該選定方法選定之分隔片之黏著片材。 The present invention relates to a method of selecting a separator and an adhesive sheet using the separator selected by the selected method.
作為具有黏著劑層及基材層之黏著片材之製造方法,已知有因生產效率及成本性優異故而將構成基材層之材料與構成黏著劑層之材料共擠壓的成形方法(例如專利文獻1)。又,黏著片材通常以與黏著劑層接觸之方式而配置有分隔片作為至使用為止之保護材。於此種黏著片材中,可於藉由共擠壓而使黏著片材成形之情形時,抑制異物混入黏著劑層與分隔片之間,且獲得黏著劑層與分隔片接觸之面較為平滑之黏著片材,因此,研究將經共擠壓之黏著劑層形成材料於熔融之狀態下與分隔片貼合之方法。然而,以此種方式獲得之黏著片材於大多情況下,分隔片之剝離較為困難,黏著片材之處理性降低。又,針對此種問題,若使用輕剝離之分隔片,則處理性提高,但大多情況下,黏著片材之保管時黏著劑層之黏著力降低。如此,難以同時實現黏著片材之良好之處理性與適度之黏著力。 As a method for producing an adhesive sheet having an adhesive layer and a substrate layer, a molding method in which a material constituting a base material layer and a material constituting the adhesive layer are co-extruded due to excellent production efficiency and cost is known (for example, Patent Document 1). Further, the adhesive sheet is usually provided with a separator as a protective material until use in contact with the adhesive layer. In such an adhesive sheet, when the adhesive sheet is formed by co-extrusion, foreign matter is prevented from being mixed between the adhesive layer and the separator, and the surface where the adhesive layer is in contact with the separator is smooth. The sheet is adhered, and therefore, a method of bonding the coextruded adhesive layer forming material to the separator in a molten state is studied. However, in many cases, the adhesive sheet obtained in this manner is difficult to peel off the separator, and the sheet is rationally lowered. Moreover, when the separator which is lightly peeled is used, the handleability improves, but in many cases, the adhesive force of the adhesive layer at the time of storage of the adhesive sheet is reduced. In this way, it is difficult to achieve the good and rational adhesion of the adhesive sheet at the same time.
黏著片材中使用之分隔片係根據剝離劑之種類或其剝離力等而適當選定所需之分隔片。然而,如上所述,於與熔融之黏著劑層形成材料貼合之情形時,存在於獲得之黏著片材中分隔片本來之能力並未發揮之情形。因此,以熔融共擠壓成形所製造之黏著片材中使用之分隔片必需首先選 擇候補之分隔片,並於實際製造黏著片材後研究分隔片之適合度。因此,於每次變更黏著片材之構成時,必需製作黏著片材並研究分隔片之適合度,故而並不容易選定適當之分隔片。 The separator used in the adhesive sheet is appropriately selected according to the kind of the release agent, its peeling force, and the like. However, as described above, in the case of bonding with the molten adhesive layer forming material, there is a case where the original ability of the separator in the obtained adhesive sheet is not exerted. Therefore, the separator used in the adhesive sheet produced by melt co-extrusion must first be selected. Select the replacement piece and study the fit of the piece after actually making the adhesive sheet. Therefore, each time the structure of the adhesive sheet is changed, it is necessary to prepare an adhesive sheet and study the suitability of the separator. Therefore, it is not easy to select an appropriate separator.
專利文獻1:日本專利特開2009-275209號公報 Patent Document 1: Japanese Patent Laid-Open Publication No. 2009-275209
本發明係為解決上述先前之課題而完成者,其目的在於提供一種可簡便地選定適於至少具有黏著劑層之黏著片材之分隔片的方法。 The present invention has been made to solve the above problems, and an object of the invention is to provide a method for easily selecting a separator suitable for an adhesive sheet having at least an adhesive layer.
本發明之分隔片之選定方法包括:將至少形成黏著劑層之材料於熔融之狀態下與分隔片貼合而獲得至少具有黏著劑層與分隔片之黏著片材的步驟;自獲得之黏著片材剝離該分隔片並將該黏著片材之黏著劑層與評價用分隔片貼合而製作評價用黏著片材的步驟;及以一對緩衝材與一對加壓板夾持該評價用黏著片材,於加壓板面溫度140℃、壓力5 MPa下保持1分鐘之後,藉由剝離速度為300 mm/分鐘下之180°剝離試驗對評價用分隔片之剝離力進行評價的步驟。 The method for selecting a separator of the present invention comprises the steps of: bonding at least a material forming an adhesive layer to a separator in a molten state to obtain an adhesive sheet having at least an adhesive layer and a separator; and self-obtaining adhesive sheets The separator is peeled off, and the adhesive sheet of the adhesive sheet is bonded to the evaluation separator to form a pressure-sensitive adhesive sheet for evaluation; and the evaluation adhesive is sandwiched between the pair of cushioning materials and the pair of pressure plates. The sheet was subjected to a step of evaluating the peeling force of the separator for separation by a 180° peel test at a peeling speed of 300 mm/min after the sheet temperature was maintained at 140 ° C and a pressure of 5 MPa for 1 minute.
於較佳之實施形態中,選定於上述評價步驟中所測定之剝離力為2.0 N/50 mm以下之分隔片。 In a preferred embodiment, the separator having a peeling force measured in the above evaluation step of 2.0 N/50 mm or less is selected.
於較佳之實施形態中,上述黏著片材之黏著劑層包含聚烯烴系樹脂。 In a preferred embodiment, the adhesive layer of the adhesive sheet comprises a polyolefin resin.
於較佳之實施形態中,上述聚烯烴系樹脂包含使用茂金屬觸媒而聚合之非晶質丙烯-(1-丁烯)共聚物。 In a preferred embodiment, the polyolefin-based resin comprises an amorphous propylene-(1-butene) copolymer polymerized using a metallocene catalyst.
於本發明之另一實施形態中,提供一種黏著片材。該黏著片材包含:基材層、黏著劑層、及由上述選定方法選定之分隔片。 In another embodiment of the invention, an adhesive sheet is provided. The adhesive sheet comprises a substrate layer, an adhesive layer, and a separator selected by the above selected method.
根據本發明,可簡便地選定適合黏著片材之分隔片。 According to the present invention, the separator suitable for the adhesive sheet can be easily selected.
本發明之分隔片之選定方法係選定適合黏著片材之分隔片之方法。根據本發明之方法,可簡便地選擇適合藉由將至少形成黏著劑層之材料於熔融之狀態下與分隔片貼合而獲得之黏著片材的分隔片。本發明之分隔片之選定方法包括:將至少形成黏著劑層之材料於熔融之狀態下與分隔片貼合而獲得至少具有黏著劑層與分隔片之黏著片材的步驟;自獲得之黏著片材剝離該分隔片並將該黏著片材之黏著劑層與評價用分隔片貼合而製作評價用黏著片材的步驟;及以一對緩衝材及一對加壓板夾持該評價用黏著片材,於加壓板面溫度140℃、壓力5 MPa下保持1分鐘之後,藉由剝離速度為300 mm/分鐘下之180°剝離試驗而對評價用分隔片之剝離力進行評價的步驟。根據本發明之選定方法,可藉由對分隔片之剝離力進行評價而簡便地選定適合黏著片材之分隔片。 The method of selecting the separator of the present invention is a method of selecting a separator suitable for adhering the sheet. According to the method of the present invention, it is possible to easily select a separator suitable for an adhesive sheet obtained by laminating at least a material forming an adhesive layer with a separator in a molten state. The method for selecting a separator of the present invention comprises the steps of: bonding at least a material forming an adhesive layer to a separator in a molten state to obtain an adhesive sheet having at least an adhesive layer and a separator; and self-obtaining adhesive sheets The separator is peeled off, and the adhesive sheet of the adhesive sheet is bonded to the evaluation separator to form a pressure-sensitive adhesive sheet for evaluation; and the evaluation adhesive is sandwiched between a pair of cushioning materials and a pair of pressure plates. The sheet was subjected to a step of evaluating the peeling force of the separator for evaluation by a 180° peeling test at a peeling speed of 300 mm/min after the sheet temperature was maintained at 140 ° C and a pressure of 5 MPa for 1 minute. According to the selected method of the present invention, the separator suitable for the adhesive sheet can be easily selected by evaluating the peeling force of the separator.
本發明之選定方法包括將至少形成黏著劑層之材料於熔融之狀態下與分隔片貼合而獲得至少具有黏著劑層與分隔片之黏著片材的步驟。該黏著片材典型情況下依序具有基材層、黏著劑層及分隔片。 The selected method of the present invention comprises the step of bonding at least a material forming the adhesive layer to the separator in a molten state to obtain an adhesive sheet having at least an adhesive layer and a separator. The adhesive sheet typically has a substrate layer, an adhesive layer, and a separator in sequence.
作為使上述黏著片材成形之方法,並無特別限制,包括將至少形成黏著劑層之材料於熔融之狀態下與分隔片貼合之步驟即可。上述成形方法例如包括:將形成黏著劑層之材料及形成基材層之材料於熔融後擠壓而獲得黏著劑層與基材層之積層體的步驟;及於至少形成黏著劑層之材料於熔融之狀態下將該積層體之黏著劑層與分隔片貼合而獲得黏著片材的步驟。 The method for forming the above-mentioned adhesive sheet is not particularly limited, and may include a step of bonding at least a material forming the pressure-sensitive adhesive layer to the separator in a molten state. The above-mentioned forming method includes, for example, a step of extruding a material forming the adhesive layer and a material forming the substrate layer after melting to obtain a laminate of the adhesive layer and the substrate layer, and a material for forming at least the adhesive layer The step of bonding the adhesive layer of the laminate to the separator in a molten state to obtain an adhesive sheet.
於獲得上述黏著劑層與基材層之積層體之步驟中,該積層體例如可藉由對連結於模具之至少兩台擠壓機中之一台供給形成黏著劑層之材料,對另一台供給形成基材層之材料,並於熔融後擠壓而獲得。使上述黏著片材成形時之條件(例如模具溫度)可根據構成該黏著片材之各層之材料而適當設定。例如,模具溫度可設定為黏著片材之各層之形成材料成為熔融狀態之溫度。於一實施形態中,模具溫度可設定為160℃~220℃。 In the step of obtaining the laminate of the adhesive layer and the substrate layer, the laminate may be supplied with a material forming an adhesive layer, for example, by one of at least two extruders attached to the mold. The stage is supplied with a material forming the substrate layer, and is obtained by extrusion after melting. The conditions (for example, the mold temperature) at the time of molding the above-mentioned adhesive sheet can be appropriately set depending on the materials constituting the respective layers of the adhesive sheet. For example, the mold temperature can be set to a temperature at which the material forming the layers of the adhesive sheet becomes a molten state. In one embodiment, the mold temperature can be set to 160 ° C to 220 ° C.
將上述積層體與分隔片貼合之步驟具體而言,可藉由如下方式而進行:於獲得上述積層體之步驟中,於形成經擠壓之積層體之至少該黏著劑層的材料於熔融之狀態下使該積層體之黏著劑層與分隔片接觸,並利用接觸輥成形法進 行拉取。使形成上述黏著劑層之材料與分隔片接觸時之條件(例如,使構成黏著劑層之材料與分隔片接觸之溫度及接觸壓力)可根據構成黏著片材之各層之材料而適當設定。例如,使構成黏著劑層之材料與分隔片接觸之溫度可設定為維持至少形成黏著劑層之材料熔融之狀態的溫度。於一實施形態中,使構成黏著劑層之材料與分隔片接觸之溫度可設定為120℃~200℃。 Specifically, the step of bonding the laminate to the separator may be carried out by: in the step of obtaining the laminate, at least the material of the adhesive layer forming the extruded laminate is melted In this state, the adhesive layer of the laminate is brought into contact with the separator, and the contact roll forming method is used. Line pull. The conditions (for example, the temperature at which the material constituting the adhesive layer is brought into contact with the separator and the contact pressure) when the material forming the pressure-sensitive adhesive layer is brought into contact with the separator can be appropriately set depending on the material constituting each layer of the pressure-sensitive adhesive sheet. For example, the temperature at which the material constituting the adhesive layer is brought into contact with the separator may be set to a temperature at which at least the state in which the material forming the adhesive layer is melted is maintained. In one embodiment, the temperature at which the material constituting the adhesive layer is brought into contact with the separator may be set to 120 ° C to 200 ° C.
作為該步驟中使用之分隔片(以下亦稱為製造用分隔片),可使用任意適當之分隔片。例如,於該技術領域中,可使用通用之分隔片作為黏著片材之分隔片。具體而言,可列舉:三菱樹脂製造之商品名MRF-38、Higashiyama Film公司製造之商品名HY-S06等。 As the separator used in this step (hereinafter also referred to as a separator for production), any appropriate separator can be used. For example, in the technical field, a general separator can be used as a separator for an adhesive sheet. Specific examples include MRF-38 manufactured by Mitsubishi Plastics Co., Ltd., and HY-S06 manufactured by Higashiyama Film Co., Ltd., and the like.
本發明之選定方法中之評價步驟中使用的評價用黏著片材係以如下方式而獲得。首先,自藉由上述A項之方法而獲得之黏著片材剝離分隔片。該分隔片之剝離可藉由任意適當之機構而進行,可使用任意適當之剝離機進行剝離,亦可以手進行剝離。 The evaluation adhesive sheet used in the evaluation step in the selected method of the present invention is obtained in the following manner. First, the adhesive sheet is peeled off from the adhesive sheet obtained by the method of the above item A. The peeling of the separator can be carried out by any appropriate mechanism, and peeling can be carried out using any appropriate peeling machine, or peeling can be carried out by hand.
繼而,將剝離了分隔片之黏著片材之黏著劑層與作為選定之對象之評價用分隔片貼合。由於在下述剝離力之評價步驟中進行加壓,故而於評價用黏著片材之製作步驟中,無需將該黏著片材與該評價用分隔片牢固地貼合,貼合至維持該黏著片材與該評價用分隔片之積層狀態之程度即可。 Then, the adhesive layer from which the adhesive sheet of the separator was peeled off was bonded to the evaluation separator which was selected as the object to be selected. Since the pressurization is performed in the evaluation step of the peeling force described below, it is not necessary to firmly bond the adhesive sheet to the evaluation separator in the step of producing the adhesive sheet for evaluation, and the adhesive sheet is bonded to the adhesive sheet. The degree of the laminated state with the separator for evaluation may be sufficient.
上述評價用分隔片之剝離力評價步驟係以如下方式進行。將上述B步驟中獲得之評價用黏著片材以一對緩衝材夾持後,進而以一對加壓板夾持,於加壓板面溫度140℃、壓力5 MPa下保持1分鐘,進行加壓。關於黏著片材中使用之分隔片,若加壓板面溫度超過140℃,則存在分隔片與黏著劑層之剝離急遽變得困難之傾向。因此,可藉由將加壓板面溫度設為140℃而進行評價用黏著片材之加壓,並對加壓後之黏著片材中之評價用分隔片之剝離力進行評價,而選定合適之分隔片作為黏著片材之分隔片。再者,本發明之剝離力評價試驗中之加壓板面溫度係指加壓板表面之溫度。 The peeling force evaluation step of the above-mentioned evaluation separator sheet was carried out as follows. The evaluation adhesive sheet obtained in the above step B was sandwiched between a pair of cushioning materials, and further sandwiched between a pair of pressure plates, and held at a pressure plate surface temperature of 140 ° C and a pressure of 5 MPa for 1 minute. Pressure. In the separator used for the adhesive sheet, if the temperature of the pressure plate surface exceeds 140 ° C, the peeling of the separator sheet and the pressure-sensitive adhesive layer tends to be difficult. Therefore, the pressure of the pressure-sensitive adhesive sheet for evaluation can be increased by setting the temperature of the pressure plate surface to 140 ° C, and the peeling force of the evaluation separator sheet in the pressure-sensitive adhesive sheet after pressurization can be evaluated and selected. The separator is used as a separator for the adhesive sheet. Further, the pressure plate surface temperature in the peeling force evaluation test of the present invention means the temperature of the surface of the pressure plate.
於上述加壓中,為了防止對黏著片材施加過度之壓力,而於評價用黏著片材與加壓板之間配置有緩衝材。作為該緩衝材,可使用可用於熱壓之任意適當之緩衝材。作為緩衝材,例如可列舉:橡膠、耐熱性彈性體、以黏合劑結合有機或無機纖維者、不織布、橡膠與不織布之積層體等。加壓中使用之緩衝材只要選擇使用可使施加於評價用黏著片材之壓力成為適當之壓力的適當之緩衝材即可。例如,可藉由調整緩衝材之構成材料、尺寸(面積)而調整對評價用黏著片材施加之壓力。更具體而言,針對尺寸為150 mm×200 mm之分隔片,可使用面積為130 mm×160 mm之橡膠板。 In the above pressurization, a cushioning material is disposed between the evaluation adhesive sheet and the pressure plate in order to prevent excessive pressure from being applied to the adhesive sheet. As the cushioning material, any appropriate cushioning material which can be used for hot pressing can be used. Examples of the cushioning material include a rubber, a heat-resistant elastic body, a combination of an organic or inorganic fiber with a binder, a non-woven fabric, a laminate of a rubber and a non-woven fabric, and the like. The cushioning material used for pressurization may be selected from a suitable cushioning material which allows the pressure applied to the pressure-sensitive adhesive sheet for evaluation to be an appropriate pressure. For example, the pressure applied to the evaluation adhesive sheet can be adjusted by adjusting the constituent material and size (area) of the cushioning material. More specifically, for a separator having a size of 150 mm × 200 mm, a rubber sheet having an area of 130 mm × 160 mm can be used.
又,為了防止於加壓時緩衝材及評價用黏著片材之黏 連,亦可於緩衝材與評價用黏著片材之間各配置樹脂片材,進行加壓。該樹脂片材只要為可用作分隔片之樹脂片材即可,可使用任意適當之片材,例如可使用聚對苯二甲酸乙二酯系樹脂片材、聚醯亞胺系樹脂膜等。該樹脂片材之厚度通常為38 μm~75 μm。 Moreover, in order to prevent sticking of the cushioning material and the adhesive sheet for evaluation at the time of pressurization Further, a resin sheet may be placed between the cushioning material and the pressure-sensitive adhesive sheet for evaluation, and pressurized. The resin sheet may be any resin sheet that can be used as a separator, and any suitable sheet may be used. For example, a polyethylene terephthalate resin sheet or a polyimide film may be used. . The thickness of the resin sheet is usually from 38 μm to 75 μm.
評價用黏著片材之加壓可使用可設定上述加壓板面溫度及壓力之任意適當之機構而進行。例如,可使用市售之加壓機而進行,具體而言,可列舉東洋精機公司製造之MINI TEST PRESS-10等。 The pressurization of the pressure-sensitive adhesive sheet for evaluation can be carried out by any appropriate mechanism capable of setting the temperature and pressure of the pressure plate surface. For example, it can be carried out using a commercially available press machine, and specifically, MINI TEST PRESS-10 manufactured by Toyo Seiki Co., Ltd., and the like can be mentioned.
將加壓後之評價用黏著片材放置至變成室溫為止,進行評價用分隔片之剝離試驗。該剝離試驗係藉由於剝離速度300 mm/分鐘、剝離角度180°下剝離評價用分隔片而進行。 The adhesive sheet for evaluation after pressurization was left to room temperature, and the peeling test of the separator for evaluation was performed. This peeling test was performed by peeling the evaluation separator sheet at a peeling speed of 300 mm/min and a peeling angle of 180°.
可根據藉由上述剝離試驗測定之剝離力並視分隔片所要求之特性,而選擇所需之分隔片。例如,於需要處理性優異且保持適度之黏著力之分隔片之情形時,可較佳地使用上述剝離試驗中測定之剝離力為2.0 N/50 mm以下之分隔片。又,於需要黏著劑層與分隔片之密接性更高之分隔片之情形時,使用上述剝離試驗中測定之剝離力超過2.0 N/50 mm之分隔片即可。就於市售之膠帶貼附裝置(例如,日東精機公司製造之背面研磨用保護膠帶貼附裝置,商品名DR3000III等)中之操作方面而言,以上述剝離試驗中測定之剝離力2.0 N/50 mm為基準,可選擇所需之分隔片。再者,於需要處理性更高之分隔片之情形時,使用上述剝 離試驗中測定之剝離力更小之分隔片即可。 The desired separator can be selected according to the peeling force measured by the above peeling test and depending on the characteristics required for the separator. For example, in the case of a separator which is excellent in handleability and maintains an appropriate adhesive strength, a separator having a peeling force measured in the above peeling test of 2.0 N/50 mm or less can be preferably used. Further, in the case where a separator having a higher adhesiveness between the adhesive layer and the separator is required, the separator having a peeling force measured in the above peeling test exceeding 2.0 N/50 mm may be used. In terms of handling in a commercially available tape attaching device (for example, a protective tape attaching device for back grinding manufactured by Nitto Seiki Co., Ltd., trade name DR3000III, etc.), the peeling force measured in the above peeling test is 2.0 N/ With a 50 mm reference, you can choose the separator you want. Furthermore, in the case of a separator which requires a higher degree of handling, the above peeling is used. The separator having a smaller peeling force measured in the test may be used.
本發明使用之黏著片材典型情況下包含基材層、黏著劑層及分隔片。又,該黏著片材亦可視需要包含任意適當之其他層。作為該其他層,例如可列舉賦予耐熱性之表面層。 The adhesive sheet used in the present invention typically comprises a substrate layer, an adhesive layer and a separator. Further, the adhesive sheet may optionally contain any other suitable layer. As the other layer, for example, a surface layer to which heat resistance is imparted can be mentioned.
黏著片材之厚度(除分隔片之厚度以外)較佳為90 μm~285 μm、更佳為105 μm~225 μm、進而較佳為130 μm~210 μm。 The thickness of the adhesive sheet (excluding the thickness of the separator) is preferably from 90 μm to 285 μm, more preferably from 105 μm to 225 μm, and still more preferably from 130 μm to 210 μm.
上述分隔片係藉由本發明之分隔片之選定方法而選定者。分隔片通常具有基材層及剝離劑層。該基材層及剝離劑層可以任意適當之材料構成。該分隔片較佳為於本發明之選定方法中經評價之分隔片之剝離力為2.0 N/50 mm以下、更佳為0.05 N/50 mm~2.0 N/50 mm、進而較佳為0.05 N/50 mm~1.8 N/50 mm。藉由使用此種分隔片,而獲得具有優異之處理性且保持適度之黏著力的黏著片材。又,於形成分隔片更不易自黏著劑層剝離之黏著片材之情形時,使用於本發明之選定方法中經評價之剝離力超過2.0 N/50 mm之分隔片即可。 The separator is selected by the method of selecting the separator of the present invention. The separator usually has a substrate layer and a release agent layer. The base material layer and the release agent layer may be formed of any suitable material. Preferably, the separator has a peeling force of 2.0 N/50 mm or less, more preferably 0.05 N/50 mm to 2.0 N/50 mm, and still more preferably 0.05 N, which is evaluated in the selected method of the present invention. /50 mm~1.8 N/50 mm. By using such a separator, an adhesive sheet having excellent practicability and maintaining a moderate adhesive force is obtained. Further, in the case of forming an adhesive sheet in which the separator is less likely to be peeled off from the adhesive layer, the separator having an evaluation peeling force exceeding 2.0 N/50 mm in the selected method of the present invention may be used.
分隔片之厚度並無特別限制,可設定為任意適當之厚度。分隔片之厚度例如可設定為25 μm~250 μm。 The thickness of the separator is not particularly limited and can be set to any appropriate thickness. The thickness of the separator can be set, for example, from 25 μm to 250 μm.
上述黏著劑層係藉由任意適當之黏著劑而構成,例如可 列舉包含聚烯烴系樹脂、丙烯酸系樹脂、苯乙烯系樹脂等熱塑性樹脂之黏著劑等。該黏著劑層較佳為包含聚烯烴系樹脂,具體而言,可列舉:低密度聚乙烯、超低密度聚乙烯、低結晶聚丙烯、非晶質丙烯-(1-丁烯)共聚物、離子聚合物樹脂、乙烯-乙酸乙烯酯共聚物、乙烯-(甲基)丙烯酸共聚物、乙烯-(甲基)丙烯酸酯-馬來酸酐共聚物、乙烯-甲基丙烯酸縮水甘油酯共聚物等乙烯共聚物或聚烯烴改性聚合物等。該黏著劑層更佳為包含非晶質丙烯-(1-丁烯)共聚物。藉由使用此種黏著劑層,而可獲得對被接著體之污染較少、同時實現黏著力與剝離性、且可藉由共擠壓成形而製造之黏著片材。進而,若為此種黏著劑層,則可藉由與基材層之共擠壓成形而製造黏著片材,且可以較少之步驟數且不使用有機溶劑而獲得黏著片材。再者,於本說明書中,「非晶質」係指不具有如結晶質般明確之熔點之性質。 The above adhesive layer is formed by any suitable adhesive, for example An adhesive containing a thermoplastic resin such as a polyolefin resin, an acrylic resin or a styrene resin is used. The pressure-sensitive adhesive layer preferably contains a polyolefin-based resin, and specific examples thereof include low-density polyethylene, ultra-low-density polyethylene, low-crystalline polypropylene, and amorphous propylene-(1-butene) copolymer. Ethylene polymer resin, ethylene-vinyl acetate copolymer, ethylene-(meth)acrylic acid copolymer, ethylene-(meth)acrylate-maleic anhydride copolymer, ethylene-glycidyl methacrylate copolymer, etc. Copolymer or polyolefin modified polymer, and the like. The adhesive layer more preferably contains an amorphous propylene-(1-butene) copolymer. By using such an adhesive layer, it is possible to obtain an adhesive sheet which is less contaminated by the adherend, achieves adhesiveness and peelability, and can be produced by co-extrusion molding. Further, in the case of such an adhesive layer, an adhesive sheet can be produced by co-extrusion with a base material layer, and an adhesive sheet can be obtained with a small number of steps and without using an organic solvent. In the present specification, "amorphous" means a property which does not have a melting point as defined by crystallinity.
上述非晶質丙烯-(1-丁烯)共聚物較佳為可藉由使用茂金屬觸媒使丙烯與1-丁烯聚合而獲得。更詳細而言,非晶質丙烯-(1-丁烯)共聚物例如可藉由進行使用茂金屬觸媒使丙烯與1-丁烯聚合之聚合步驟並於該聚合步驟後進行殘留觸媒去除步驟、異物去除步驟等後處理步驟而獲得。非晶質丙烯-(1-丁烯)共聚物係經過此種步驟而以例如粉末狀、顆粒狀等形狀而獲得。作為茂金屬觸媒,例如可列舉:包含茂金屬化合物與鋁氧烷之茂金屬均勻混合觸媒、於微粒子狀之載體上擔載有茂金屬化合物之茂金屬擔載型觸媒等。使用茂金屬觸媒聚合之非晶質丙烯-(1-丁烯)共聚物顯示狹 窄之分子量分佈。 The above amorphous propylene-(1-butene) copolymer is preferably obtained by polymerizing propylene and 1-butene using a metallocene catalyst. More specifically, the amorphous propylene-(1-butene) copolymer can be subjected to, for example, a polymerization step of polymerizing propylene and 1-butene using a metallocene catalyst and performing residual catalyst removal after the polymerization step. Obtained by a post-treatment step such as a step, a foreign matter removal step, and the like. The amorphous propylene-(1-butene) copolymer is obtained in such a form as a powder, a pellet or the like through such a step. Examples of the metallocene catalyst include a metallocene supported catalyst containing a metallocene compound and a metallocene uniformly mixed catalyst, and a metallocene compound supported on a fine particle carrier. Amorphous propylene-(1-butene) copolymer polymerized using metallocene catalyst shows narrow Narrow molecular weight distribution.
上述非晶質丙烯-(1-丁烯)共聚物中來自丙烯之構成單元之含有比例較佳為80莫耳%~99莫耳%、更佳為85莫耳%~99莫耳%、進而較佳為90莫耳%~99莫耳%。 The content ratio of the constituent unit derived from propylene in the amorphous propylene-(1-butene) copolymer is preferably from 80 mol% to 99 mol%, more preferably from 85 mol% to 99 mol%, and further It is preferably 90% by mole to 99% by mole.
上述非晶質丙烯-(1-丁烯)共聚物中來自1-丁烯之構成單元之含有比例較佳為1莫耳%~15莫耳%、更佳為1莫耳%~10莫耳%。若為此種範圍,則可獲得韌性與柔軟性之平衡優異之黏著片材。 The content ratio of the constituent unit derived from 1-butene in the amorphous propylene-(1-butene) copolymer is preferably from 1 mol% to 15 mol%, more preferably from 1 mol% to 10 mol%. %. When it is such a range, an adhesive sheet excellent in the balance of toughness and flexibility can be obtained.
上述非晶質丙烯-(1-丁烯)共聚物可為嵌段共聚物,亦可為無規共聚物。 The above amorphous propylene-(1-butene) copolymer may be a block copolymer or a random copolymer.
上述非晶質丙烯-(1-丁烯)共聚物亦可於無損本發明之效果之範圍內進而包含來自其他單體之構成單元。作為其他單體,例如可列舉:乙烯、1-戊烯、1-己烯、1-辛烯、1-癸烯、4-甲基-1-戊烯、3-甲基-1-戊烯等α-烯烴等。 The amorphous propylene-(1-butene) copolymer may further contain constituent units derived from other monomers within the range which does not impair the effects of the present invention. Examples of the other monomer include ethylene, 1-pentene, 1-hexene, 1-octene, 1-decene, 4-methyl-1-pentene, and 3-methyl-1-pentene. Such as α-olefins and the like.
上述黏著劑層亦可於無損本發明之效果之範圍內進而包含其他成分。作為該其他成分,例如可列舉:抗氧化劑、紫外線吸收劑、光穩定劑、耐熱穩定劑、抗靜電劑等。其他成分之種類及使用量可根據目的而適當地進行選擇。 The above-mentioned adhesive layer may further contain other components within the range which does not impair the effects of the present invention. Examples of the other component include an antioxidant, an ultraviolet absorber, a light stabilizer, a heat stabilizer, and an antistatic agent. The type and amount of other components can be appropriately selected depending on the purpose.
黏著劑層之厚度較佳為20 μm~100 μm,更佳為30 μm~65 μm。 The thickness of the adhesive layer is preferably from 20 μm to 100 μm, more preferably from 30 μm to 65 μm.
上述基材層可使用任意適當之材料而構成,例如可列舉:聚酯(聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸丁二酯等)、聚烯烴(聚乙 烯、聚丙烯、乙烯-丙烯共聚物等)、聚乙烯醇、聚二氯亞乙烯、聚氯乙烯、氯乙烯-乙酸乙烯酯共聚物、乙烯-乙酸乙烯酯共聚物、聚乙酸乙烯酯、聚醯胺、聚醯亞胺、纖維素類、氟系樹脂、聚醚、聚苯乙烯系樹脂(聚苯乙烯等)、聚碳酸酯、聚醚碸等。較佳為上述基材層包含乙烯-乙酸乙烯酯共聚物。 The base material layer may be formed using any appropriate material, and examples thereof include polyester (polyethylene terephthalate, polyethylene naphthalate, polybutylene terephthalate, and polynaphthalene dicarboxylic acid). Butadiene ester, etc., polyolefin (polyethyl b Alkene, polypropylene, ethylene-propylene copolymer, etc.), polyvinyl alcohol, polydivinylidene chloride, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, ethylene-vinyl acetate copolymer, polyvinyl acetate, poly Amidoxime, polyimine, cellulose, fluorine resin, polyether, polystyrene resin (polystyrene, etc.), polycarbonate, polyether oxime or the like. Preferably, the substrate layer comprises an ethylene-vinyl acetate copolymer.
上述基材層亦可於無損本發明之效果之範圍內進而包含其他成分。作為該其他成分,例如可使用與上文中說明之黏著劑層中可包含之其他成分同樣之成分。 The base material layer may further contain other components within the range which does not impair the effects of the present invention. As the other component, for example, the same components as those other components which can be contained in the above-mentioned adhesive layer can be used.
基材層之厚度較佳為30 μm~185 μm,更佳為65 μm~175 μm。 The thickness of the substrate layer is preferably from 30 μm to 185 μm, more preferably from 65 μm to 175 μm.
作為本發明之黏著片材中包含之其他層,例如可列舉可對黏著片材賦予耐熱性之表面層。該表面層可使用具有耐熱性之任意適當之樹脂,較佳為包含聚丙烯系樹脂。上述聚丙烯系樹脂較佳為藉由使用有茂金屬觸媒之聚合而獲得。更詳細而言,聚丙烯系樹脂例如可藉由進行使用茂金屬觸媒使包含丙烯之單體組合物聚合之聚合步驟並於該聚合步驟後進行殘留觸媒去除步驟、異物去除步驟等後處理步驟而獲得。聚丙烯系樹脂係經過此種步驟而以例如粉末狀、顆粒狀等形狀而獲得。作為茂金屬觸媒,例如可列舉上文中例示者。 Examples of the other layer included in the adhesive sheet of the present invention include a surface layer which can impart heat resistance to the adhesive sheet. As the surface layer, any suitable resin having heat resistance can be used, and a polypropylene resin is preferable. The above polypropylene-based resin is preferably obtained by polymerization using a metallocene catalyst. More specifically, the polypropylene-based resin can be subjected to, for example, a polymerization step of polymerizing a monomer composition containing propylene using a metallocene catalyst, and a post-treatment such as a residual catalyst removal step or a foreign matter removal step after the polymerization step. Obtained by the steps. The polypropylene resin is obtained in such a form as a powder or a pellet by such a procedure. As the metallocene catalyst, for example, those exemplified above can be cited.
上述聚丙烯系樹脂亦可使用市售品。作為市售品之聚丙烯系樹脂之具體例,可列舉Japan Polypropylene股份有限 公司製造之商品名「WINTEC(穩特固)」、「WELNEX(維妮舒)」系列等。 Commercially available products can also be used as the polypropylene resin. Specific examples of the polypropylene-based resin which is commercially available include Japan Polypropylene Co., Ltd. The company's trade names are "WINTEC" and "WELNEX" series.
上述表面層亦可於無損本發明之效果之範圍內進而包含其他成分。作為該其他成分,可列舉與上文中說明之黏著劑層中可包含之其他成分相同者。其他成分之種類及使用量可根據目的而適當地進行選擇。 The above surface layer may further contain other components within the range which does not impair the effects of the present invention. The other component may be the same as the other components which may be included in the adhesive layer described above. The type and amount of other components can be appropriately selected depending on the purpose.
以下,藉由實施例對本發明進行具體說明,但本發明絲毫不受該等實施例限定。再者,實施例等中之試驗及評價方法如下。又,份意指重量份。 Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited by the examples. Furthermore, the test and evaluation methods in the examples and the like are as follows. Also, parts mean parts by weight.
作為形成可賦予耐熱性之表面層之材料,使用藉由茂金屬觸媒而聚合之聚丙烯系樹脂(Japan Polypropylene公司製造,商品名「WELNEX:RFGV4A」;熔點130℃,軟化點120℃,Mw/Mn=2.9)。 As a material for forming a surface layer capable of imparting heat resistance, a polypropylene resin polymerized by a metallocene catalyst (manufactured by Japan Polypropylene Co., Ltd., trade name "WELNEX: RFGV4A"; melting point 130 ° C, softening point 120 ° C, Mw is used. /Mn = 2.9).
作為形成基材層之材料,使用乙烯-乙酸乙烯酯共聚物(三井Dupont公司製造,商品名「EVAFLEX P-1007」)。 As a material for forming the base material layer, an ethylene-vinyl acetate copolymer (manufactured by Mitsui Dupont Co., Ltd., trade name "EVAFLEX P-1007") was used.
作為形成黏著劑層之材料,使用藉由茂金屬觸媒而聚合之非晶質丙烯-(1-丁烯)共聚物(住友化學公司製造,商品名「TAFTHREN H5002」:來自丙烯之構成單元90莫耳%/來自1-丁烯之構成單元10莫耳%,Mw=230,000,Mw/Mn=1.8)。 As a material for forming the adhesive layer, an amorphous propylene-(1-butene) copolymer polymerized by a metallocene catalyst (manufactured by Sumitomo Chemical Co., Ltd., trade name "TAFTHREN H5002": constituent unit derived from propylene 90 is used. Molar % / constituent unit from 1-butene 10 mol%, Mw = 230,000, Mw / Mn = 1.8).
將上述形成表面層之材料100份、上述形成基材層之材料100份及上述形成黏著劑層之材料100份投入各自之擠壓機中,並進行T型模熔融共擠壓(模具溫度:180℃)。藉由 接觸輥使製造用分隔片(三菱樹脂公司製造,MRF38,厚度38 μm)貼合(氣隙:150 mm,接觸溫度:165℃)於自模具共擠壓出之表面層/基材層/黏著劑層之積層體之黏著劑層,而獲得表面層(厚度30 μm)/基材層(厚度130 μm)/黏著劑層(厚度45 μm)/分隔片之試驗用黏著片材。再者,表面層、基材層及黏著劑層之厚度係藉由T型模出口之形狀而控制。 100 parts of the material for forming the surface layer, 100 parts of the material for forming the substrate layer, and 100 parts of the material for forming the adhesive layer were put into respective extruders, and T-die melt co-extrusion was carried out (mold temperature: 180 ° C). By The contact roll was bonded to a manufacturing separator (Mitsubishi Resin, MRF38, thickness 38 μm) (air gap: 150 mm, contact temperature: 165 ° C) on the surface layer/substrate layer/adhesive co-extruded from the mold. The adhesive layer of the laminate of the agent layer was obtained to obtain a test adhesive sheet of a surface layer (thickness: 30 μm) / a substrate layer (thickness: 130 μm) / an adhesive layer (thickness: 45 μm) / separator. Furthermore, the thickness of the surface layer, the substrate layer and the adhesive layer is controlled by the shape of the T-die exit.
自參考例1中獲得之黏著片材剝離黏著劑層側之分隔片。繼而,於黏著劑層上貼合評價用分隔片1(Higashiyama Film公司製造,HY-S30,厚度38 μm),而獲得評價用黏著片材。 The adhesive sheet obtained in Reference Example 1 peeled off the separator on the side of the adhesive layer. Then, the separator 1 for evaluation (HY-S30, manufactured by Higashiyama Film Co., Ltd., thickness: 38 μm) was bonded to the pressure-sensitive adhesive layer to obtain an adhesive sheet for evaluation.
使用加壓機(東洋精機公司製造,MINI TEST PRESS-10,板面面積:250 mm×250 mm)加壓所獲得之評價用黏著片材。使用三菱樹脂製造之MRN38作為樹脂片材(分隔片),並使用橡膠板(厚度:1 mm,130 mm×160 mm)作為緩衝材。評價用黏著片材於依序積層有不鏽鋼板(SUS(Steel Use Stainless,日本不鏽鋼標準)板)/樹脂片材/緩衝材/樹脂片材/評價用黏著片材/樹脂片材/緩衝材/樹脂片材/不鏽鋼板後,以加壓板夾持,並於加壓板面溫度140℃、加壓壓力5 MPa下保持1分鐘。繼而,將黏著片材放置至室溫為止,測定黏著片材之評價用分隔片之剝離力(剝離速度:300 mm/分鐘,剝離角度:180°)。將測定之剝 離力示於表1。 The evaluation adhesive sheet obtained was pressed using a press machine (manufactured by Toyo Seiki Co., Ltd., MINI TEST PRESS-10, panel area: 250 mm × 250 mm). MRN38 made of Mitsubishi resin was used as a resin sheet (separator), and a rubber sheet (thickness: 1 mm, 130 mm × 160 mm) was used as a cushioning material. Adhesive sheet for evaluation is laminated with stainless steel plate (SUS (Steel Use Stainless) plate) / resin sheet / cushioning material / resin sheet / evaluation adhesive sheet / resin sheet / cushioning material / After the resin sheet/stainless steel plate, it was sandwiched by a pressurizing plate, and held at a press plate surface temperature of 140 ° C and a pressurizing pressure of 5 MPa for 1 minute. Then, the adhesive sheet was allowed to stand at room temperature, and the peeling force of the evaluation sheet for the adhesive sheet (peeling speed: 300 mm/min, peeling angle: 180°) was measured. Peeling The force is shown in Table 1.
除使用評價用分隔片2(Higashiyama Film公司製造,HY-TS11,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the evaluation separator sheet 2 (Higashiyama Film Co., Ltd., HY-TS11, thickness: 75 μm) was used instead of the evaluation separator sheet 1. The measured peeling force is shown in Table 1.
除使用評價用分隔片3(Higashiyama Film公司製造,HY-TS15,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the separator sheet for evaluation 3 (HY-TS15, thickness: 75 μm, manufactured by Higashiyama Film Co., Ltd.) was used instead of the separator sheet 1 for evaluation. The measured peeling force is shown in Table 1.
除使用評價用分隔片4(三菱樹脂公司製造,MRE38,厚度38 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the evaluation separator sheet 4 (manufactured by Mitsubishi Plastics Co., Ltd., MRE 38, thickness: 38 μm) was used instead of the evaluation separator sheet 1. The measured peeling force is shown in Table 1.
除使用評價用分隔片5(三菱樹脂公司製造,MRN38,厚度38 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the separator sheet for evaluation 5 (manufactured by Mitsubishi Plastics Co., Ltd., MRN 38, thickness: 38 μm) was used instead of the separator sheet 1 for evaluation. The measured peeling force is shown in Table 1.
除使用評價用分隔片6(三菱樹脂公司製造,MRF38,厚度38 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the evaluation separator sheet 6 (MRF38, thickness: 38 μm, manufactured by Mitsubishi Plastics Co., Ltd.) was used instead of the evaluation separator sheet 1. The measured peeling force is shown in Table 1.
除使用評價用分隔片7(Higashiyama Film公司製造,HY-S10,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the separator sheet for evaluation 7 (HY-S10, thickness: 75 μm, manufactured by Higashiyama Film Co., Ltd.) was used instead of the separator sheet 1 for evaluation. The measured peeling force is shown in Table 1.
除使用評價用分隔片8(Higashiyama Film公司製造,HY-S06,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the separator sheet for evaluation 8 (HY-S06, thickness: 75 μm, manufactured by Higashiyama Film Co., Ltd.) was used instead of the separator sheet 1 for evaluation. The measured peeling force is shown in Table 1.
除使用評價用分隔片9(Higashiyama Film公司製造,HY-TS05G,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the separator sheet for evaluation 9 (HY-TS05G, thickness: 75 μm, manufactured by Higashiyama Film Co., Ltd.) was used instead of the separator sheet 1 for evaluation. The measured peeling force is shown in Table 1.
除使用評價用分隔片10(Higashiyama Film公司製造,HY-US20,厚度75 μm)代替評價用分隔片1以外,與評價用分隔片1同樣地測定評價用分隔片之剝離力。將測定之剝離力示於表1。 The peeling force of the evaluation separator sheet was measured in the same manner as the evaluation separator sheet 1 except that the evaluation separator sheet 10 (Higashiyama Film Co., Ltd., HY-US20, thickness: 75 μm) was used instead of the evaluation separator sheet 1. The measured peeling force is shown in Table 1.
除使用評價用分隔片1~10以外,與參考例1同樣地獲得黏著片材1~10。將獲得之黏著片材1~10供於以下之評價中。將結果示於表2。 Adhesive sheets 1 to 10 were obtained in the same manner as in Reference Example 1 except that the evaluation separators 1 to 10 were used. The obtained adhesive sheets 1 to 10 were used in the following evaluations. The results are shown in Table 2.
測定獲得之黏著片材中之分隔片之剝離力(剝離速度:300 mm/min,剝離角度:180°)。 The peeling force of the separator in the obtained adhesive sheet was measured (peeling speed: 300 mm/min, peeling angle: 180°).
將獲得之黏著片材於50℃下老化2天後,剝離貼合於黏著劑層上之分隔片,藉由按照JIS Z 0237(2000)之方法(貼合條件:2 kg輥往返一次,剝離速度:300 mm/min,剝離角度180°)測定該黏著劑層對於4吋半導體晶圓之鏡面(矽製造)之黏著力。若測定之值為0.005 N/20 mm以上,則作為黏著片材而具有充分之黏著力。 After the obtained adhesive sheet was aged at 50 ° C for 2 days, the separator attached to the adhesive layer was peeled off by a method in accordance with JIS Z 0237 (2000) (adhesion conditions: 2 kg roller reciprocating once, peeling off Speed: 300 mm/min, peeling angle 180°) The adhesion of the adhesive layer to the mirror surface of a 4 Å semiconductor wafer was measured. When the measured value is 0.005 N/20 mm or more, it has sufficient adhesion as an adhesive sheet.
使用實施例1中測定之分隔片之剝離力為2.0 N/50 mm以下之分隔片1~5的黏著片材1~5中,分隔片之剝離容易且適度地維持黏著劑層之黏著力。又,使用實施例1中測定之 分隔片之剝離力超過2.0 N/50 mm之分隔片6~10的黏著片材6~10中,與分隔片1~5相比用於剝離分隔片所需之力較大。 In the adhesive sheets 1 to 5 of the separators 1 to 5 having a peeling force of 2.0 N/50 mm or less in the separator measured in Example 1, the peeling of the separator was easy and the adhesion of the pressure-sensitive adhesive layer was moderately maintained. Further, the measurement was carried out in Example 1. In the adhesive sheets 6 to 10 of the separators 6 to 10 in which the peeling force of the separator exceeds 2.0 N/50 mm, the force required for peeling off the separator is larger than that of the separators 1 to 5.
本發明之分隔片之選定方法例如可較佳地用於黏著片材中使用之分隔片之選定。 The method of selecting the separator of the present invention can be preferably used, for example, for the selection of the separator used in the adhesive sheet.
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JP2013001738A (en) | 2013-01-07 |
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KR101427504B1 (en) | 2014-08-07 |
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