JP2014088572A - Double side pressure-sensitive adhesive sheet for fixing polishing material - Google Patents
Double side pressure-sensitive adhesive sheet for fixing polishing material Download PDFInfo
- Publication number
- JP2014088572A JP2014088572A JP2013268971A JP2013268971A JP2014088572A JP 2014088572 A JP2014088572 A JP 2014088572A JP 2013268971 A JP2013268971 A JP 2013268971A JP 2013268971 A JP2013268971 A JP 2013268971A JP 2014088572 A JP2014088572 A JP 2014088572A
- Authority
- JP
- Japan
- Prior art keywords
- sensitive adhesive
- pressure
- adhesive layer
- adhesive sheet
- double
- 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.)
- Granted
Links
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- 238000005498 polishing Methods 0.000 title abstract description 65
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Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本発明は、研磨材を研磨装置へ固定するための研磨材固定用両面感圧接着シートに関する。 The present invention relates to a double-sided pressure-sensitive adhesive sheet for fixing an abrasive for fixing an abrasive to a polishing apparatus.
従来、自動車、光学機器、半導体等の分野では様々な部品、部材の表面研磨が行われている。例えば、液晶ディスプレイ用ガラス、ハードディスク用基板、光学レンズ、シリコンウェハ等の基板の鏡面研磨は、硬質樹脂パッドや研磨布等の研磨材と両面感圧接着シーを貼り合せた研磨部材を、研磨装置に貼り、研磨液を用いて行われている。 Conventionally, surface polishing of various parts and members has been performed in the fields of automobiles, optical devices, semiconductors, and the like. For example, mirror polishing of substrates such as glass for liquid crystal displays, substrates for hard disks, optical lenses, silicon wafers, etc., a polishing member with a polishing material such as a hard resin pad or polishing cloth and a double-sided pressure sensitive adhesive sheet bonded It is carried out using a polishing liquid.
その中でも例えば、被研磨体がハードディスク用基板のときは、表面を鏡面研磨する必要があるが、用いる研磨材や両面感圧接着シートには、表面に数ミクロンレベルの凹凸（粗さともいう）が存在している。 Among them, for example, when the object to be polished is a hard disk substrate, the surface needs to be mirror-polished, but the polishing material used and the double-sided pressure-sensitive adhesive sheet have unevenness on the surface of several microns (also called roughness). Is present.
そして研磨工程は、例えば研磨材を、両面感圧接着シートを介して研磨装置の研磨定盤に貼り付け、研磨材を馴染ませるための「ドレッシング」という仮研磨を行った後に、４０℃雰囲気下で研磨が実施される。この研磨中に、両面感圧接着シートを含む研磨部材は数百ｇ／ｃｍ2の圧力とせん断方向の力を受けることになる。 In the polishing step, for example, an abrasive is attached to a polishing surface plate of a polishing apparatus via a double-sided pressure-sensitive adhesive sheet, and after performing a temporary polishing called “dressing” for familiarizing the abrasive, an atmosphere of 40 ° C. Polishing is carried out. During this polishing, the polishing member including the double-sided pressure-sensitive adhesive sheet is subjected to a pressure of several hundred g / cm 2 and a force in the shear direction.
両面感圧接着シートは、研磨材への強い密着性を得るために従来からある工業用途向けの凝集力の高い感圧接着剤が用いられていた。このような感圧接着剤は研磨材や研磨定盤への見かけの密着力を得やすいが、凝集力が強すぎて柔軟性に欠けるために、研磨定盤に貼り付けたままの形状を維持し、研磨材に微小な凹凸や粗さがのこったまま、研磨工程が進行する。そして凹凸の存在が研磨後の被研磨体表面の仕上が悪化させ、ハードディスク自体の品質や収率を低下させていた。そのため両面感圧接着シートに、研磨材を平滑に固定できる等の特性が求められていた。 For the double-sided pressure-sensitive adhesive sheet, a conventional pressure-sensitive adhesive having high cohesive force for industrial use has been used in order to obtain strong adhesion to the abrasive. Such pressure-sensitive adhesives are easy to obtain an apparent adhesion to abrasives and polishing surface plates, but because they are too cohesive and lack flexibility, they maintain their shape as they are attached to the polishing surface plate. However, the polishing process proceeds with the fine irregularities and roughness remaining on the abrasive. And the presence of the irregularities deteriorates the finish of the surface of the polished object after polishing, and deteriorates the quality and yield of the hard disk itself. Therefore, characteristics such as the ability to fix the abrasive smoothly to the double-sided pressure-sensitive adhesive sheet have been demanded.
そこで、両面感圧接着シートの平滑性、即ち感圧接着剤層の表面平滑性を高めるために、感圧接着剤層と接する剥離シートに、表面が平滑なフィルム剥離ライナーを使う方法が行われた。しかし、フィルム剥離ライナーを使用すると、感圧接着剤層の表面が極端に平滑になるため、研磨材を研磨装置に貼る場合に、感圧接着剤層と研磨定盤の界面に大きな空気溜まりが生じやすく、その空気により、研磨材が平滑に固定できなかった。 Therefore, in order to improve the smoothness of the double-sided pressure-sensitive adhesive sheet, that is, the surface smoothness of the pressure-sensitive adhesive layer, a method of using a film release liner having a smooth surface for the release sheet in contact with the pressure-sensitive adhesive layer is performed. It was. However, when a film release liner is used, the surface of the pressure-sensitive adhesive layer becomes extremely smooth. Therefore, when an abrasive is applied to a polishing apparatus, a large air pocket is formed at the interface between the pressure-sensitive adhesive layer and the polishing surface plate. It was easy to occur, and the abrasive could not be fixed smoothly by the air.
また、両面感圧接着シートの基材（芯材）にウレタン発泡体などの緩衝材を使用して緩和性を得る方法が半導体研磨の分野では採用されている。しかし、前記発泡体は感圧接着剤との密着性が低く、厚みのバラつきが大きいため、ハードディスク研磨では使用することが難しい。 Further, a method of obtaining relaxation by using a cushioning material such as urethane foam for the base material (core material) of the double-sided pressure-sensitive adhesive sheet is employed in the field of semiconductor polishing. However, the foam is difficult to use in hard disk polishing because of its low adhesion to the pressure sensitive adhesive and large variation in thickness.
一方、研磨は、研磨液を用いる場合が多く、そのｐＨは約１〜１２で、過酸化水素水を
含有する場合もある。そのため両面感圧接着シートに耐薬品性が必要とされる。そして研
磨効率の向上の点から、長時間連続使用される場合が多くなってきた。
On the other hand, polishing often uses a polishing liquid, and has a pH of about 1 to 12 and may contain hydrogen peroxide. Therefore, chemical resistance is required for the double-sided pressure-sensitive adhesive sheet. And from the point of improvement of polishing efficiency, it has been increasingly used continuously for a long time.
そのため研磨定盤と接する両面感圧接着シート表面の粗さが大きいままであると、研磨定盤と両面感圧接着シートの界面に研磨液が侵入し、密着性が徐々に低化し、研磨時に加わる力に耐えきれず、研磨定盤から剥がれて被研磨体を損傷する等問題が生じていた。 Therefore, if the roughness of the surface of the double-sided pressure-sensitive adhesive sheet in contact with the polishing surface plate remains large, the polishing liquid enters the interface between the polishing surface plate and the double-sided pressure-sensitive adhesive sheet, and the adhesiveness gradually decreases. Inability to withstand the force applied, problems such as peeling from the polishing surface plate and damaging the object to be polished occurred.
そこで、特許文献１および２には本発明と用途は異なるが、粗面密着性や応力緩和に関する感圧接着シートが提案されている。 Therefore, Patent Documents 1 and 2 propose a pressure-sensitive adhesive sheet relating to rough surface adhesion and stress relaxation, although the application is different from that of the present invention.
特許文献１では、アクリル系光重合性組成物を用い、各感圧接着剤層の溶剤不溶分に差を設ける旨が記載されている。しかし、溶剤不溶分が高いために、研磨材表面の微小な粗さを緩和しにくい。さらに感圧接着剤組成にアクリル酸を使用しているため、研磨液耐性が悪く研磨中の振動で研磨材や研磨定盤から剥離する問題があった。 Patent Document 1 describes that an acrylic photopolymerizable composition is used and a difference is provided in the solvent insoluble content of each pressure-sensitive adhesive layer. However, since the solvent insoluble content is high, it is difficult to reduce the fine roughness of the surface of the abrasive. Furthermore, since acrylic acid is used for the pressure-sensitive adhesive composition, there is a problem that the resistance to the polishing liquid is poor and the vibration during polishing causes separation from the abrasive and the polishing surface plate.
また、特許文献２では、感圧接着シート全体の１０％伸張応力が約１０Ｎに調整する旨が記載されている。しかし研磨材とのラミネートを考えた場合、感圧接着シートが柔らかいため、平坦性が要求される研磨材がカールしてしまうという問題があった。また、その柔軟性が原因で研磨時に加わる力に耐えきれずに剥離するという問題があった。 Patent Document 2 describes that the 10% elongation stress of the entire pressure-sensitive adhesive sheet is adjusted to about 10N. However, when considering a laminate with an abrasive, the pressure-sensitive adhesive sheet is soft, and there is a problem that an abrasive requiring flatness is curled. Further, due to its flexibility, there is a problem that it peels without being able to withstand the force applied during polishing.
また、特許文献３には、ドライ条件下における特に研磨材への密着性を向上させるための方法が提案されている。特許文献３には、水酸基系熱活性型アクリル接着剤とフェノール樹脂とからなるガラス転移温度が２０℃以上のホットメルト接着剤を用いる旨が記載されている。しかし、ガラス転移温度が高く、架橋剤としてエポキシ樹脂を使用しているため、テープの柔軟性が無く研磨材や研磨定盤側感圧接着剤の微小な粗さを緩和せずに被研磨体の平滑性が得にくいという問題があった。 Patent Document 3 proposes a method for improving the adhesion to a polishing material, particularly under dry conditions. Patent Document 3 describes that a hot melt adhesive having a glass transition temperature of 20 ° C. or higher composed of a hydroxyl group-based thermally active acrylic adhesive and a phenol resin is used. However, since the glass transition temperature is high and epoxy resin is used as a cross-linking agent, there is no flexibility of the tape, and the object to be polished is not relaxed without reducing the fine roughness of the abrasive or polishing surface plate side pressure sensitive adhesive. There was a problem that it was difficult to obtain smoothness.
本発明は、研磨材を研磨装置へ平滑に固定できることで被研磨体の鏡面研磨が容易にできて、さらに研磨液に曝されたときにも密着性を維持できる耐薬液性が良好な研磨材固定用両面感圧接着シートの提供を目的とする。 The present invention is a polishing material with good chemical resistance that can easily fix the polishing material to a polishing apparatus so that it can be easily mirror-polished and can maintain adhesion even when exposed to a polishing liquid. An object is to provide a double-sided pressure-sensitive adhesive sheet for fixing.
以上の課題を解決するために、本発明者は鋭意研究し、本発明に至った。 In order to solve the above-mentioned problems, the present inventor has intensively studied to arrive at the present invention.
即ち、第１の発明は、プラスチック基材の一方の面に感圧接着剤層（ａ）が、もう一方の面に感圧接着剤層（ｂ）がそれぞれ設けられてなる研磨材固定用両面感圧接着シートであって、
感圧接着剤層（ａ）の、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（１）において、Ａが−０．５０〜−０．２０であることを特徴とする研磨材固定用両面感圧接着シートに関する。
ｌｏｇ Ｇ（ｔ）＝Ａｌｏｇ ｔ＋Ｂ ・・・式（１）
〔式（１）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＡおよびＢは定数をそれぞれ表す。〕
That is, the first aspect of the present invention is an abrasive fixing double-sided surface in which a pressure-sensitive adhesive layer (a) is provided on one side of a plastic substrate and a pressure-sensitive adhesive layer (b) is provided on the other side. A pressure sensitive adhesive sheet,
The following formula (1), which is an approximate straight line representing the time dependence of the relaxation modulus at 40 ° C. of the pressure-sensitive adhesive layer (a), is characterized in that A is −0.50 to −0.20. The present invention relates to a double-sided pressure-sensitive adhesive sheet for fixing an abrasive.
log G (t) = Alog t + B (1)
[In formula (1), t represents time, G (t) represents relaxation modulus, and A and B represent constants, respectively. ]
また、第２の発明は、プラスチック基材の一方の面に感圧接着剤層（ａ）が、もう一方の面に感圧接着剤層（ｂ）が、設けられてなる研磨材固定用両面感圧接着シートであって、前記研磨材固定用両面感圧接着シートの、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（２）において、Ｃが−０．５５〜−０．２５であることを特徴とする研磨材固定用両面感圧接着シートに関する。
ｌｏｇＧ（ｔ）＝Ｃｌｏｇ ｔ＋Ｄ ・・・式（２）
〔式（２）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＣおよびＤは定数をそれぞれ表す。〕
The second aspect of the invention is an abrasive fixing double-sided surface in which a pressure-sensitive adhesive layer (a) is provided on one side of a plastic substrate and a pressure-sensitive adhesive layer (b) is provided on the other side. In the following formula (2) which is a pressure-sensitive adhesive sheet and is an approximate straight line representing the time dependence of the relaxation elastic modulus at 40 ° C. of the double-sided pressure-sensitive adhesive sheet for fixing an abrasive, C is −0.55 The present invention relates to a double-sided pressure-sensitive adhesive sheet for fixing an abrasive, which is -0.25.
logG (t) = Clog t + D (2)
[In formula (2), t represents time, G (t) represents relaxation modulus, and C and D represent constants, respectively. ]
また、第３の発明は、感圧接着剤層（ａ）が、水酸基含有アクリル系ポリマーと、水酸基価５０〜１８０ｍｇＫＯＨ／ｇのテルペンフェノール系樹脂と、イソシアネート系架橋剤とを含む感圧接着剤から形成されてなることを特徴とする上記発明の研磨材固定用両面感圧接着シートに関する。 The third invention is a pressure-sensitive adhesive in which the pressure-sensitive adhesive layer (a) includes a hydroxyl group-containing acrylic polymer, a terpene phenol resin having a hydroxyl value of 50 to 180 mgKOH / g, and an isocyanate crosslinking agent. It is related with the double-sided pressure sensitive adhesive sheet for abrasive | polishing material fixation of the said invention characterized by being formed from.
さらに、第４の発明は、感圧接着剤層（ａ）の溶剤不溶分が５〜３０％であることを特徴とする上記発明の研磨材固定用両面感圧接着シートに関する。 Further, the fourth invention relates to the double-sided pressure-sensitive adhesive sheet for fixing an abrasive according to the invention, wherein the solvent-insoluble content of the pressure-sensitive adhesive layer (a) is 5 to 30%.
本発明は、研磨材を研磨装置へ平滑に固定でき、また被研磨体の鏡面研磨が容易にできて、さらに研磨液に曝されたときにも密着性を維持できる研磨材固定用両面感圧接着シートの提供することができるようになった。 The present invention provides a double-sided pressure-sensitive material for fixing an abrasive that can fix the abrasive smoothly to a polishing apparatus, facilitates mirror polishing of an object to be polished, and maintains adhesion even when exposed to a polishing liquid. An adhesive sheet can be provided.
本発明の両面感圧接着シートは、感圧接着剤層（ａ）／プラスチック基材／感圧接着剤層（ｂ）という構成である。 The double-sided pressure-sensitive adhesive sheet of the present invention has a structure of pressure-sensitive adhesive layer (a) / plastic substrate / pressure-sensitive adhesive layer (b).
本発明の研磨材固定用両面感圧接着シートは、研磨材を研磨装置に固定した後の研磨工程中において、研磨材および両面感圧接着シートの微小な粗さを緩和する機能を有する。 The double-sided pressure-sensitive adhesive sheet for fixing an abrasive of the present invention has a function of reducing the fine roughness of the abrasive and the double-sided pressure-sensitive adhesive sheet during the polishing step after the abrasive is fixed to the polishing apparatus.
本発明の研磨材固定用両面感圧接着シートは、プラスチック基材の一方の面に感圧接着剤層（ａ）が、他の面に感圧接着剤層（ｂ）がそれぞれ設けられてなる研磨材固定用両面感圧接着シートであって、
感圧接着剤層（ａ）の、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（１）において、傾きＡが−０．５０〜−０．２０であることが好ましい。より好ましくは、−０．４５〜−０．２５である。前記数値範囲にＡが入ることで、感圧接着剤（ａ）層に存在する粗さがドレッシング工程中に緩和され、研磨部材全体として平滑性を得ることができる。また感圧接着剤層（ａ）は研磨定盤と良好な密着性が得られることで、感圧接着剤層（ａ）と研磨定盤の界面に研磨液の侵入がない。そのため、長時間の研磨が可能になった。ここで傾きＡが−０．２０を超える場合は、微小な粗さを緩和しにくい。−０．５０より小さい場合は、柔軟になりすぎて研磨材を長時間固定することが難しい。
ｌｏｇ Ｇ（ｔ）＝Ａｌｏｇ ｔ＋Ｂ ・・・式（１）
〔式（１）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＡおよびＢは定数をそれぞれ表す。〕
なお、研磨工程における標準的な温度は４０℃である。
The double-sided pressure-sensitive adhesive sheet for fixing an abrasive of the present invention is provided with a pressure-sensitive adhesive layer (a) on one side of a plastic substrate and a pressure-sensitive adhesive layer (b) on the other side. A double-sided pressure-sensitive adhesive sheet for fixing abrasives,
In the following formula (1), which is an approximate straight line representing the time dependence of the relaxation modulus at 40 ° C. of the pressure-sensitive adhesive layer (a), the slope A is preferably −0.50 to −0.20. . More preferably, it is -0.45--0.25. When A is in the numerical range, the roughness present in the pressure-sensitive adhesive (a) layer is relaxed during the dressing process, and smoothness can be obtained as a whole polishing member. Further, the pressure-sensitive adhesive layer (a) has good adhesion to the polishing platen, so that the polishing liquid does not enter the interface between the pressure-sensitive adhesive layer (a) and the polishing platen. Therefore, it was possible to polish for a long time. Here, when the slope A exceeds −0.20, it is difficult to reduce the minute roughness. If it is smaller than −0.50, it becomes too flexible and it is difficult to fix the abrasive for a long time.
log G (t) = Alog t + B (1)
[In formula (1), t represents time, G (t) represents relaxation modulus, and A and B represent constants, respectively. ]
The standard temperature in the polishing process is 40 ° C.
Ｇ（ｔ）とは、微小な歪みを加えたときの応力から計算される緩和弾性率であり、感圧接着剤のような粘弾性体では、一般的に時間と共に徐々に低下するが、この低下の仕方（傾き）が研磨部材の平滑性向上のための指標となることを見出した。 G (t) is a relaxation elastic modulus calculated from the stress when a minute strain is applied. Generally, in a viscoelastic body such as a pressure-sensitive adhesive, it gradually decreases with time. It has been found that the method of lowering (inclination) is an index for improving the smoothness of the polishing member.
さらに、研磨材固定用両面感圧接着シートの、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（２）において、Ｃが−０．５５〜−０．２５であることが好ましく、さらに好ましくは−０．５０〜−０．２５である。上記同様の理由で、Ｃが−０．２５を超える場合は、微小粗さを緩和しにくい。−０．５０より小さい場合は、柔軟になりすぎて研磨材を長時間固定することが難しい。
ｌｏｇＧ（ｔ）＝Ｃｌｏｇ ｔ＋Ｄ ・・・式（２）
〔式（２）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＣおよびＤは定数をそれぞれ表す。〕
Furthermore, in the following formula (2) that is an approximate straight line representing the time dependence of the relaxation modulus at 40 ° C. of the double-sided pressure-sensitive adhesive sheet for fixing an abrasive, C is −0.55 to −0.25. Is more preferable, and -0.50 to -0.25 is more preferable. For the same reason as described above, when C exceeds −0.25, it is difficult to reduce the fine roughness. If it is smaller than −0.50, it becomes too flexible and it is difficult to fix the abrasive for a long time.
logG (t) = Clog t + D (2)
[In formula (2), t represents time, G (t) represents relaxation modulus, and C and D represent constants, respectively. ]
本発明において、感圧接着剤層（ａ）と感圧接着剤層（ｂ）は、それぞれ異なる感圧接着剤を用いても良いし、同じ感圧接着剤を用いても良い。 In the present invention, the pressure-sensitive adhesive layer (a) and the pressure-sensitive adhesive layer (b) may use different pressure-sensitive adhesives or the same pressure-sensitive adhesive.
感圧接着剤層（ａ）に用いる感圧接着剤としては、アクリル系、ゴム系、ウレタン系またはポリエステル系のポリマーが挙げられるが、応力緩和性と耐薬品性の面からアクリル系が好ましい。前記アクリル系ポリマーはラジカル重合性不飽和モノマーを、例えば溶液重合法、塊状重合法、乳化重合法等によって重合することにより得られる。 Examples of the pressure-sensitive adhesive used for the pressure-sensitive adhesive layer (a) include acrylic, rubber-based, urethane-based, and polyester-based polymers, and acrylic is preferable from the viewpoint of stress relaxation and chemical resistance. The acrylic polymer can be obtained by polymerizing a radical polymerizable unsaturated monomer by, for example, a solution polymerization method, a bulk polymerization method, an emulsion polymerization method or the like.
本発明の研磨材固定用両面感圧接着シートが使用される環境は、長時間にわたり強酸性から強アルカリ性の研磨液に曝されながらも、研磨材や研磨定盤から剥がれてはならないため、感圧接着剤層は大きな接着力と耐薬品性が必要である。そのためラジカル重合性不飽和モノマーの選択は大変重要である。 The environment in which the double-sided pressure-sensitive adhesive sheet for fixing an abrasive according to the present invention is used must be peeled off from an abrasive or a polishing surface plate while being exposed to a strongly acidic to strongly alkaline polishing liquid for a long time. The pressure adhesive layer needs to have a large adhesive force and chemical resistance. Therefore, the selection of radically polymerizable unsaturated monomer is very important.
ラジカル重合性不飽和モノマーとしては、アルキル基の炭素数が１〜１４の(メタ)アクリル酸アルキルエステルを主成分とすることが好ましい。かかる（メタ）アクリル酸アルキルエステルとしては（メタ）アクリル酸メチル、（メタ）アクリル酸エチル、（メタ）アクリル酸プロピル、（メタ）アクリル酸ｉｓｏ−プロピル、（メタ）アクリル酸ブチル、（メタ）アクリル酸ｉｓｏ−ブチル、（メタ）アクリル酸ヘキシル、（メタ）アクリル酸オクチル、（メタ）アクリル酸２−エチルヘキシル、（メタ）アクリル酸デシル、（メタ）アクリル酸ドデシル等の直鎖または分岐脂肪族アルコールのアクリル酸エステル及び対応するメタクリル酸エステル等が挙げられる。使用される（メタ）アクリル酸アルキルエステルのアルキル基の炭素数は１〜１０がより好ましく、１〜８がさらに好ましい。 As the radically polymerizable unsaturated monomer, it is preferable that the main component is a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 14 carbon atoms. Such alkyl (meth) acrylates include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, iso-propyl (meth) acrylate, butyl (meth) acrylate, (meth) Linear or branched aliphatic such as iso-butyl acrylate, hexyl (meth) acrylate, octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, decyl (meth) acrylate, dodecyl (meth) acrylate Examples include acrylate esters of alcohol and the corresponding methacrylate esters. As for carbon number of the alkyl group of the (meth) acrylic-acid alkylester used, 1-10 are more preferable, and 1-8 are more preferable.
上記（メタ）アクリル酸アルキルエステルは、ラジカル重合性不飽和モノマーの合計１００重量％中７０〜９９．９重量％含有されることが好ましく、また１種または２種以上含有することができる。
そして、大きな接着力を得るためには、ラジカル重合性不飽和モノマーの合計１００重量％中、アクリル酸ブチルが５０〜９５重量％含有されることが好ましい。
The (meth) acrylic acid alkyl ester is preferably contained in an amount of 70 to 99.9% by weight in a total of 100% by weight of the radical polymerizable unsaturated monomer, and can be contained in one kind or two or more kinds.
And in order to obtain big adhesive force, it is preferable that 50 to 95 weight% of butyl acrylate is contained in the total 100 weight% of a radically polymerizable unsaturated monomer.
本発明における研磨材固定用両面感圧接着シートは大きな接着力が必要である。接着性を得るために極性基を有するモノマーが使用される。その中でも水酸基含有モノマーとカルボキシル基含有モノマーが好ましい。研磨液がアルカリ性である場合、カルボキシル基含有モノマーを用いた感圧接着剤は中和されることにより接着力が低下しやすい。従って、本発明においては極性基を有するモノマーが水酸基含有モノマーであることが好ましい。 The double-sided pressure-sensitive adhesive sheet for fixing an abrasive in the present invention requires a large adhesive force. A monomer having a polar group is used to obtain adhesion. Of these, a hydroxyl group-containing monomer and a carboxyl group-containing monomer are preferred. In the case where the polishing liquid is alkaline, the pressure-sensitive adhesive using the carboxyl group-containing monomer is easily neutralized and the adhesive force is likely to be reduced. Therefore, in the present invention, the monomer having a polar group is preferably a hydroxyl group-containing monomer.
前記水酸基含有モノマーはラジカル重合性不飽和モノマーの合計１００重量％中０．１〜１０重量％含有することが好ましく、０．２〜５重量％含有することがより好ましく、０．３〜４重量％含有することがさらに好ましい。水酸基含有モノマーとしては、（メタ）アクリル酸２−ヒドロキシエチル、（メタ）アクリル酸２−ヒドロキシプロピル、（メタ）アクリル酸２−ヒドロキシブチル、ポリエチレングリコール（メタ）アクリレート等のアルコール性水酸基含有モノマーが挙げられる。 The hydroxyl group-containing monomer is preferably contained in an amount of 0.1 to 10% by weight, more preferably 0.2 to 5% by weight, more preferably 0.3 to 4% by weight, based on 100% by weight of the radical polymerizable unsaturated monomer. % Content is more preferable. Examples of the hydroxyl group-containing monomer include alcoholic hydroxyl group-containing monomers such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, and polyethylene glycol (meth) acrylate. Can be mentioned.
水酸基含有モノマーの割合が０．１重量％未満の場合、感圧接着剤層の研磨材等への強い接着性が得られにくい。一方、水酸基含有モノマーの割合が１０重量％を超えると、特に強アルカリ性の研磨液に曝された場合に研磨材や研磨装置から剥がれやすくなる。 When the proportion of the hydroxyl group-containing monomer is less than 0.1% by weight, it is difficult to obtain strong adhesion to the abrasive or the like of the pressure sensitive adhesive layer. On the other hand, when the proportion of the hydroxyl group-containing monomer exceeds 10% by weight, it becomes easy to peel off from the abrasive or the polishing apparatus particularly when exposed to a strongly alkaline polishing liquid.
また、前記ジカル重合性不飽和モノマーとして、上記以外のモノマーを必要に応じて使用することもできる。
具体的には、例えばグリシジルアクリレート、グリシジルメタクリレート等のエポキシ基含有モノマー。Ｎ−ヒドロキシアルキル（メタ）アクリルアミド、Ｎ―アルコキシアルキル（メタ）アクリルアミド、メチロール化アクリルアミド、Ｎ−（１，１−ジメチル−３オキソブチル）アクリルアミド、ダイアセトンアクリルアミド等の（メタ）アクリルアミドモノマー。燐酸基含有ビニルモノマーや酢酸ビニル、スチレン、ブタジエン等のビニルモノマー。アセトアセトキシエチルメタクリレート、アルコキシシリル基含有モノマー等が挙げられ、ラジカル重合性不飽和モノマーの合計１００重量％中０〜１０重量％の割合で用いることができ、これらは１種または２種以上使用できる。
In addition, as the dical polymerizable unsaturated monomer, a monomer other than the above can be used as necessary.
Specifically, for example, epoxy group-containing monomers such as glycidyl acrylate and glycidyl methacrylate. (Meth) acrylamide monomers such as N-hydroxyalkyl (meth) acrylamide, N-alkoxyalkyl (meth) acrylamide, methylolated acrylamide, N- (1,1-dimethyl-3oxobutyl) acrylamide, and diacetone acrylamide. Phosphoric acid group-containing vinyl monomers and vinyl monomers such as vinyl acetate, styrene and butadiene. Examples include acetoacetoxyethyl methacrylate, alkoxysilyl group-containing monomers, and the like, and can be used in a proportion of 0 to 10% by weight in a total of 100% by weight of radical polymerizable unsaturated monomers, and these can be used alone or in combination of two or more. .
前記アクリル系ポリマーのガラス転移温度は０℃以下が好ましく、−７０℃〜−５℃がより好ましく、−６０℃〜−１０℃がわらに好ましい。ガラス転移温度が０℃を超えると、十分な接着性が確保できない傾向にある。 The glass transition temperature of the acrylic polymer is preferably 0 ° C or lower, more preferably -70 ° C to -5 ° C, and more preferably -60 ° C to -10 ° C. When the glass transition temperature exceeds 0 ° C., sufficient adhesiveness tends to be not ensured.
なお、アクリル系ポリマーのガラス転移温度は、それを構成するラジカル重合性不飽和モノマーの組成比と、それぞれのモノマーからなるホモポリマーのガラス転移温度を基に、公知の方法により算出することができる。 The glass transition temperature of the acrylic polymer can be calculated by a known method based on the composition ratio of the radically polymerizable unsaturated monomer constituting the acrylic polymer and the glass transition temperature of the homopolymer composed of each monomer. .
さらにアクリル系ポリマーは、重量平均分子量が４０万〜９０万であることが好ましく、５０万〜８５万であることがより好ましく、さらに好ましくは６０万〜８０万である。重量平均分子量が４０万より小さい場合には、感圧接着剤層（ａ）の凝集力が低く、研磨時に加わるせん断力に耐え切れずに、研磨材や研磨装置から剥がれる恐れがある。一方、重量平均分子量が９０万よりも大きい場合には、感圧接着剤層（ａ）の粗さ緩和性能が低下しやすい。なお重量平均分子量はゲルパーミエイションクロマトグラフィー（ＧＰＣ）による、標準のポリスチレン換算の値である。 Furthermore, the acrylic polymer preferably has a weight average molecular weight of 400,000 to 900,000, more preferably 500,000 to 850,000, and still more preferably 600,000 to 800,000. When the weight average molecular weight is less than 400,000, the cohesive force of the pressure-sensitive adhesive layer (a) is low, and there is a risk that the pressure-sensitive adhesive layer (a) may not withstand the shearing force applied during polishing and may be peeled off from the abrasive or polishing apparatus. On the other hand, when the weight average molecular weight is larger than 900,000, the roughness relaxation performance of the pressure-sensitive adhesive layer (a) tends to decrease. The weight average molecular weight is a standard polystyrene equivalent value determined by gel permeation chromatography (GPC).
アクリル系ポリマーは、種々の重合開始剤を用い、その量、重合温度等の重合諸条件を適宜調整することにより得ることができる。ラジカル重合性不飽和モノマーを重合する際には、開始剤として過酸化物やアゾ系化合物が用いられる。 The acrylic polymer can be obtained by using various polymerization initiators and appropriately adjusting the polymerization conditions such as the amount and polymerization temperature. When polymerizing a radically polymerizable unsaturated monomer, a peroxide or an azo compound is used as an initiator.
本発明において用いられる過酸化物としては、ケトンパーオキサイド類、パーオキシケタール類、ハイドロパーオキサイド類、ジアルキルパーオキサイド類、ジアシルパーオキサイド類、パーオキシジカーボネート類、パーオキシエステル類等を挙げることができる。 Examples of the peroxide used in the present invention include ketone peroxides, peroxyketals, hydroperoxides, dialkyl peroxides, diacyl peroxides, peroxydicarbonates, peroxyesters, and the like. Can do.
本発明では、感圧接着剤が、水酸基と反応し得る化合物を架橋剤として含有することが好ましい。水酸基と反応し得る架橋剤としては、エポキシ系架橋剤やイソシアネート系架橋剤等が挙げられる。エポキシ系架橋剤を単独で使用した場合には感圧接着剤層が強固になりやすく、本発明ではイソシアネート系架橋剤を用いることが好ましい。 In the present invention, the pressure-sensitive adhesive preferably contains a compound capable of reacting with a hydroxyl group as a crosslinking agent. Examples of the crosslinking agent capable of reacting with a hydroxyl group include an epoxy crosslinking agent and an isocyanate crosslinking agent. When an epoxy-based crosslinking agent is used alone, the pressure-sensitive adhesive layer tends to be strong, and in the present invention, it is preferable to use an isocyanate-based crosslinking agent.
イソシアネート系架橋剤は、アクリル系ポリマー１００重量部に対して、０．０１〜１０重量部用いることが好ましく、０．０５〜５重量部用いることがより好ましい。０．０１重量部未満は、感圧接着剤層の凝集力が不足する恐れがあり、１００重量部を超えると、感圧接着剤層（ａ）が微小な表面粗さを緩和しにくくなる恐れがある。 The isocyanate crosslinking agent is preferably used in an amount of 0.01 to 10 parts by weight, more preferably 0.05 to 5 parts by weight, based on 100 parts by weight of the acrylic polymer. If the amount is less than 0.01 part by weight, the cohesive force of the pressure-sensitive adhesive layer may be insufficient. If the amount exceeds 100 parts by weight, the pressure-sensitive adhesive layer (a) may not easily relieve minute surface roughness. There is.
前記イソシアネート系架橋剤としては、ジイソシアネート化合物、ジイソシアネート化合物を３官能ポリオール成分で変性したいわゆるアダクト体、ジイソシアネート化合物が水と反応したビュレット体、ジイソシアネート化合物３分子から形成されるイソシアヌレート環を有する３量体（イソシアヌレート体）を使用することができる。ジイソシアネート化合物としては、芳香族ジイソシアネート、脂肪族ジイソシアネート、芳香脂肪族ジイソシアネート、脂環族ジイソシアネート等が挙げられる。 Examples of the isocyanate-based crosslinking agent include a diisocyanate compound, a so-called adduct obtained by modifying a diisocyanate compound with a trifunctional polyol component, a burette obtained by reacting the diisocyanate compound with water, and a 3 amount having an isocyanurate ring formed from three molecules of the diisocyanate compound. The body (isocyanurate body) can be used. Examples of the diisocyanate compound include aromatic diisocyanate, aliphatic diisocyanate, araliphatic diisocyanate, and alicyclic diisocyanate.
芳香族ジイソシアネートとしては、１，３−フェニレンジイソシアネート、４，４’−ジフェニルジイソシアネート、１，４−フェニレンジイソシアネート、４，４’−ジフェニルメタンジイソシアネート、２，４−トリレンジイソシアネート、２，６−トリレンジイソシアネート、４，４’−トルイジンジイソシアネート、ジアニシジンジイソシアネート、４，４’−ジフェニルエーテルジイソシアネート等を挙げることができる。 As aromatic diisocyanates, 1,3-phenylene diisocyanate, 4,4'-diphenyl diisocyanate, 1,4-phenylene diisocyanate, 4,4'-diphenylmethane diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate Examples thereof include isocyanate, 4,4′-toluidine diisocyanate, dianisidine diisocyanate, and 4,4′-diphenyl ether diisocyanate.
脂肪族ジイソシアネートとしては、トリメチレンジイソシアネート、テトラメチレンジイソシアネート、ヘキサメチレンジイソシアネート、ペンタメチレンジイソシアネート、１，２−プロピレンジイソシアネート、２，３−ブチレンジイソシアネート、１，３−ブチレンジイソシアネート、ドデカメチレンジイソシアネート、２，４，４−トリメチルヘキサメチレンジイソシアネート等を挙げることができる。 Aliphatic diisocyanates include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1,2-propylene diisocyanate, 2,3-butylene diisocyanate, 1,3-butylene diisocyanate, dodecamethylene diisocyanate, 2,4 , 4-trimethylhexamethylene diisocyanate and the like.
芳香脂肪族ジイソシアネートとしては、ω，ω’−ジイソシアネート−１，３−ジメチルベンゼン、ω，ω’−ジイソシアネート−１，４−ジメチルベンゼン、ω，ω’−ジイソシアネート−１，４−ジエチルベンゼン、１，４−テトラメチルキシリレンジイソシアネート、１，３−テトラメチルキシリレンジイソシアネート等を挙げることができる。 Examples of the araliphatic diisocyanate include ω, ω′-diisocyanate-1,3-dimethylbenzene, ω, ω′-diisocyanate-1,4-dimethylbenzene, ω, ω′-diisocyanate-1,4-diethylbenzene, 1, Examples include 4-tetramethylxylylene diisocyanate and 1,3-tetramethylxylylene diisocyanate.
脂環族ジイソシアネートとしては、３−イソシアネートメチル−３，５，５−トリメチルシクロヘキシルイソシアネート、１，３−シクロペンタンジイソシアネート、１，３−シクロヘキサンジイソシアネート、１，４−シクロヘキサンジイソシアネート、メチル−２，４−シクロヘキサンジイソシアネート、メチル−２，６−シクロヘキサンジイソシアネート、４，４’−メチレンビス（シクロヘキシルイソシアネート）、１，４−ビス（イソシアネートメチル）シクロヘキサン、１，４−ビス（イソシアネートメチル）シクロヘキサン等を挙げることができる。 Examples of alicyclic diisocyanates include 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate, 1,3-cyclopentane diisocyanate, 1,3-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, methyl-2,4- Examples include cyclohexane diisocyanate, methyl-2,6-cyclohexane diisocyanate, 4,4′-methylenebis (cyclohexyl isocyanate), 1,4-bis (isocyanate methyl) cyclohexane, 1,4-bis (isocyanate methyl) cyclohexane, and the like. .
本発明に用いられるジイソシアネート化合物としては、２，４−トリレンジイソシアネート、ヘキサメチレンジイソシアネート、３−イソシアネートメチル−３，５，５−トリメチルシクロヘキシルイソシアネート（別名：イソホロンジイソシアネート）が好ましい。また、これらのジイソシアネート化合物のアダクト体、ビュレット体、イソシアヌレート体も好適に使用することができる。 As the diisocyanate compound used in the present invention, 2,4-tolylene diisocyanate, hexamethylene diisocyanate, and 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate (also known as isophorone diisocyanate) are preferable. In addition, adducts, burettes and isocyanurates of these diisocyanate compounds can also be suitably used.
本発明で用いる感圧接着剤は、フェノール骨格のある樹脂を含むことで、上記緩和弾性率と耐薬品性等を実現しやすくなることを見出した。 It has been found that the pressure-sensitive adhesive used in the present invention easily realizes the relaxation elastic modulus and chemical resistance by including a resin having a phenol skeleton.
フェノール骨格を有する樹脂としては、例えばロジン変性フェノール樹脂、フェノール変性キシレン樹脂およびテルペンフェノール樹脂が好ましい。その中でも水添テルペンフェノールは耐薬品性に優れるためより好ましい。前記水添テルペンフェノールは、水酸基価が５０〜１８０ｍｇＫＯＨ／ｇであることが好ましく、６０〜１６０ｍｇＫＯＨ／ｇであることがより好ましく、６５〜１５０ｍｇＫＯＨ／ｇがさらに好ましい。水酸基価が５０ｍｇＫＯＨ／ｇより小さい場合には、研磨材やプラスチック基材への密着性が低くなりやすい。一方、１８０ｍｇＫＯＨ／ｇを超える場合には、感圧接着剤層が硬くなりすぎて、感圧接着剤層の微小な表面粗さを緩和しにくくなる恐れがある。 As the resin having a phenol skeleton, for example, rosin-modified phenol resin, phenol-modified xylene resin and terpene phenol resin are preferable. Among them, hydrogenated terpene phenol is more preferable because of its excellent chemical resistance. The hydrogenated terpene phenol preferably has a hydroxyl value of 50 to 180 mgKOH / g, more preferably 60 to 160 mgKOH / g, and still more preferably 65 to 150 mgKOH / g. When the hydroxyl value is smaller than 50 mgKOH / g, the adhesion to an abrasive or a plastic substrate tends to be low. On the other hand, when it exceeds 180 mgKOH / g, the pressure-sensitive adhesive layer becomes too hard, and there is a possibility that the minute surface roughness of the pressure-sensitive adhesive layer is difficult to relax.
また、フェノール骨格を有する樹脂の軟化点は、６０〜１８０℃であることが好ましく、７０〜１６０℃であることが好ましく、さらに好ましくは１００〜１５０℃である。 Moreover, it is preferable that the softening point of resin which has a phenol skeleton is 60-180 degreeC, it is preferable that it is 70-160 degreeC, More preferably, it is 100-150 degreeC.
フェノール骨格を有する樹脂は、アクリル系ポリマー１００重量部に対して５〜５０重量部使用することが好ましく、５〜４５重量部使用することがより好ましく、１０〜４５重量部使用することがさらに好ましい。 The resin having a phenol skeleton is preferably used in an amount of 5 to 50 parts by weight based on 100 parts by weight of the acrylic polymer, more preferably 5 to 45 parts by weight, and even more preferably 10 to 45 parts by weight. .
また、本発明においては、上記緩和弾性率と耐薬品性等を低下させない範囲内で、フェノール骨格を有する粘着付与樹脂以外のロジン系樹脂、テルペン系樹脂、芳香族系石油系樹脂および脂肪族系石油樹脂等を併用することもできる。 In the present invention, the rosin resin, terpene resin, aromatic petroleum resin and aliphatic resin other than the tackifying resin having a phenol skeleton are used within the range in which the relaxation modulus and chemical resistance are not lowered. Petroleum resin can be used in combination.
ロジン系樹脂としては、天然ロジン、ロジンエステル、水添ロジン、水添ロジンエステル、重合ロジン、重合ロジンエステル、不均化ロジン、不均化ロジンエステル等が挙げられる。 Examples of the rosin resin include natural rosin, rosin ester, hydrogenated rosin, hydrogenated rosin ester, polymerized rosin, polymerized rosin ester, disproportionated rosin, and disproportionated rosin ester.
テルペン系樹脂としては、α−ピネン樹脂、β−ピネン樹脂、等が挙げられる。 Examples of the terpene resin include α-pinene resin and β-pinene resin.
芳香族系石油樹脂としては、スチレンオリゴマー、α−メチルスチレン／スチレン共重合体等が挙げられる。 Examples of aromatic petroleum resins include styrene oligomers and α-methylstyrene / styrene copolymers.
さらに本発明における感圧接着剤は各種の添加剤等を含有することが可能である。例えば、シランカップリング剤、界面活性剤、消泡剤、可塑剤、着色剤、フィラー、撥水剤等である。 Furthermore, the pressure-sensitive adhesive in the present invention can contain various additives. For example, silane coupling agents, surfactants, antifoaming agents, plasticizers, colorants, fillers, water repellents, and the like.
本発明における感圧接着剤層（ａ）の溶剤不溶分は、５〜３０％であることが好ましく、１０〜２５％であることがより好ましい。５％未満のときは、感圧接着剤層（ａ）の凝集力が不足する恐れがある。一方、１０重量部を超えると、研磨材や感圧接着シートの微小な表面粗さを緩和しにくくなる。 The solvent-insoluble content of the pressure-sensitive adhesive layer (a) in the present invention is preferably 5 to 30%, and more preferably 10 to 25%. If it is less than 5%, the cohesive force of the pressure-sensitive adhesive layer (a) may be insufficient. On the other hand, when it exceeds 10 parts by weight, it becomes difficult to reduce the minute surface roughness of the abrasive or the pressure-sensitive adhesive sheet.
本発明の両面感圧接着シートは、プラスチック基材の一方の面に感圧接着剤層（ａ）を形成し、他方の面に感圧接着剤層（ａ）を形成されたものである。前記プラスチック基材としては、平坦な形状のプラスチックシートを用いることができる。 The double-sided pressure-sensitive adhesive sheet of the present invention has a pressure-sensitive adhesive layer (a) formed on one surface of a plastic substrate and a pressure-sensitive adhesive layer (a) formed on the other surface. As the plastic substrate, a flat plastic sheet can be used.
前記プラスチックシートは、例えばポリビニルアルコールフィルムやトリアセチルセルロースフィルム、ポリプロピレン、ポリエチレン、ポリシクロオレフィン、エチレン−酢酸ビニル共重合体などのポリオレフィン系樹脂のフィルム、ポリエチレンテレフタレートやポリブチレンテレフタレートなどのポリエステル系樹脂のフィルム、ポリカーボネート系樹脂のフィルム、ポリノルボルネン系樹脂のフィルム、ポリアリレート系樹脂のフィルム、アクリル系樹脂のフィルム、ポリフェニレンサルファイド樹脂のフィルム、ポリスチレン樹脂のフィルム、ビニル系樹脂のフィルム、ポリアミド系樹脂のフィルム、ポリイミド系樹脂のフィルム、エポキシ系樹脂のフィルムなどが使用できる。またこれらは単独でも用いることもできるし、複数を積層して用いることもできる。さらにその表面をコロナ処理やマット処理したものを用いることもできる。 The plastic sheet is, for example, a film of a polyolefin resin such as a polyvinyl alcohol film or a triacetyl cellulose film, polypropylene, polyethylene, polycycloolefin, ethylene-vinyl acetate copolymer, or a polyester resin such as polyethylene terephthalate or polybutylene terephthalate. Film, polycarbonate resin film, polynorbornene resin film, polyarylate resin film, acrylic resin film, polyphenylene sulfide resin film, polystyrene resin film, vinyl resin film, polyamide resin film A polyimide resin film, an epoxy resin film, or the like can be used. Moreover, these can also be used individually and can also be laminated | stacked and used. Furthermore, the surface of which has been subjected to corona treatment or mat treatment can also be used.
プラスチック基材は、研磨工程における応力や熱によって変形しにくいものがよく、ヤング率が１ＧＰａ〜６ＧＰａが好ましく、２ＧＰａ〜６ＧＰａがより好ましい。さらに好ましくは３ＧＰａ〜５ＧＰａである。 The plastic substrate is preferably one that is not easily deformed by stress or heat in the polishing step, and the Young's modulus is preferably 1 GPa to 6 GPa, more preferably 2 GPa to 6 GPa. More preferably, it is 3 GPa to 5 GPa.
プラスチック基材は厚みムラの無いものが好ましく、厚み精度は±１０％以内が好ましく、±５％以内がより好ましく、±３％以内がさらに好ましい。 The plastic substrate preferably has no thickness unevenness, and the thickness accuracy is preferably within ± 10%, more preferably within ± 5%, and even more preferably within ± 3%.
本発明の研磨材固定用両面感圧接着シートは、感圧接着剤を剥離シート上にコーティングし、乾燥し、感圧接着剤層を設けた後、該感圧接着剤層とプラスチック基材とを貼り合わせ、感圧接着剤層をシート基材上に転写する方法、あるいはプラスチック基材に直接感圧接着剤をコーティング、乾燥して剥離シートを張り合わせる方法、あるいは両方の方法を片方ずつ用いて得られることが好ましい。また感圧接着剤層（ａ）および（ｂ）の片面あるいは両面には、剥離処理された紙剥離シートが積層されることが好ましい。 The double-sided pressure-sensitive adhesive sheet for fixing an abrasive according to the present invention comprises a pressure-sensitive adhesive coated on a release sheet, dried and provided with a pressure-sensitive adhesive layer. A method to transfer the pressure-sensitive adhesive layer onto the sheet substrate, or a method to coat the pressure-sensitive adhesive directly on the plastic substrate, dry and paste the release sheet, or both methods Is preferably obtained. Moreover, it is preferable that the paper release sheet by which the peeling process was carried out is laminated | stacked on the single side | surface or both surfaces of a pressure sensitive adhesive layer (a) and (b).
感圧接着剤をコーティングする方法としては、例えば、コンマコーター、ブレードコーター、グラビアコーター等のロールコーター、スロットダイコーター、リップコーター、カーテンコーター等のコーティング装置を用いることができる。 As a method for coating the pressure sensitive adhesive, for example, a coating machine such as a roll coater such as a comma coater, a blade coater, or a gravure coater, a slot die coater, a lip coater, or a curtain coater can be used.
感圧接着剤層（ａ）の乾燥厚さは、１０〜１００μｍであることが重要であり、１５〜９０μｍであることが好ましく、２０〜８０μｍであることがより好ましい。 The dry thickness of the pressure-sensitive adhesive layer (a) is important to be 10 to 100 μm, preferably 15 to 90 μm, and more preferably 20 to 80 μm.
以下に、本発明の具体的な実施例を比較例と併せて説明するが、本発明は、下記実施例に限定されない。また、下記実施例および比較例中、「部」および「％」は、それぞれ「重量部」および「重量％」を表す。 Specific examples of the present invention will be described below together with comparative examples, but the present invention is not limited to the following examples. In the following examples and comparative examples, “parts” and “%” represent “parts by weight” and “% by weight”, respectively.
（合成例１）
ラジカル重合性不飽和モノマーとしてアクリル酸ブチル：３０部、アクリル酸２−エチルヘキシル：１５部、アクリル酸メチル：４部、アクリル酸：１部を、さらに酢酸エチル：４６部、ベンゾイルパーオキサイド：０．０２部を混合し、滴下槽に仕込んだ。
加熱装置、撹拌機、還流冷却装置、温度計、窒素導入管および滴下槽を備えた重合用容器にアクリル酸ブチル：３０部、アクリル酸２−エチルヘキシル：１５部、アクリル酸メチル：４部、アクリル酸：１部、酢酸エチル：１８部、トルエン：１８部、ベンゾイルパーオキサイド：０．０２部を仕込み、重合槽内の空気を窒素ガスで置換した後、攪拌しながら窒素雰囲気下、還流温度下で滴下を開始した。滴下終了後、さらに攪拌しながら重合率が８０％に達したところで、ベンゾイルパーオキサイド０．０４部を添加し、重合率が９９％以上になるまで５時間反応を続けた。
(Synthesis Example 1)
As radical polymerizable unsaturated monomers, butyl acrylate: 30 parts, 2-ethylhexyl acrylate: 15 parts, methyl acrylate: 4 parts, acrylic acid: 1 part, ethyl acetate: 46 parts, benzoyl peroxide: 0. 02 parts were mixed and charged into the dropping tank.
Polymerization vessel equipped with heating device, stirrer, reflux cooling device, thermometer, nitrogen introduction tube and dropping tank, butyl acrylate: 30 parts, 2-ethylhexyl acrylate: 15 parts, methyl acrylate: 4 parts, acrylic Acid: 1 part, Ethyl acetate: 18 parts, Toluene: 18 parts, Benzoyl peroxide: 0.02 part were charged, and the air in the polymerization tank was replaced with nitrogen gas. The dropping was started. After completion of dropping, when the polymerization rate reached 80% with further stirring, 0.04 part of benzoyl peroxide was added, and the reaction was continued for 5 hours until the polymerization rate reached 99% or more.
次いで、酢酸エチル４０部を加えて室温まで冷却し、反応を終了した。この反応溶液は、無色透明で固形分４４．８重量％、粘度２００００ｍＰａ・ｓであり、共重合体の重量平均分子量は６５０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成から得られるポリマーの、理論的に求められるガラス転移温度は−５３．５℃である。不揮発分、重量平均分子量は以下の方法に従って求めた。 Next, 40 parts of ethyl acetate was added and cooled to room temperature to complete the reaction. This reaction solution was colorless and transparent, had a solid content of 44.8% by weight and a viscosity of 20000 mPa · s, and the copolymer had a weight average molecular weight of 650,000. The theoretically required glass transition temperature of the polymer obtained from the composition of the radical polymerizable unsaturated monomer is −53.5 ° C. The nonvolatile content and the weight average molecular weight were determined according to the following method.
＜不揮発分の測定＞
各反応溶液約１ｇを金属容器に秤量し、１５０℃オーブンにて２０分間乾燥して、残分を秤量して残率計算をし、不揮発分濃度とした。
<Measurement of non-volatile content>
About 1 g of each reaction solution was weighed into a metal container, dried in an oven at 150 ° C. for 20 minutes, the residue was weighed, and the remaining rate was calculated to obtain a nonvolatile content concentration.
＜粘度の測定＞
各反応溶液を２５℃中でＢ型粘度計（東京計器社製）にて、１２ｒｐｍ、１分間回転の条件で測定した。
<Measurement of viscosity>
Each reaction solution was measured with a B-type viscometer (manufactured by Tokyo Keiki Co., Ltd.) at 25 ° C. under the conditions of 12 rpm and 1 minute rotation.
＜重量平均分子量の測定＞
ＧＰＣ（ゲルパーミエーションクロマトグラフィー；ＨＰＣ−８０２０ 東ソー社製）を用いた。ＧＰＣは溶媒（テトラヒドロフラン）に溶解した物質をその分子サイズの差によって分離定量する液体クロマトグラフィーであり、重量平均分子量の決定はポリスチレン換算で行った。
<Measurement of weight average molecular weight>
GPC (gel permeation chromatography; HPC-8020 manufactured by Tosoh Corporation) was used. GPC is liquid chromatography in which a substance dissolved in a solvent (tetrahydrofuran) is separated and quantified based on the difference in molecular size, and the weight average molecular weight was determined in terms of polystyrene.
（合成例２）
ラジカル重合性不飽和モノマーとしてアクリル酸ブチル：３０部、アクリル酸２−エチルヘキシル：１５部、アクリル酸メチル：４部、アクリル酸２−ヒドロキシエチル：１部を、さらに酢酸エチル：４６部、ベンゾイルパーオキサイド：０．０２部を混合し、滴下槽に仕込んだ。
加熱装置、撹拌機、還流冷却装置、温度計、窒素導入管および滴下槽を備えた重合用容器にアクリル酸ブチル：３０部、アクリル酸２−エチルヘキシル：１５部、アクリル酸メチル：４部、アクリル酸２−ヒドロキシエチル：１部、酢酸エチル：１８部、トルエン：１８部、ベンゾイルパーオキサイド：０．０２部を仕込み、重合槽内の空気を窒素ガスで置換した後、攪拌しながら窒素雰囲気下、還流温度下で滴下を開始した。滴下終了後、さらに攪拌しながら重合率が８０％に達したところで、ベンゾイルパーオキサイド０．０４部を添加し、重合率が９９％以上になるまで５時間反応を続けた。
(Synthesis Example 2)
As radically polymerizable unsaturated monomers, butyl acrylate: 30 parts, 2-ethylhexyl acrylate: 15 parts, methyl acrylate: 4 parts, 2-hydroxyethyl acrylate: 1 part, ethyl acetate: 46 parts, benzoyl par Oxide: 0.02 part was mixed and charged into the dropping tank.
Polymerization vessel equipped with heating device, stirrer, reflux cooling device, thermometer, nitrogen introduction tube and dropping tank, butyl acrylate: 30 parts, 2-ethylhexyl acrylate: 15 parts, methyl acrylate: 4 parts, acrylic 2-hydroxyethyl acid: 1 part, ethyl acetate: 18 parts, toluene: 18 parts, benzoyl peroxide: 0.02 part were charged, and the air in the polymerization tank was replaced with nitrogen gas. The dropping was started at the reflux temperature. After completion of dropping, when the polymerization rate reached 80% with further stirring, 0.04 part of benzoyl peroxide was added, and the reaction was continued for 5 hours until the polymerization rate reached 99% or more.
次いで、酢酸エチル４０部を加えて室温まで冷却し、反応を終了した。この反応溶液は、無色透明で固形分４４．６重量％、粘度７０００ｍＰａ・ｓであり、共重合体の重量平均分子量は５５０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成から得られるポリマーの、理論的に求められるガラス転移温度は−５４．６℃である。 Next, 40 parts of ethyl acetate was added and cooled to room temperature to complete the reaction. This reaction solution was colorless and transparent, had a solid content of 44.6% by weight, a viscosity of 7000 mPa · s, and the weight average molecular weight of the copolymer was 550,000. The theoretically required glass transition temperature of the polymer obtained from the composition of the radical polymerizable unsaturated monomer is −54.6 ° C.
（実施例１）
合成例１で得られたアクリル系ポリマー溶液１００重量部に対して水酸基価：１４０ｍｇＫＯＨ／ｇ、軟化点１１２℃のテルペンフェノール系樹脂であるシルバレスＴＰ３００（Ａｒｉｚｏｎａ Ｃｈｅｍｉｃａｌ社製）を１５重量部、酢酸エチル：１５重量部、架橋剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７重量部を添加及び混合して感圧接着剤を作製した。
この感圧接着剤を紙剥離ライナー（以下、剥離ライナーという）に塗工乾燥して、乾燥膜厚４０μｍの感圧接着剤層が形成された感圧接着剤層キャストフィルムを得た。
Example 1
15 parts by weight of ethyl acetate with a hydroxyl value of 140 mg KOH / g and Silvales TP300 (Arizona Chemical), a terpene phenol resin having a softening point of 112 ° C., with respect to 100 parts by weight of the acrylic polymer solution obtained in Synthesis Example 1. : 15 parts by weight, tolylene diisocyanate trimethylolpropane adduct as a crosslinking agent: 0.7 parts by weight was added and mixed to prepare a pressure-sensitive adhesive.
This pressure-sensitive adhesive was applied to a paper release liner (hereinafter referred to as a release liner) and dried to obtain a pressure-sensitive adhesive layer cast film in which a pressure-sensitive adhesive layer having a dry film thickness of 40 μm was formed.
一方、上記感圧接着剤を紙剥離ライナーに塗工、乾燥し、乾燥膜厚４０μｍの感圧接着剤層を形成した。そしてプラスチック基材として厚み２５μｍのＰＥＴフィルム（ヤング率４ＧＰａ）をラミネートし、紙剥離ライナー／感圧接着剤層（ａ）／プラスチック基材の片面感圧接着シートを得た。さらに、厚さ３８μｍのフィルム剥離ライナーに上記感圧接着剤を乾燥膜厚が４０μｍになるように塗工乾燥させ、得られた片面感圧接着シートのプラスチック基材面にラミネートして、両面感圧接着シートを得た。 On the other hand, the pressure-sensitive adhesive was coated on a paper release liner and dried to form a pressure-sensitive adhesive layer having a dry film thickness of 40 μm. Then, a PET film (Young's modulus 4 GPa) having a thickness of 25 μm was laminated as a plastic substrate to obtain a single-sided pressure-sensitive adhesive sheet of paper release liner / pressure-sensitive adhesive layer (a) / plastic substrate. Further, the above pressure sensitive adhesive is applied and dried on a 38 μm thick film release liner so that the dry film thickness is 40 μm, and laminated on the plastic substrate surface of the obtained single side pressure sensitive adhesive sheet. A pressure-bonding sheet was obtained.
＜溶剤不溶分の測定＞
感圧接着剤キャストフィルムを秤量した２００メッシュのステンレス製金網（重量Ｗ０）に貼り付け秤量した重量Ｗ１と、ステンレス製金網に貼り付けた試料を酢酸エチル中で５時間還流抽出後、１００℃で１時間乾燥させ秤量した重量Ｗ２とから、下記の式で溶剤不溶分を算出した。
溶剤不溶分（％）＝［（Ｗ２−Ｗ０）／（Ｗ１−Ｗ０）］×１００
<Measurement of solvent insolubles>
A pressure sensitive adhesive cast film was attached to a weighed 200 mesh stainless steel wire mesh (weight W0), and the weight W1 weighed and the sample attached to the stainless steel wire mesh were refluxed and extracted in ethyl acetate for 5 hours at 100 ° C. From the weight W2 which was dried for 1 hour and weighed, the solvent insoluble content was calculated by the following formula.
Solvent insoluble content (%) = [(W2-W0) / (W1-W0)] × 100
＜感圧接着剤層の緩和弾性率測定＞
感圧接着剤キャストフィルムを数回重ね合わせることで厚さが約１ｍｍの感圧接着剤層サンプルを作製した。
緩和弾性率測定はＴＡ Ｉｎｓｔｒｕｍｅｎｔｓ社製ＡＲＥＳにて、４０℃雰囲気下、歪み２０％、１時間の条件で行った。
両対数グラフから近似直線ｌｏｇ Ｇ（ｔ）＝−０．１９ｌｏｇ ｔ＋Ｂを得た。
<Measurement of relaxation modulus of pressure-sensitive adhesive layer>
A pressure-sensitive adhesive layer sample having a thickness of about 1 mm was prepared by overlapping the pressure-sensitive adhesive cast film several times.
The relaxation elastic modulus was measured with ARES manufactured by TA Instruments under the conditions of 20% strain and 1 hour in a 40 ° C. atmosphere.
An approximate straight line log G (t) = − 0.19 log t + B was obtained from the log-log graph.
＜両面感圧接着シートの緩和弾性率測定＞
両面感圧接着シートを１０枚重ね合わせて厚さが約１ｍｍのサンプルを作製した。
緩和弾性率測定はＴＡ Ｉｎｓｔｒｕｍｅｎｔｓ社製ＡＲＥＳにて、４０℃雰囲気下、歪み２０％、１時間の条件で行った。
両対数グラフから近似直線ｌｏｇ Ｇ（ｔ）＝−０．２７ｌｏｇ ｔ＋Ｄを得た。
<Measurement of relaxation modulus of pressure-sensitive adhesive sheet on both sides>
A sample having a thickness of about 1 mm was prepared by superposing 10 double-sided pressure-sensitive adhesive sheets.
The relaxation elastic modulus was measured with ARES manufactured by TA Instruments under the conditions of 20% strain and 1 hour in a 40 ° C. atmosphere.
An approximate straight line log G (t) = − 0.27 log t + D was obtained from the log-log graph.
＜接着力評価試料作製＞
両面感圧接着シートを幅２５ｍｍ、長さ１００ｍｍに裁断し、非測定面であるフィルム剥離ライナー側感圧接着剤層に厚さ２５μｍのＰＥＴフィルムを貼り合せた。
<Preparation of adhesive strength evaluation sample>
The double-sided pressure-sensitive adhesive sheet was cut to a width of 25 mm and a length of 100 mm, and a PET film having a thickness of 25 μm was bonded to the film release liner side pressure-sensitive adhesive layer which is a non-measurement surface.
＜耐薬品性＞
薬品浸漬前接着力
上記接着力評価試料を４０℃雰囲気下に約１時間放置した後、同雰囲気下で紙剥離ライナー側感圧接着剤層をステンレス板に貼り、２ｋｇロールを１往復通過して圧着した。
圧着して２０分後、引張試験機を用いて、１８０度方向へ３００ｍｍ／分の速度で引き剥がし、その強度を記録した。
薬品浸漬後接着力
上記接着力評価試料の紙剥離ライナーを剥がして、ｐＨ１１のＫＯＨ水溶液及びｐＨ１．５の硫酸中にそれぞれ４０℃で２４時間浸漬した。４０℃雰囲気下で各薬品から取り出してすぐにステンレス板に上記同様の条件で貼り合わせ、圧着して２０分後、引張試験機を用いて、１８０度方向へ３００ｍｍ／分の速度で引き剥がし、その強度を記録した。
<Chemical resistance>
Adhesive strength before chemical immersion After leaving the above-mentioned adhesive strength evaluation sample in a 40 ° C. atmosphere for about 1 hour, a paper release liner side pressure sensitive adhesive layer is pasted on a stainless steel plate in the same atmosphere, and a 2 kg roll is passed once and twice. Crimped.
Twenty minutes after the pressure bonding, it was peeled off at a speed of 300 mm / min in the direction of 180 ° using a tensile tester, and the strength was recorded.
Adhesive strength after chemical immersion The paper release liner of the above adhesive strength evaluation sample was peeled off and immersed in a pH 11 KOH aqueous solution and a pH 1.5 sulfuric acid at 40 ° C. for 24 hours, respectively. Immediately after taking out from each chemical in a 40 ° C atmosphere, it was bonded to a stainless steel plate under the same conditions as described above, and after 20 minutes of pressure bonding, it was peeled off at a speed of 300 mm / min in the direction of 180 ° using a tensile tester. The intensity was recorded.
＜保持力＞
接着力評価試料の紙剥離ライナー側感圧接着剤層をＪＩＳ−Ｚ１５２８準拠で測定した（８０℃、荷重１ｋｇ、貼り付け面積２５ｍｍ×２５ｍｍ、対ステンレス板）。
<Retention force>
The pressure-sensitive adhesive layer on the paper release liner side of the adhesive strength evaluation sample was measured according to JIS-Z1528 (80 ° C., load 1 kg, pasting area 25 mm × 25 mm, stainless steel plate).
＜微小粗さ緩和前の表面粗さ測定＞
両面感圧接着シートの紙剥離ライナーを剥がし、感圧接着剤層の表面粗さＲａをレーザー変位計ＬＴ−８０１０（キーエンス社製）にて測定した。
<Measurement of surface roughness before micro roughness reduction>
The paper release liner of the double-sided pressure-sensitive adhesive sheet was peeled off, and the surface roughness Ra of the pressure-sensitive adhesive layer was measured with a laser displacement meter LT-8010 (manufactured by Keyence Corporation).
＜微小粗さ緩和後の表面粗さ測定＞
両面感圧接着シートの紙剥離ライナーを剥がし、フィルム剥離ライナー（表面粗さＲａ＝０．２μｍ）の剥離処理面を貼りあわせ、２００ｇ／ｃｍ2の圧力で１時間圧着した。圧着後、このフィルム剥離ライナーを剥がし、感圧接着剤層の表面粗さＲａをレーザー変位計にて測定した。
評価基準として、緩和後のＲａは小さいほど平滑であることを意味しており、緩和前後の変化量が大きいことがよい。
<Measurement of surface roughness after micro roughness reduction>
The paper release liner of the double-sided pressure-sensitive adhesive sheet was peeled off, the release treatment surface of the film release liner (surface roughness Ra = 0.2 μm) was attached, and pressure-bonded at a pressure of 200 g / cm 2 for 1 hour. After pressure bonding, the film release liner was peeled off, and the surface roughness Ra of the pressure-sensitive adhesive layer was measured with a laser displacement meter.
As an evaluation criterion, the smaller the Ra after relaxation, the smoother it is, and it is preferable that the amount of change before and after the relaxation is large.
これらの測定結果を表１に示す。 These measurement results are shown in Table 1.
（実施例２）
実施例１で用いた感圧接着剤を紙剥離ライナーに塗工乾燥して、乾燥膜厚４０μｍの感圧接着剤層が形成された感圧接着剤層キャストフィルムを得た。
(Example 2)
The pressure-sensitive adhesive used in Example 1 was applied to a paper release liner and dried to obtain a pressure-sensitive adhesive layer cast film on which a pressure-sensitive adhesive layer having a dry film thickness of 40 μm was formed.
また、上記感圧接着剤を紙剥離ライナーに塗工、乾燥し、乾燥膜厚４０μｍの感圧接着剤層を形成した。そしてプラスチック基材として厚み２５μｍのＰＥＴフィルム（ヤング率４ＧＰａ）をラミネートし、紙剥離ライナー／感圧接着剤層（ａ）／プラスチック基材の片面感圧接着シートを得た。 The pressure sensitive adhesive was coated on a paper release liner and dried to form a pressure sensitive adhesive layer having a dry film thickness of 40 μm. Then, a PET film (Young's modulus 4 GPa) having a thickness of 25 μm was laminated as a plastic substrate to obtain a single-sided pressure-sensitive adhesive sheet of paper release liner / pressure-sensitive adhesive layer (a) / plastic substrate.
さらに、厚さ３８μｍのフィルム剥離ライナーにゴム系感圧接着剤（緩和弾性率ｌｏｇＧ（ｔ）＝−０．１４ｌｏｇ ｔ＋Ｄ'）を塗工乾燥させ、得られた片面感圧接着シートのプラスチック基材面にラミネートして、両面感圧接着シートを得た。 Further, a rubber-based pressure-sensitive adhesive (relaxation modulus log G (t) = − 0.14 log t + D ′) was applied to a film release liner having a thickness of 38 μm and dried, and the plastic substrate of the obtained single-sided pressure-sensitive adhesive sheet Laminated on the surface, a double-sided pressure-sensitive adhesive sheet was obtained.
（実施例３）
プラスチック基材として、厚み３０μｍのポリプロピレンフィルム（ヤング率２ＧＰａ）を使用した他は、実施例１と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Example 3)
A pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained in the same manner as in Example 1 except that a polypropylene film having a thickness of 30 μm (Young's modulus 2 GPa) was used as the plastic substrate.
（実施例４）
合成例２で得られたアクリル系ポリマー溶液１００重量部に対して水酸基価：１４０ｍｇＫＯＨ／ｇ、軟化点１１２℃のテルペンフェノール系樹脂であるシルバレスＴＰ３００を１５重量部、酢酸エチル：１５重量部、架橋剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．４３重量部を添加及び混合して感圧接着剤を作製した。この感圧接着剤を紙剥離ライナーに塗工乾燥して、乾燥膜厚４０μｍの感圧接着剤層が形成された感圧接着剤層キャストフィルムを得た。
(Example 4)
100 parts by weight of the acrylic polymer solution obtained in Synthesis Example 2 has a hydroxyl value of 140 mg KOH / g, 15 parts by weight of Silvales TP300, a terpene phenol resin having a softening point of 112 ° C., and 15 parts by weight of ethyl acetate. Tolylene diisocyanate trimethylolpropane adduct as an agent: 0.43 parts by weight were added and mixed to prepare a pressure-sensitive adhesive. This pressure-sensitive adhesive was coated on a paper release liner and dried to obtain a pressure-sensitive adhesive layer cast film on which a pressure-sensitive adhesive layer having a dry film thickness of 40 μm was formed.
次に上記感圧接着剤を紙剥離ライナーに塗工、乾燥し、乾燥膜厚４０μｍの感圧接着剤層を形成した。そしてプラスチック基材として厚み２５μｍのＰＥＴフィルム（ヤング率４ＧＰａ）をラミネートし、紙剥離ライナー／感圧接着剤層（ａ）／プラスチック基材の片面感圧接着シートを得た。さらに、厚さ３８μｍのフィルム剥離ライナーに上記感圧接着剤を乾燥膜厚が４０μｍになるように塗工乾燥させ、得られた片面感圧接着シートのプラスチック基材面にラミネートして、両面感圧接着シートを得た。 Next, the pressure-sensitive adhesive was coated on a paper release liner and dried to form a pressure-sensitive adhesive layer having a dry film thickness of 40 μm. Then, a PET film (Young's modulus 4 GPa) having a thickness of 25 μm was laminated as a plastic substrate to obtain a single-sided pressure-sensitive adhesive sheet of paper release liner / pressure-sensitive adhesive layer (a) / plastic substrate. Further, the above pressure sensitive adhesive is applied and dried on a 38 μm thick film release liner so that the dry film thickness is 40 μm, and laminated on the plastic substrate surface of the obtained single side pressure sensitive adhesive sheet. A pressure-bonding sheet was obtained.
（実施例５）
実施例３の架橋剤の添加量を０．２２重量部に変更して感圧接着剤を作製した。他は、実施例１と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Example 5)
A pressure-sensitive adhesive was produced by changing the amount of the crosslinking agent of Example 3 to 0.22 parts by weight. Otherwise, in the same manner as in Example 1, a pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained.
（比較例１）
合成例２で得られたアクリル系ポリマー溶液１００重量部に対して水酸基価：１４０ｍｇＫＯＨ／ｇ、軟化点１１２℃のテルペンフェノール系樹脂であるシルバレスＴＰ３００を１５重量部、酢酸エチル：１５重量部、架橋剤としてＮ，Ｎ，Ｎ'，Ｎ'，−テトラグリシジル−メ
タ−キシリレンジアミン：０．５重量部を添加及び混合して感圧接着剤を作製した。他は、実施例１と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Comparative Example 1)
100 parts by weight of the acrylic polymer solution obtained in Synthesis Example 2 has a hydroxyl value of 140 mg KOH / g, 15 parts by weight of Silvales TP300, a terpene phenol resin having a softening point of 112 ° C., and 15 parts by weight of ethyl acetate. N, N, N ′, N ′,-tetraglycidyl-meta-xylylenediamine: 0.5 part by weight as an agent was added and mixed to prepare a pressure-sensitive adhesive. Otherwise, in the same manner as in Example 1, a pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained.
（比較例２）
架橋剤を使用せずに感圧接着剤を作製し、他は、実施例１と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Comparative Example 2)
A pressure-sensitive adhesive was prepared without using a crosslinking agent, and a pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained in the same manner as in Example 1 except for that.
（比較例３）
プラスチック基材として、厚み５０μｍのポリエチレンフィルム（ヤング率０．５ＧＰｃ）を使用した他は、実施例１と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Comparative Example 3)
A pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained in the same manner as in Example 1 except that a polyethylene film (Young's modulus 0.5 GPc) having a thickness of 50 μm was used as the plastic substrate.
（比較例４）
合成例２で得られたアクリル系ポリマー溶液１００重量部に対して水酸基価：０ｍｇＫＯＨ／ｇ、酸化：１２ｍｇ／ｇ、軟化点１２５℃のロジンエステル系樹脂であるペンセルＤ−１２５（荒川化学社製）を１５重量部、酢酸エチル：１５重量部、架橋剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．４３重量部を添加及び混合して感圧接着剤を得た。他は、実施例３と同様にして、感圧接着剤キャストフィルムと両面感圧接着シートを得た。
(Comparative Example 4)
Pencel D-125 (manufactured by Arakawa Chemical Co., Ltd.), which is a rosin ester resin having a hydroxyl value of 0 mgKOH / g, oxidation: 12 mg / g, and a softening point of 125 ° C. with respect to 100 parts by weight of the acrylic polymer solution obtained in Synthesis Example 2. 15 parts by weight, ethyl acetate: 15 parts by weight, and tolylene diisocyanate trimethylolpropane adduct: 0.43 parts by weight as a crosslinking agent were added and mixed to obtain a pressure-sensitive adhesive. Otherwise, a pressure-sensitive adhesive cast film and a double-sided pressure-sensitive adhesive sheet were obtained in the same manner as in Example 3.
実施例２〜５および比較例１〜４は、実施例１と同様の評価を行った。結果を表１に示す。 Examples 2 to 5 and Comparative Examples 1 to 4 were evaluated in the same manner as Example 1. The results are shown in Table 1.
表１の結果より、比較例１〜４は、緩和弾性率の近似直線が所定の傾きが得られなかったため、表面の粗さが緩和できない結果や、感圧接着剤層界面に薬液が侵入し、接着力測定で糊残りが発生する結果が得られたため研磨材固定用として用いるのは困難である。
これに対して、実施例１〜５は、緩和弾性率の近似直線が所定の傾きであったことで、耐薬液性や表面の粗さの緩和について良好な結果が得られた。したがって研磨材固定用両面感圧接着シートとして好適に使用できることがわかる。
From the results shown in Table 1, in Comparative Examples 1 to 4, the approximate straight line of the relaxation elastic modulus did not obtain a predetermined slope, so that the surface roughness could not be relaxed and the chemical solution entered the interface of the pressure sensitive adhesive layer. In addition, it is difficult to use as an abrasive fixing because a result of adhesive residue is obtained in the adhesive force measurement.
On the other hand, in Examples 1 to 5, good results were obtained for chemical resistance and surface roughness relaxation because the approximate straight line of the relaxation elastic modulus had a predetermined slope. Therefore, it turns out that it can be conveniently used as a double-sided pressure-sensitive adhesive sheet for fixing abrasives.
Claims (4)
感圧接着剤層（ａ）の、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（１）において、Ａが−０．５０〜−０．２０であることを特徴とする研磨材固定用両面感圧接着シート。
ｌｏｇ Ｇ（ｔ）＝Ａｌｏｇ ｔ＋Ｂ ・・・式（１）
〔式（１）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＡおよびＢは定数をそれぞれ表す。〕 A double-sided pressure-sensitive adhesive sheet for fixing an abrasive comprising a pressure-sensitive adhesive layer (a) on one side of a plastic substrate and a pressure-sensitive adhesive layer (b) on the other side,
The following formula (1), which is an approximate straight line representing the time dependence of the relaxation modulus at 40 ° C. of the pressure-sensitive adhesive layer (a), is characterized in that A is −0.50 to −0.20. Double-sided pressure-sensitive adhesive sheet for fixing abrasives.
log G (t) = Alog t + B (1)
[In formula (1), t represents time, G (t) represents relaxation modulus, and A and B represent constants, respectively. ]
前記研磨材固定用両面感圧接着シートの、４０℃における緩和弾性率の時間依存性を表す近似直線である下記式（２）において、Ｃが−０．５５〜−０．２５であることを特徴とする研磨材固定用両面感圧接着シート。
ｌｏｇＧ（ｔ）＝Ｃｌｏｇ ｔ＋Ｄ ・・・式（２）
〔式（２）中、ｔは時間を、Ｇ（ｔ）は緩和弾性率を、ＣおよびＤは定数をそれぞれ表す。〕 A pressure-sensitive adhesive layer (a) on one side of a plastic substrate, and a pressure-sensitive adhesive layer (b) on the other side, a double-sided pressure-sensitive adhesive sheet for fixing an abrasive,
In the following formula (2), which is an approximate straight line representing the time dependency of the relaxation elastic modulus at 40 ° C. of the double-sided pressure-sensitive adhesive sheet for fixing the abrasive, C is −0.55 to −0.25. A double-sided pressure-sensitive adhesive sheet for fixing abrasives.
logG (t) = Clog t + D (2)
[In formula (2), t represents time, G (t) represents relaxation modulus, and C and D represent constants, respectively. ]
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| JPH03171627A (en) * | 1989-08-01 | 1991-07-25 | Mitsui Toatsu Chem Inc | Wafer processing film |
| JP2001131500A (en) * | 1999-11-02 | 2001-05-15 | Sekisui Chem Co Ltd | Double coated adhesive tape for abrasive cloth fixing |
| JP2004083633A (en) * | 2002-08-23 | 2004-03-18 | Nihon Micro Coating Co Ltd | Adhesive tape for polishing pad and polishing tape |
| JP2008255253A (en) * | 2007-04-06 | 2008-10-23 | Toyo Ink Mfg Co Ltd | Double-sided pressure-sensitive adhesive sheet for abrasive |
| JP2010065095A (en) * | 2008-09-09 | 2010-03-25 | Sekisui Chem Co Ltd | Self-adhesive, double-sided pressure-sensitive adhesive sheet, and display |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03171627A (en) * | 1989-08-01 | 1991-07-25 | Mitsui Toatsu Chem Inc | Wafer processing film |
| JP2001131500A (en) * | 1999-11-02 | 2001-05-15 | Sekisui Chem Co Ltd | Double coated adhesive tape for abrasive cloth fixing |
| JP2004083633A (en) * | 2002-08-23 | 2004-03-18 | Nihon Micro Coating Co Ltd | Adhesive tape for polishing pad and polishing tape |
| JP2008255253A (en) * | 2007-04-06 | 2008-10-23 | Toyo Ink Mfg Co Ltd | Double-sided pressure-sensitive adhesive sheet for abrasive |
| JP2010065095A (en) * | 2008-09-09 | 2010-03-25 | Sekisui Chem Co Ltd | Self-adhesive, double-sided pressure-sensitive adhesive sheet, and display |
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