JP2012135951A - Polyester film for double-sided adhesive tape - Google Patents

Polyester film for double-sided adhesive tape Download PDF

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JP2012135951A
JP2012135951A JP2010289872A JP2010289872A JP2012135951A JP 2012135951 A JP2012135951 A JP 2012135951A JP 2010289872 A JP2010289872 A JP 2010289872A JP 2010289872 A JP2010289872 A JP 2010289872A JP 2012135951 A JP2012135951 A JP 2012135951A
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film
double
adhesive tape
polyester film
thickness
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Takashi Suzuki
孝 鈴木
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Mitsubishi Plastics Inc
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Abstract

PROBLEM TO BE SOLVED: To provide a biaxially oriented polyester film for a double-sided adhesive tape, which is capable of highly enhancing winding property and workability of the biaxially oriented polyester film, and also which is suitable as an adhering member used in an application in which extremely thin clearance of ≤10 μm is required.SOLUTION: The biaxially oriented polyester film for the double-sided adhesive tape is characterized in that a plane orientation degree is 0.170 to 0.190, contracion ratio at 120°C for 3 min. is ≤2.0% in both of a film longitudinal direction and a width direction, and the thickness is 1 to 4 μm.

Description

本発明は、両面粘着テープ、さらに詳しくは、携帯電話、PDAなどの携帯端末機器や薄膜表示体等の部材固定用、光ディスクの基板貼り合わせ用、偏光板の固定用などとして好適な、両面粘着テープの基材として使用される両面粘着テープ用二軸配向ポリエステルフィルムに関する。   The present invention relates to a double-sided pressure-sensitive adhesive tape, more specifically, a double-sided pressure-sensitive adhesive suitable for fixing a mobile terminal device such as a mobile phone or a PDA, a member of a thin film display, a substrate for an optical disk, a polarizing plate, and the like. The present invention relates to a biaxially oriented polyester film for double-sided pressure-sensitive adhesive tape used as a base material for a tape.

近年、携帯電話、PDAなどの携帯端末機器、デジタルカメラ、デジタルビデオカメラなどの電子・光学部品などにおいては、高機能化と並行して、薄型化や軽量化、さらには表示体のペーパー化などが図られている。例えば携帯電話は、表示の拡大化と携帯性とを向上させるために、構成される主要部品それぞれが薄膜化傾向にある。   In recent years, in mobile terminal devices such as mobile phones and PDAs, electronic and optical parts such as digital cameras and digital video cameras, etc., in parallel with higher functionality, thinner and lighter, and further, paper for display bodies, etc. Is planned. For example, in a mobile phone, in order to improve display enlargement and portability, each major component that is configured tends to be thin.

これらの部品の部材固定用として、一部の用途では粘着材層を転写するテープを使用して薄型化に対応しているが、この場合、芯材がないため、耐久性に劣るという問題が生じる。そこで、超薄膜の両面テープが多く開発されるようになり、特許文献1および2などには、基材として2〜6μmのポリエステルフィルムの両面に粘着剤層を有する粘着テープが開示されている。   For fixing parts of these parts, in some applications, tapes that transfer the adhesive material layer are used to support thinning, but in this case, there is no core material, so there is a problem of poor durability Arise. Accordingly, many ultra-thin double-sided tapes have been developed, and Patent Documents 1 and 2 disclose pressure-sensitive adhesive tapes having pressure-sensitive adhesive layers on both sides of a 2 to 6 μm polyester film as a base material.

しかしながら、上記文献には、粘着テープの厚さ構成と破断強度、粘着剤層の構成について開示されているが、基材ポリエステルフィルムについては具体的に記載されていない。   However, the above document discloses the thickness structure and breaking strength of the pressure-sensitive adhesive tape and the structure of the pressure-sensitive adhesive layer, but does not specifically describe the base polyester film.

特に近年、より部品間のクリアランスが狭くなり、10μm以下という極めて狭いクリアランスに要求される10μm未満の粘着テープについては、十分な粘着力を発揮するためには4μm以下の極めて薄いポリエステルフィルムを基材として使用しなければならない。   Particularly in recent years, the clearance between parts has become narrower, and for an adhesive tape of less than 10 μm required for an extremely narrow clearance of 10 μm or less, an extremely thin polyester film of 4 μm or less is used as a base material in order to exhibit sufficient adhesive force. Must be used as

また、クリアランスが狭くなるにつれ、粘着テープの厚さ振れが小さいものが要求されるようになってきているが、基材の厚さ振れが、粘着テープの厚さ振れに特に影響する。そのため、従来の極薄基材フィルムよりも厚さ振れの良い基材フィルムが要求されるようになった。   Further, as the clearance becomes narrower, the adhesive tape having a small thickness fluctuation is required, but the thickness fluctuation of the base material particularly affects the thickness fluctuation of the adhesive tape. Therefore, a base film having a better thickness swing than the conventional ultra-thin base film has been required.

すなわち、携帯電話、PDAなどの携帯端末機器、デジタルカメラ、デジタルビデオカメラなどの電子・光学部品において、部材固定用として粘着テープのさらなる薄膜化の要求が求められているが、薄膜化により、粘着テープが基材フィルムの厚さ振れに影響で接着部材に許容されるクリアランスを超えてしまう問題が残ったままである。   That is, there is a demand for further thinning of the adhesive tape for fixing components in electronic and optical parts such as mobile terminal devices such as mobile phones and PDAs, digital cameras, and digital video cameras. The problem remains that the tape exceeds the clearance allowed for the adhesive member due to the thickness fluctuation of the base film.

特開2005−105212号公報JP 2005-105212 A 特開2007−169327号公報JP 2007-169327 A

本発明は、上記の従来の問題点を解決しようとするものであり、巻取り性や作業性を向上させるだけでなく、10μm以下という極めて薄いクリアランスを要求される接着部材として好適な両面粘着テープ用二軸配向ポリエステルフィルムを提供することである。   The present invention is intended to solve the above-mentioned conventional problems, and not only improves winding properties and workability, but also a double-sided pressure-sensitive adhesive tape suitable as an adhesive member that requires an extremely thin clearance of 10 μm or less. It is to provide a biaxially oriented polyester film.

本発明者は、上記の解決課題について、鋭意検討した結果、以下に記載のフィルムを開発するに至った。   As a result of intensive studies on the above problems, the present inventors have developed the films described below.

すなわち、本発明の要旨は、面配向度が0.170〜0.190であり、120℃で3分間の収縮率がフィルム長手方向および幅方向ともに2.0%以下であり、厚さが1〜4μmであることを特徴とする両面粘着テープ用二軸配向ポリエステルフィルムに存する。   That is, the gist of the present invention is that the degree of plane orientation is 0.170 to 0.190, the shrinkage ratio at 120 ° C. for 3 minutes is 2.0% or less in both the film longitudinal direction and the width direction, and the thickness is 1 It exists in the biaxially-oriented polyester film for double-sided adhesive tapes characterized by being -4micrometer.

本発明の両面粘着テープ用二軸配向ポリエステルフィルムは、携帯電話、PDAなどの携帯端末機器、デジタルカメラ、デジタルビデオカメラなどの電子・光学部品の部材固定用の極めて薄いクリアランスにも用いられる粘着テープの基材フィルムとして好適であり、本発明の工業的価値は高い。   The biaxially oriented polyester film for double-sided pressure-sensitive adhesive tape of the present invention is an adhesive tape that is also used for extremely thin clearance for fixing members of electronic and optical components such as mobile terminal devices such as mobile phones and PDAs, digital cameras, and digital video cameras. Therefore, the industrial value of the present invention is high.

本発明のポリエステルフィルムは、押出口金から溶融押出される、いわゆる押出法により押し出した溶融ポリエステルシートを冷却した後、必要に応じ、延伸したフィルムである。   The polyester film of the present invention is a film stretched as necessary after cooling a melted polyester sheet extruded by a so-called extrusion method that is melt-extruded from an extrusion die.

本発明のフィルムを構成するポリエステルとは、ジカルボン酸と、ジオールとからあるいはヒドロキシカルボン酸とから重縮合によって得られるエステル基を含むポリマーを指す。ジカルボン酸としては、テレフタル酸、イソフタル酸、アジピン酸、アゼライン酸、セバシン酸、2,6−ナフタレンジカルボン酸、1,4−シクロヘキサンジカルボン酸等を、ジオールとしては、エチレングリコール、1,4−ブタンジオール、ジエチレングリコール、トリエチレングリコール、ネオペンチルグリコール、1,4−シクロヘキサンジメタノール、ポリエチレングリコール等を、ヒドロキシカルボン酸としては、p−ヒドロキシ安息香酸、6−ヒドロキシ−2−ナフトエ酸等をそれぞれ例示することができる。その製法としては、例えば、芳香族ジカルボン酸の低級アルキルエステルとグリコールとの間でエステル交換反応をさせるか、あるいは芳香族ジカルボン酸とグリコールとを直接エステル化させるかして、実質的に芳香族ジカルボン酸のビスグリコールエステル、またはその低重合体を形成させ、次いでこれを減圧下、加熱して 重縮合させる方法が採用される。   The polyester constituting the film of the present invention refers to a polymer containing an ester group obtained by polycondensation from a dicarboxylic acid and a diol or from a hydroxycarboxylic acid. Examples of dicarboxylic acids include terephthalic acid, isophthalic acid, adipic acid, azelaic acid, sebacic acid, 2,6-naphthalenedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid, and diols include ethylene glycol and 1,4-butane. Examples include diol, diethylene glycol, triethylene glycol, neopentyl glycol, 1,4-cyclohexanedimethanol, polyethylene glycol and the like, and examples of hydroxycarboxylic acid include p-hydroxybenzoic acid and 6-hydroxy-2-naphthoic acid. be able to. As the production method, for example, a transesterification reaction is carried out between a lower alkyl ester of an aromatic dicarboxylic acid and a glycol, or an aromatic dicarboxylic acid and a glycol are directly esterified to form a substantially aromatic compound. A method is employed in which a bisglycol ester of a dicarboxylic acid or a low polymer thereof is formed and then polycondensed by heating under reduced pressure.

かかるポリマーの代表的なものとして、ポリエチレンテレフタレートやポリエチレンー2、6ナフタレート等が例示される。これらのポリマーはホモポリマーであってもよく、また第3成分を共重合させたものでもよい。   Typical examples of such polymers include polyethylene terephthalate and polyethylene-2, 6 naphthalate. These polymers may be homopolymers or may be a copolymer of the third component.

本発明におけるポリエステルフィルムには、フィルム製膜時の巻き上げ工程や、粘着テープ作製時や使用時の作業性を向上させるため、表面を粗面化してフィルムに適度な滑り性が付与される。   The polyester film in the present invention is provided with an appropriate slipperiness by roughening the surface in order to improve the winding process at the time of film formation and the workability at the time of production and use of the adhesive tape.

具体的には、フィルムの表面を適当に粗面化するために、通常、平均粒径0.4〜2.0μm、好ましくは0.8〜1.5μmの粒子を通常0.1〜5.0重量%、好ましくは0.1〜3.0重量%、さらに好ましくは0.2〜2.0重量%含有させる。   Specifically, in order to appropriately roughen the surface of the film, particles having an average particle diameter of 0.4 to 2.0 [mu] m, preferably 0.8 to 1.5 [mu] m are usually 0.1 to 5. 0% by weight, preferably 0.1-3.0% by weight, more preferably 0.2-2.0% by weight.

かかる粒子の例としては炭酸カルシウム、炭酸マグネシウム、硫酸カルシウム、硫酸バリウム、リン酸リチウム、リン酸マグネシウム、リン酸カルシウム、フッ化リチウム、酸化アルミニウム、酸化ケイ素、酸化チタン、カオリン等の無機粒子やアクリル樹脂、グアナミン樹脂や架橋高分子微粉体等の有機粒子を挙げることができるが、これらに限定されるものではない。また、2成分以上を同時に用いてもよい。2成分以上用いる場合は、それらの全体の平均粒径および含有量が上記した範囲内にあることが好ましい。   Examples of such particles include inorganic particles such as calcium carbonate, magnesium carbonate, calcium sulfate, barium sulfate, lithium phosphate, magnesium phosphate, calcium phosphate, lithium fluoride, aluminum oxide, silicon oxide, titanium oxide, kaolin, acrylic resin, Although organic particles, such as a guanamine resin and a crosslinked polymer fine powder, can be mentioned, it is not limited to these. Two or more components may be used simultaneously. When two or more components are used, it is preferable that the average particle diameter and content thereof are in the above-described range.

平均粒径が0.4μm未満であったり、粒子の含有量が0.1重量%未満であったりする場合は、フィルム表面の粗面化が不足し、十分な巻取り作業性が得られないことがある。また、平均粒径が2.0μmを超える場合、粒子による突起が大きすぎて、突起周辺の厚さが大きくなり、接着部材に許容されるクリアランスを超えてしまう不具合が生じることがある。含有量が5.0重量%を超える場合、フィルム表面が粗面化しすぎて、粘着剤を均一に塗布することが困難となる場合がある。   When the average particle size is less than 0.4 μm or the particle content is less than 0.1% by weight, the film surface is insufficiently roughened and sufficient winding workability cannot be obtained. Sometimes. When the average particle size exceeds 2.0 μm, the protrusions due to the particles are too large, the thickness around the protrusions is increased, and there may be a problem that the clearance allowed for the adhesive member is exceeded. If the content exceeds 5.0% by weight, the film surface may become too rough and it may be difficult to uniformly apply the pressure-sensitive adhesive.

本発明においては上記したような方法により表面を適度に粗面化したフィルムを得るが、作業性や加工性を考慮すると、フィルム表面の平均粗さ(Ra)は通常0.03〜0.2μm、好ましくは0.04〜0.16μmの範囲となるように便宜、条件を選択する。 本発明におけるポリエステルフィルムに上記した粒子を添加する方法としては、特に限定されるものではなく、公知の方法を採用し得る。例えば、ポリエステルを製造する任意の段階において添加することができるが、好ましくはエステル化の段階、もしくはエステル交換反応終了後重縮合反応開始前の段階でエチレングリコール等に分散させたスラリーとして添加し重縮合反応を進めてもよい。また、ベント付き混練押出機を用い、エチレングリコールまたは水などに分散させた粒子のスラリーとポリエステル原料とをブレンドする方法、または、混練押出機を用い、乾燥させた粒子とポリエステル原料とをブレンドする方法などによって行われる。   In the present invention, a film having an appropriately roughened surface is obtained by the method as described above. In consideration of workability and workability, the average roughness (Ra) of the film surface is usually 0.03 to 0.2 μm. For convenience, the conditions are selected to be in the range of 0.04 to 0.16 μm. The method for adding the above-described particles to the polyester film in the present invention is not particularly limited, and a known method can be adopted. For example, it can be added at any stage for producing the polyester, but it is preferably added as a slurry dispersed in ethylene glycol or the like at the stage of esterification or before the start of the polycondensation reaction after completion of the transesterification reaction. The condensation reaction may proceed. Also, a method of blending a slurry of particles dispersed in ethylene glycol or water with a vented kneading extruder and a polyester raw material, or a blending of dried particles and a polyester raw material using a kneading extruder. It is done by methods.

本発明で使用するポリエステルの極限粘度は、フィルムにした時に0.40〜0.75dl/g、さらには0.50〜0.70dl/gとなるようにすることが好ましい。フィルムの極限粘度が0.40dl/g未満では、フィルムの機械的強度が弱くなる傾向があり、極限粘度が0.75を超える場合は、溶融粘度が高くなり、押出機に負荷がかかったり、製造コストがかかったりする上、厚さ振れが悪化する傾向がある。   The intrinsic viscosity of the polyester used in the present invention is preferably 0.40 to 0.75 dl / g, more preferably 0.50 to 0.70 dl / g when formed into a film. If the intrinsic viscosity of the film is less than 0.40 dl / g, the mechanical strength of the film tends to be weakened. If the intrinsic viscosity exceeds 0.75, the melt viscosity becomes high, and the extruder is loaded. In addition to manufacturing costs, the thickness fluctuation tends to deteriorate.

本発明におけるポリエステルは上記したポリエステル原料をエクストルーダーに代表される周知の溶融押出装置に供給し、当該ポリマーの融点以上の温度に加熱し溶融する。次いでスリット状のダイより溶融ポリマーを押出しながら、回転冷却ドラム状でガラス転移温度以下の温度になるよう急冷固化し、実質的に非晶状態の未配向シートを得る。このシートを二軸方向に延伸してフィルム化し、熱固定を施すことで得られる。この場合、延伸方法は逐次二軸延伸でも同時二軸延伸でもよい。また、必要に応じ、熱固定を施す前または後に再度縦および/または横方向に延伸してもよい。   The polyester in the present invention is melted by supplying the above-described polyester raw material to a known melt-extrusion apparatus represented by an extruder, and heating to a temperature equal to or higher than the melting point of the polymer. Next, while extruding the molten polymer from the slit-shaped die, it is rapidly cooled and solidified so that it is in the form of a rotary cooling drum or lower than the glass transition temperature to obtain a substantially amorphous unoriented sheet. This sheet is obtained by stretching in a biaxial direction to form a film and heat-setting. In this case, the stretching method may be sequential biaxial stretching or simultaneous biaxial stretching. Moreover, you may extend | stretch longitudinally and / or a horizontal direction again before or after performing heat setting as needed.

本発明においては十分な寸法安定性を得るため、フィルムの面配向度が0.170〜0.190、好ましくは0.170〜0.185になるように延伸倍率を面積倍率として16〜25倍、好ましくは18〜24倍とすることが好ましい。またフィルムの面配向度が0.170未満では、薄いクリアランスを要求される両面粘着シートの基材として十分に使用可能な厚さ振れの少ないフィルムを得ることができず、またフィルムの面配向が0.190を超えると横延伸時に破断し、製膜が困難になる。   In the present invention, in order to obtain sufficient dimensional stability, the film has a plane orientation of 0.170 to 0.190, preferably 0.170 to 0.185, and a draw ratio of 16 to 25 times as an area ratio. , Preferably 18 to 24 times. Also, if the degree of surface orientation of the film is less than 0.170, a film with little thickness fluctuation that can be used sufficiently as a base material for a double-sided pressure-sensitive adhesive sheet requiring thin clearance cannot be obtained, and the surface orientation of the film is not good. If it exceeds 0.190, the film will break during transverse stretching, making film formation difficult.

本発明のポリエステルフィルムの厚さは1〜4μm、好ましくは1.5〜3μmである。厚さが4μmを超えると、十分な粘着力を備えた粘着層を付与した時に薄膜両面テープを提供する本発明の目的が達せられない。厚さが1μmより薄くなるとフィルムの腰が損なわれ取り扱いが困難になり作業性が悪化する。   The thickness of the polyester film of the present invention is 1 to 4 μm, preferably 1.5 to 3 μm. If the thickness exceeds 4 μm, the object of the present invention for providing a thin film double-sided tape cannot be achieved when an adhesive layer having sufficient adhesive force is applied. When the thickness is less than 1 μm, the waist of the film is damaged, handling becomes difficult, and workability deteriorates.

本発明のポリエステルフィルムの収縮率は、120℃において2.0%以下、好ましくは1.5%以下、さらに好ましくは1.0%以下である。2.0%を超えると粘着基材として使用した時、フィルムの収縮によって部材のずれが生じたり、粘着剤の高温保持力が損なわれたりする。   The shrinkage rate of the polyester film of the present invention is 2.0% or less, preferably 1.5% or less, more preferably 1.0% or less at 120 ° C. When it exceeds 2.0%, when used as an adhesive substrate, the member may be displaced due to shrinkage of the film, or the high temperature holding power of the adhesive may be impaired.

本発明のポリエステルフィルムの長手方向と幅方向の破断強度は、通常200MPa以上、好ましくは250MPa以上である。優れた強度を有する粘着テープを得ることができる。   The breaking strength in the longitudinal direction and the width direction of the polyester film of the present invention is usually 200 MPa or more, preferably 250 MPa or more. An adhesive tape having excellent strength can be obtained.

以下に実施例を挙げて本発明をさらに詳細に説明するが、本発明はその主旨を越えない限り、以下の実施例に限定されるものではない。なお、実施例および比較例における評価方法やサンプルの処理方法は下記のとおりである。また、実施例および比較例中の「部」は「重量部」を示す。
(1)極限粘度の測定方法
ポリエステルに非相溶な他のポリマー成分および顔料を除去したポリエステル1gを精秤し、フェノール/テトラクロロエタン=50/50(重量比)の混合溶媒100mlを加えて溶解させ、30℃で測定した。
(2)平均粒径(d50)
(株)島津製作所社製遠心沈降式粒度分布測定装置SA−CP3型を用いてスト−クスの抵抗値にもとづく沈降法によって粒子の大きさを測定した。
(3)平均粗さRaの測定方法
小坂研究所製表面粗さ測定機SE3500を使用し、JIS−B−0601−1994の方法に準じてRaを測定した。なおカットオフ値は80μmとして測定した。
(4)基材ポリエステルフィルムの厚さの測定方法
試料の重量、長さ、幅、密度より次式にて測定した。
EXAMPLES The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to the following examples unless it exceeds the gist of the present invention. In addition, the evaluation method and the processing method of a sample in an Example and a comparative example are as follows. Further, “parts” in Examples and Comparative Examples represents “parts by weight”.
(1) Method for measuring intrinsic viscosity 1 g of polyester from which other polymer components and pigments incompatible with polyester have been removed are precisely weighed and dissolved by adding 100 ml of a mixed solvent of phenol / tetrachloroethane = 50/50 (weight ratio). And measured at 30 ° C.
(2) Average particle diameter (d50)
The particle size was measured by a sedimentation method based on the resistance value of the stock using a centrifugal sedimentation type particle size distribution analyzer SA-CP3 manufactured by Shimadzu Corporation.
(3) Measuring method of average roughness Ra Ra was measured according to the method of JIS-B-0601-1994 using the surface roughness measuring machine SE3500 by Kosaka Laboratory. The cut-off value was measured as 80 μm.
(4) Method for measuring the thickness of the base polyester film The thickness was measured by the following formula from the weight, length, width and density of the sample.

厚さ=(試料の重量)÷((試料の長さ)×(試料の幅)×(試料の密度))
(5)面配向度の測定方法
アタゴ光学社製アッベ式屈折計を用い、フィルム面内の屈折率の最大値nγ、それに直角の方向の屈折率nβ、およびフィルムの厚さ方向の屈折率nαを測定し、次式より面配向度を算出した。なお、屈折率の測定は、ナトリウムD線を用い、23℃で行った。
Thickness = (sample weight) ÷ ((sample length) x (sample width) x (sample density))
(5) Method of measuring degree of plane orientation Using an Abbe refractometer manufactured by Atago Optical Co., Ltd., the maximum refractive index nγ in the film plane, the refractive index nβ in the direction perpendicular to it, and the refractive index nα in the thickness direction of the film And the degree of plane orientation was calculated from the following equation. The refractive index was measured at 23 ° C. using sodium D line.

面配向度(ΔP)=(nγ+nβ)÷2−nα
(6)収縮率の測定方法
試料を無張力状態で所定の温度(120℃)に保ったオーブン中、3分間熱処理し、その前後の試料の長さを測定して次式にて算出した。なお、フィルムの縦方向(MD)と幅方向(TD)のそれぞれについて測定した。
Plane orientation degree (ΔP) = (nγ + nβ) ÷ 2-nα
(6) Measuring method of shrinkage rate The sample was heat treated for 3 minutes in an oven maintained at a predetermined temperature (120 ° C.) in a tensionless state, and the length of the sample before and after that was measured and calculated by the following formula. In addition, it measured about each of the vertical direction (MD) and width direction (TD) of a film.

収縮率={(熱処理前のサンプル長)−(熱処理後のサンプル長)}/(熱処理前のサンプル長)×100
(7)破断強度の測定方法
インテスコ社製引張り試験機モデル2001型を用いて、温度23℃、湿度50%RHに調節された室内において長さ(チャック間)50mm、幅15mmの試料サンプルを200mm/分の歪み速度で引張り、フィルム破断時の荷重を測定し、下記式により破断強度を求めた。なお、フィルムの縦方向(MD)と幅方向(TD)のそれぞれについて測定した。
Shrinkage rate = {(sample length before heat treatment) − (sample length after heat treatment)} / (sample length before heat treatment) × 100
(7) Measuring method of breaking strength Using a tensile tester model 2001 type manufactured by Intesco Corporation, a sample sample having a length (between chucks) of 50 mm and a width of 15 mm in a room adjusted to a temperature of 23 ° C. and a humidity of 50% RH is 200 mm. The film was pulled at a strain rate of / min, the load at the time of film breakage was measured, and the break strength was determined by the following formula. In addition, it measured about each of the vertical direction (MD) and width direction (TD) of a film.

破断強度(MPa)=切断時の荷重(N)/試料フィルムの断面積(mm2
(8)フィルムの厚さ振れの測定方法
安立電気社製連続厚み測定機にて、長手方向に3m測定し、最大、最小および平均厚さを測定し、次式により厚さ斑を測定し、10回の測定の平均値を厚さ振れとした。
Breaking strength (MPa) = Load at cutting (N) / Cross-sectional area of sample film (mm 2 )
(8) Measuring method of film thickness fluctuation With a continuous thickness measuring machine manufactured by Anritsu Electric Co., Ltd., measuring 3 m in the longitudinal direction, measuring the maximum, minimum and average thicknesses, measuring the thickness unevenness by the following formula, The average value of 10 measurements was defined as thickness fluctuation.

厚さ斑=100×(フィルム最大厚さ−フィルム最小厚さ)/フィルム平均厚さ
(9)粘着力の測定方法
実施例、比較例にて得られた粘着テープを25mm幅のサンプルにてJIS Z 1528に準じて測定した。すなわち、試験片の一方の粘着面の25mmの長さの部分をステンレス鋼製金属板に貼合した後に、他の一方の面の剥離フィルムを剥ぎ取り、試験片とほぼ同じ大きさのJIS C 2318に規定する厚さ25μmのポリエチレンテレフタレートフィルムを貼り合わせて圧着し、JIS Z 0237の10(粘着力)により、試験板(ステンレス鋼製金属板)に対する180°引き剥がし粘着力を求めた。
(10)粘着剤層の厚さ
両面テープ(剥離フィルムA/粘着剤層A/基材ポリエステルフィルム/粘着剤層B/剥離フィルムB)を電子顕微鏡でテープの断面写真を撮影し、粘着剤層の厚さを計測した。測定は10回実施し、10回の平均値を粘着剤層の厚さとした。
(11)剥離フィルムの剥離力
50mm幅のサンプルにて、測定する側と逆側の剥離フィルムを剥ぎ取り、露出した粘着剤面をガラス板に貼付し、測定する側の剥離フィルムを引張試験機をもちいて、300mm/分の速度で180°方向に引き剥がす際の抵抗を測定し、剥離力とした。
(12)適合性;
両面粘着テープを部品間のクリアランスが10μm以下となる部分に適用して、該クリアランスに部品がずれなく適合させることができるか否かで判断し、適合できるものを「○」、適合できないものを「×」とした。
Thickness unevenness = 100 × (maximum film thickness−minimum film thickness) / average film thickness (9) Measuring method of adhesive strength The adhesive tape obtained in Examples and Comparative Examples was JIS with a 25 mm wide sample. Measured according to Z 1528. That is, after pasting a 25 mm long part of one adhesive surface of a test piece to a stainless steel metal plate, the release film on the other side was peeled off, and JIS C having the same size as the test piece was removed. A polyethylene terephthalate film having a thickness of 25 μm specified in 2318 was bonded and pressure-bonded, and the adhesive strength was determined by peeling 180 ° from the test plate (stainless steel metal plate) according to 10 (adhesive strength) of JIS Z 0237.
(10) Pressure-sensitive adhesive layer thickness Double-sided tape (peeling film A / pressure-sensitive adhesive layer A / base polyester film / pressure-sensitive adhesive layer B / peeling film B) is taken with an electron microscope and a cross-sectional photograph of the tape is taken. The thickness of was measured. The measurement was carried out 10 times, and the average value of 10 times was taken as the thickness of the pressure-sensitive adhesive layer.
(11) Peeling force of peeling film With a 50 mm width sample, the peeling film on the side opposite to the side to be measured is peeled off, the exposed pressure-sensitive adhesive surface is stuck on a glass plate, and the peeling film on the side to be measured is tension tester Was used to measure the resistance at the time of peeling in the direction of 180 ° at a speed of 300 mm / min.
(12) compatibility;
Apply double-sided adhesive tape to the part where the clearance between parts is 10 μm or less, and judge whether the part can be fitted to the clearance without any deviation. It was set as “x”.

以下の実施例および比較例にて使うポリエステル原料は次の方法にて製造した。
<ポリエステルの製造>
テレフタル酸ジメチル100重量部、エチレングリコール60重量部を出発原料とし、触媒として、酢酸マグネシウム・四水塩0.09重量部を反応器に取り、反応開始温度を150℃とし、メタノールの留去とともに徐々に反応温度を上昇させ、3時間後230℃とした。4時間後、実質的にエステル交換反応を終了させた。この反応混合物にエチルアシッドフォスフェ−ト0.04部を添加した後、平均粒子1.1μmの球状有機架橋粒子0.5重量部および三酸化アンチモン0.03部を加えて、4時間重縮合反応を行った。一方、圧力は常圧より徐々に減じ、最終的には0.3mmHgとした。反応開始後、反応槽の攪拌動力の変化により、極限粘度0.65に相当する時点で反応を停止し、窒素加圧下ポリマーを吐出させ、ポリエステル(A1)のチップを得た。この、ポリエステルの極限粘度は0.65であった。
実施例1:
<フィルムの製造>
ポリエステル(A1)チップを、ベント付き二軸押出機により、290℃で溶融押出し、静電印加密着法を用いて表面温度を40℃に設定した冷却ロール上で冷却固化して未延伸シートを得た。次いで、90℃で縦方向に3.0倍延伸した後、さらに83℃で1.4倍延伸し、テンターに導き、110℃で横方向に4.5倍延伸し、さらに225℃で熱処理を行い、厚さ2.0μmの基材ポリエステルフィルムを得た。
The polyester raw materials used in the following examples and comparative examples were produced by the following method.
<Manufacture of polyester>
Starting with 100 parts by weight of dimethyl terephthalate and 60 parts by weight of ethylene glycol, 0.09 parts by weight of magnesium acetate tetrahydrate as a catalyst is taken in the reactor, the reaction start temperature is 150 ° C., and methanol is distilled off. The reaction temperature was gradually raised to 230 ° C. after 3 hours. After 4 hours, the transesterification reaction was substantially terminated. After adding 0.04 part of ethyl acid phosphate to the reaction mixture, 0.5 part by weight of spherical organic crosslinked particles having an average particle size of 1.1 μm and 0.03 part of antimony trioxide were added, and polycondensation was performed for 4 hours. Reaction was performed. On the other hand, the pressure was gradually reduced from normal pressure, and finally 0.3 mmHg. After the start of the reaction, the reaction was stopped at a time corresponding to an intrinsic viscosity of 0.65 due to a change in stirring power of the reaction vessel, and the polymer was discharged under nitrogen pressure to obtain a polyester (A1) chip. The intrinsic viscosity of this polyester was 0.65.
Example 1:
<Manufacture of film>
A polyester (A1) chip is melt-extruded at 290 ° C. with a vented twin-screw extruder, and cooled and solidified on a cooling roll set at a surface temperature of 40 ° C. using an electrostatic application adhesion method to obtain an unstretched sheet. It was. Next, after stretching 3.0 times in the longitudinal direction at 90 ° C, further stretching 1.4 times at 83 ° C, leading to a tenter, stretching 4.5 times in the transverse direction at 110 ° C, and further heat treating at 225 ° C. The substrate polyester film having a thickness of 2.0 μm was obtained.

このポリエステルフィルムの特性を表1に示す。
<粘着剤組成物(塗工液)の製造>
重量平均分子量80万のアクリル酸エステル系重合体(アクリル酸ブチル95重量%、アクリル酸2重量%およびメタクリル酸メチル3重量%)、濃度30重量%の酢酸エチル溶液100重量部に対し、粘着性付与剤[荒川化学工業社製、商品名「パインクリスタルKE−359」、ロジンエステル系、軟化点94〜104℃、酸価10〜20mgKOH/g]30重量部、およびイソシアネート系架橋剤[東洋インキ製造社製、商品名「BHS8515」、固形分濃度37.5%]1重量部を加えてトルエンで希釈し、固形分濃度20重量%の粘着剤組成物(塗工液)を製造した。
<両面粘着テープの製造>
軽剥離型ポリエチレンテレフタレート(PET)剥離フィルム[三菱樹脂社製、商品名「ダイアホイルMRF38」、フィルム厚さ38μm]の剥離処理面に前記塗工液を、乾燥後の膜厚が3.5μmになるようにナイフコーターで塗布し、100℃で1分間乾燥後、前記の厚さ2.0μmのポリエステルフィルムを貼合して、片面粘着フィルムを得た。
The properties of this polyester film are shown in Table 1.
<Manufacture of an adhesive composition (coating liquid)>
Adhesiveness to 100 parts by weight of an ethyl acetate solution having a weight average molecular weight of 800,000 acrylate polymer (95% by weight of butyl acrylate, 2% by weight of acrylic acid and 3% by weight of methyl methacrylate) and a concentration of 30% by weight Giving agent [Arakawa Chemical Industries, trade name “Pine Crystal KE-359”, rosin ester type, softening point 94-104 ° C., acid value 10-20 mg KOH / g] 30 parts by weight, and isocyanate type cross-linking agent [Toyo Ink 1 part by weight, manufactured by the manufacturer, trade name “BHS8515”, solid concentration 37.5%] was added and diluted with toluene to produce a pressure-sensitive adhesive composition (coating solution) having a solid concentration of 20% by weight.
<Manufacture of double-sided adhesive tape>
Lightly-peelable polyethylene terephthalate (PET) release film [Mitsubishi Resin Co., Ltd., trade name “Diafoil MRF38”, film thickness: 38 μm] After coating with a knife coater and drying at 100 ° C. for 1 minute, the polyester film having a thickness of 2.0 μm was pasted to obtain a single-sided adhesive film.

次いで重剥離型PET剥離フィルム[三菱樹脂社製、商品名「ダイアホイルMRX38」、フィルム厚さ38μm]の剥離処理面に前記塗工液を、乾燥後の膜厚が3.5μmになるようにナイフコーターで塗布し、100℃で1分間乾燥後、前記の片面粘着フィルムのPET面と貼合して両面粘着テープを製造した。   Next, the coating liquid is applied to the release-treated surface of a heavy release type PET release film [trade name “Diafoil MRX38”, film thickness: 38 μm, manufactured by Mitsubishi Plastics Co., Ltd.] so that the film thickness after drying becomes 3.5 μm. It apply | coated with the knife coater, and after drying for 1 minute at 100 degreeC, it bonded with the PET surface of the said single-sided adhesive film, and manufactured the double-sided adhesive tape.

得られた両面粘着テープの軽剥離型PET剥離フィルムの剥離力は15mN/10mmであり、重剥離型PETフィルムの剥離力は30mN/10mmであった。この両面テープの特性を下記表1に示す。
実施例2:
実施例1のフィルムの製造において、90℃で縦方向に3.0倍延伸した後、さらに83℃で1.5倍延伸し、テンターに導き、110℃で横方向に4.7倍延伸した以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を表1に示す。
実施例3:
実施例1のフィルムの製造において、フィルムの厚さを1.5μmにした以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を表1に示す。
実施例4:
実施例1のフィルムの製造において、フィルムの厚さを4.0μmにした以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し粘着剤層の厚さを2.5μmとした以外は実施例1と同様の方法で両面粘着テープを製造した。
このポリエステルフィルムおよび両面粘着テープの特性を表1に示す。
実施例5:
実施例1のフィルムの製造において、熱固定温度を210℃とした以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を表1に示す。
比較例1:
実施例1のフィルムの製造において、90℃で縦方向に3.0倍延伸した後、さらに83℃で1.2倍延伸し、テンターに導き、110℃で横方向に4.2倍延伸した以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を下記表2に示す。
比較例2:
実施例1のフィルムの製造において、90℃で縦方向に3.0倍延伸した後、さらに83℃で1.8倍延伸し、テンターに導き、110℃で横方向に4.8倍延伸した以外は、実施例1と同様の方法でポリエステルフィルムを得たが、横延伸時に破断が多発し、連続して製膜することが困難であった。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を表2に示す。
比較例3:
実施例1のフィルムの製造において、フィルムの厚さを6.0μmにした以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し粘着剤層の厚さを1.5μmとした以外は実施例1と同様の方法で両面粘着テープを製造した。
このポリエステルフィルムおよび両面粘着テープの特性を表2に示す。
比較例4:
実施例1のフィルムの製造において、熱固定温度を190℃とした以外は、実施例1と同様の方法でポリエステルフィルムを得た。得られた基材フィルムを使用し実施例1と同様の方法で両面粘着テープを製造した。このポリエステルフィルムおよび両面粘着テープの特性を表2に示す。
The peel strength of the lightly peelable PET peel film of the obtained double-sided pressure-sensitive adhesive tape was 15 mN / 10 mm, and the peel strength of the heavy peelable PET film was 30 mN / 10 mm. The characteristics of this double-sided tape are shown in Table 1 below.
Example 2:
In the production of the film of Example 1, the film was stretched 3.0 times in the machine direction at 90 ° C., further stretched 1.5 times at 83 ° C., led to a tenter, and stretched 4.7 times in the transverse direction at 110 ° C. Except for the above, a polyester film was obtained in the same manner as in Example 1. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The characteristics of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 1.
Example 3:
In the production of the film of Example 1, a polyester film was obtained in the same manner as in Example 1 except that the thickness of the film was 1.5 μm. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The characteristics of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 1.
Example 4:
In the production of the film of Example 1, a polyester film was obtained in the same manner as in Example 1 except that the thickness of the film was 4.0 μm. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 except that the obtained base film was used and the thickness of the pressure-sensitive adhesive layer was 2.5 μm.
The characteristics of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 1.
Example 5:
In the production of the film of Example 1, a polyester film was obtained in the same manner as in Example 1 except that the heat setting temperature was 210 ° C. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The characteristics of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 1.
Comparative Example 1:
In the production of the film of Example 1, the film was stretched 3.0 times in the machine direction at 90 ° C., then stretched 1.2 times at 83 ° C., led to a tenter, and stretched 4.2 times in the transverse direction at 110 ° C. Except for the above, a polyester film was obtained in the same manner as in Example 1. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The properties of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 2 below.
Comparative Example 2:
In the production of the film of Example 1, the film was stretched 3.0 times in the machine direction at 90 ° C., further stretched 1.8 times at 83 ° C., led to a tenter, and stretched 4.8 times in the transverse direction at 110 ° C. Except for the above, a polyester film was obtained in the same manner as in Example 1. However, breakage occurred frequently during transverse stretching, and it was difficult to continuously form a film. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The properties of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 2.
Comparative Example 3:
In the production of the film of Example 1, a polyester film was obtained in the same manner as in Example 1 except that the thickness of the film was 6.0 μm. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 except that the obtained base film was used and the thickness of the pressure-sensitive adhesive layer was 1.5 μm.
The properties of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 2.
Comparative Example 4:
In the production of the film of Example 1, a polyester film was obtained in the same manner as in Example 1 except that the heat setting temperature was 190 ° C. A double-sided pressure-sensitive adhesive tape was produced in the same manner as in Example 1 using the obtained base film. The properties of this polyester film and double-sided pressure-sensitive adhesive tape are shown in Table 2.

Figure 2012135951
Figure 2012135951

Figure 2012135951
Figure 2012135951

本発明のフィルムは、例えば、極めて薄いクリアランスが要求される用途において好適に使用することができる。   The film of the present invention can be suitably used, for example, in applications that require extremely thin clearance.

Claims (1)

面配向度が0.170〜0.190であり、120℃で3分間の収縮率がフィルム長手方向および幅方向ともに2.0%以下であり、厚さが1〜4μmであることを特徴とする両面粘着テープ用二軸配向ポリエステルフィルム。 The degree of plane orientation is 0.170 to 0.190, the shrinkage rate for 3 minutes at 120 ° C. is 2.0% or less in both the film longitudinal direction and the width direction, and the thickness is 1 to 4 μm. Biaxially oriented polyester film for double-sided adhesive tape.
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JP2012136634A (en) * 2010-12-27 2012-07-19 Mitsubishi Plastics Inc Double-sided pressure-sensitive adhesive tape
JP2013014723A (en) * 2011-07-06 2013-01-24 Dic Corp Double-sided adhesive tape
JP2014118485A (en) * 2012-12-17 2014-06-30 Fujimori Kogyo Co Ltd Adhesive layer and adhesive film
JP2015093981A (en) * 2013-11-14 2015-05-18 積水化学工業株式会社 Adhesive tape
JP2020073683A (en) * 2018-12-27 2020-05-14 藤森工業株式会社 Adhesive layer and adhesive film

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