JP2016132059A - Polishing object holding material - Google Patents
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Abstract
Description
本発明は、シリコンウエハ、ハードディスクなどの製造において、これらの表面を研磨する工程で用いられる、被研磨物保持材に関するものである。 The present invention relates to an object holding material used in a process of polishing a surface of a silicon wafer, a hard disk or the like.
シリコンウエハ、ハードディスクなどの製造において、これらの表面を研磨する際には、平面研磨機の歯車と噛み合う駆動用ギアを外周に形成した円板にシリコンウエハなどの被研磨物保持用の孔を１個から複数個形成した被研磨物保持材を用い、この被研磨物保持材の保持用の孔に、被研磨物を嵌め込んで保持し、この状態で被研磨物保持材を研磨機に装着して、被研磨物保持材を平面上で駆動させることにより研磨を行っている。 In the manufacture of silicon wafers, hard disks and the like, when these surfaces are polished, a hole for holding an object to be polished such as a silicon wafer is formed in a disk having a driving gear meshing with a gear of a surface polishing machine on the outer periphery. Using a workpiece holding material formed from a plurality of pieces, the workpiece is inserted and held in the holding hole of the workpiece holding material, and in this state, the workpiece holding material is mounted on the polishing machine. Then, polishing is performed by driving the object holding material on a flat surface.
従来、このような被研磨物保持材は、ガラス繊維基材にエポキシ樹脂を含浸、乾燥した繊維強化樹脂シートを加熱加圧成形することにより形成され、研磨機の形状に応じた加工を施すことにより調製していた。
しかし、上記のようなガラス繊維を用いた被研磨物保持材は、切削加工性には優れるが、ガラス粉により、被研磨物の表面にスクラッチが発生するという問題があった。
Conventionally, such an object holding material is formed by impregnating a glass fiber base material with an epoxy resin and heat-pressing a dried fiber reinforced resin sheet, and processing according to the shape of the polishing machine. It was prepared by.
However, the material to be polished using the glass fiber as described above is excellent in machinability but has a problem that scratches are generated on the surface of the material to be polished by the glass powder.
そこで、スクラッチの発生を抑制するため、全芳香族ポリエステル繊維不織布等の有機繊維基材を用いた被研磨物保持材が開発されており、例えば、全芳香族ポリエステル繊維基材とアラミド繊維基材やガラス繊維基材とを組み合わせた被研磨物保持材が提案されている（特許文献１及び２等参照）。 Therefore, in order to suppress the generation of scratches, materials to be polished using organic fiber substrates such as wholly aromatic polyester fiber nonwoven fabrics have been developed. For example, wholly aromatic polyester fiber substrates and aramid fiber substrates are developed. Further, there has been proposed a workpiece holding material in combination with a glass fiber substrate (see Patent Documents 1 and 2, etc.).
しかし、特許文献１に記載された、全芳香族ポリエステル繊維からなる不織布を用いた被研磨物保持材は、厚み精度、機械強度の面で不十分である。また、アラミド繊維不織布を併用してもよいことが記載されているが、アラミド繊維の繊維径が大きく、不織布にするには適しておらず、厚み精度に欠け、反りの発生も懸念される。また、被研磨物保持材として使用した際の剥離に対する考慮も不十分である。
また、特許文献２に記載された、外層に全芳香族ポリエステル繊維織物、中間層に、ガラス繊維織物を用いた被研磨物保持材は、ガラス繊維が含まれているため、スクラッチ抑制効果が不十分である。
However, the material to be polished using a non-woven fabric made of wholly aromatic polyester fibers described in Patent Document 1 is insufficient in terms of thickness accuracy and mechanical strength. Moreover, although it is described that an aramid fiber nonwoven fabric may be used in combination, the fiber diameter of the aramid fiber is large and is not suitable for a nonwoven fabric. Moreover, the consideration with respect to peeling when used as a workpiece holding material is insufficient.
In addition, the object holding material described in Patent Document 2 that uses a wholly aromatic polyester fiber woven fabric for the outer layer and a glass fiber woven fabric for the intermediate layer contains glass fibers, and therefore has a scratch suppressing effect. It is enough.
本発明の目的は、被研磨物保持材の表面のスクラッチの発生が殆ど無く、厚み精度が良好で、反りが起こらず、また、耐久性に優れた被研磨物保持材を提供することにある。
また、本発明の目的は、金属元素含有量が少ない被研磨物保持材を提供することにある。
An object of the present invention is to provide an object holding material having almost no scratch on the surface of the object holding material, good thickness accuracy, no warping, and excellent durability. .
Moreover, the objective of this invention is providing the to-be-polished material holding | maintenance material with few metal element content.
本発明の目的は、繊維基材に熱硬化性樹脂を含浸してなる繊維強化樹脂シートを複数枚積層してなる被研磨物保持材であって、前記繊維強化樹脂シートが、下記（１）または（２）を繊維基材として用いた繊維強化樹脂シートを含有することを特徴とする被研磨物保持材によって達成される。
（１）総繊度が５０〜４５０ｄｔｅｘの全芳香族ポリエステルマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（２）繊度が１．０〜１０ｄｔｅｘの全芳香族ポリエステルモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。
An object of the present invention is an object holding material formed by laminating a plurality of fiber reinforced resin sheets obtained by impregnating a fiber base material with a thermosetting resin, wherein the fiber reinforced resin sheet has the following (1): Or it achieves by the to-be-polished material holding | maintenance material characterized by containing the fiber reinforced resin sheet which used (2) as a fiber base material.
(1) A woven fabric having a total fineness of 50 to 450 dtex and a total aromatic polyester multifilament having a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(2) A non-woven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of wholly aromatic polyester monofilament having a fineness of 1.0 to 10 dtex.
また、本発明の研磨用保持材は、繊維強化樹脂シートが３枚以上積層されている場合、その外層の繊維強化樹脂シートが、下記（ａ）または（ｂ）を繊維基材として用いた繊維強化樹脂シートとしてもよい。
（ａ）総繊度が５０〜４５０ｄｔｅｘのアラミドマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（ｂ）繊度が１．０〜１０ｄｔｅｘのアラミドモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。
Further, when three or more fiber reinforced resin sheets are laminated, the polishing holding material of the present invention is a fiber in which the outer layer fiber reinforced resin sheet uses the following (a) or (b) as a fiber base material. A reinforced resin sheet may be used.
(A) A woven fabric having an aramid multifilament having a total fineness of 50 to 450 dtex and a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(B) A nonwoven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of an aramid monofilament having a fineness of 1.0 to 10 dtex.
また、中間層に、全芳香族ポリエステル繊維からなる織物以外を繊維基材として用いる場合、被研磨物保持材中、繊維基材が４０〜８０質量％であり、かつ、繊維基材中の全芳香族ポリエステル繊維からなる繊維基材が１０質量％以上であることが好ましい。 Moreover, when using as a fiber base material other than the textiles which consist of a fully aromatic polyester fiber for an intermediate | middle layer, in a to-be-polished material holding material, a fiber base material is 40-80 mass%, and all in a fiber base material It is preferable that the fiber base material which consists of an aromatic polyester fiber is 10 mass% or more.
また、本発明の被研磨物保持材は、チタン、マグネシウム、アルミニウム又はケイ素の含有量が各々２０ｐｐｍ以下であることが好ましい。 Moreover, it is preferable that content of titanium, magnesium, aluminum, or silicon is 20 ppm or less in the to-be-polished material holding | maintenance material of this invention, respectively.
また、本発明において用いる熱硬化性樹脂が、エポキシ樹脂、ポリイミド樹脂、変性ポリイミド樹脂、フェノール樹脂、フェノールノボラック樹脂、クレゾールノボラック樹脂、メラミン樹脂、不飽和ポリエステル樹脂、環状オレフィン系重合体樹脂の中から選択されることが好ましい。 The thermosetting resin used in the present invention is selected from the group consisting of epoxy resin, polyimide resin, modified polyimide resin, phenol resin, phenol novolac resin, cresol novolac resin, melamine resin, unsaturated polyester resin, and cyclic olefin polymer resin. Preferably it is selected.
本発明により、厚み精度が良好で、反りが起こらず、耐久性にも優れた被研磨物保持材を提供することができる。
また、チタン、マグネシウム、アルミニウム又はケイ素の金属元素含有量が少ないことから、被研磨物保持材の表面のスクラッチの発生が殆ど無い。
According to the present invention, it is possible to provide an object-holding material having good thickness accuracy, no warpage, and excellent durability.
Moreover, since there is little metal element content of titanium, magnesium, aluminum, or silicon, there is almost no generation | occurrence | production of the scratch of the surface of a to-be-polished material holding material.
本発明の被研磨物保持材は、繊維基材に熱硬化性樹脂を含浸してなる繊維強化樹脂シートを複数枚積層してなる被研磨物保持材であって、前記繊維強化樹脂シートが、下記（１）または（２）を繊維基材として用いた繊維強化樹脂シートを含有するものである。（１）と（２）は、単独で用いても、組合せて用いても良い。
（１）総繊度が５０〜４５０ｄｔｅｘの全芳香族ポリエステルマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（２）繊度が１．０〜１０ｄｔｅｘの全芳香族ポリエステルモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。
The object holding material of the present invention is an object holding material formed by laminating a plurality of fiber reinforced resin sheets obtained by impregnating a thermosetting resin into a fiber base material, and the fiber reinforced resin sheet comprises: It contains a fiber reinforced resin sheet using the following (1) or (2) as a fiber base material. (1) and (2) may be used alone or in combination.
(1) A woven fabric having a total fineness of 50 to 450 dtex and a total aromatic polyester multifilament having a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(2) A non-woven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of wholly aromatic polyester monofilament having a fineness of 1.0 to 10 dtex.
本発明は、繊維強化樹脂シートに、上記全芳香族ポリエステル繊維基材を用いることにより、被研磨物保持材の厚み精度が良好で、反りが起こらない。また、機械強度に優れるため、耐久性が向上する。 In the present invention, by using the wholly aromatic polyester fiber base material in the fiber reinforced resin sheet, the thickness accuracy of the object-holding material is good and no warpage occurs. Moreover, since it is excellent in mechanical strength, durability improves.
本発明の被研磨物保持材は、特に、複数枚の繊維強化シートを積層して形成され、全ての繊維強化シートが、全芳香族ポリエステル繊維からなる織物を繊維基材として用いたものが、被研磨物保持材の反り、厚み精度が良好で、金属元素含有量が少なく、また、機械強度に優れ、耐久性も良好である。 The material to be polished of the present invention is particularly formed by laminating a plurality of fiber reinforced sheets, and all fiber reinforced sheets are made using a woven fabric made of wholly aromatic polyester fibers as a fiber base material. The warp of the material to be polished and the thickness accuracy are good, the metal element content is low, the mechanical strength is excellent, and the durability is also good.
また、３層以上の繊維強化樹脂シートを積層する場合に、その外層に、下記（ａ）または（ｂ）を繊維基材として用いた繊維強化樹脂シートとしてもよい。（ａ）と（ｂ）は、単独で用いても、組合せて用いても良い。
（ａ）総繊度が５０〜４５０ｄｔｅｘのアラミドマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（ｂ）繊度が１．０〜１０ｄｔｅｘのアラミドモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。
Moreover, when laminating | stacking the fiber reinforced resin sheet | seat of three or more layers, it is good also as a fiber reinforced resin sheet which used the following (a) or (b) as a fiber base material in the outer layer. (A) and (b) may be used alone or in combination.
(A) A woven fabric having an aramid multifilament having a total fineness of 50 to 450 dtex and a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(B) A nonwoven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of an aramid monofilament having a fineness of 1.0 to 10 dtex.
特に、全芳香族ポリエステル繊維不織布からなる繊維強化樹脂シートと、上記アラミド繊維基材からなる繊維強化樹脂シートとを組合せることにより、全芳香族ポリエステル繊維不織布からなる繊維強化樹脂シートのみからなる被研磨物保持材より、耐久性が上がる。 In particular, by combining a fiber reinforced resin sheet made of a wholly aromatic polyester fiber nonwoven fabric and a fiber reinforced resin sheet made of the above-mentioned aramid fiber base material, a cover made only of a fiber reinforced resin sheet made of a wholly aromatic polyester fiber nonwoven fabric is used. Durability is higher than abrasive holding material.
また、本発明において、被研磨物保持材中、繊維基材は４０〜８０質量％であることが好ましく、６０〜７５質量％であることが更に好ましい。
繊維基材が４０質量％未満では、熱硬化性樹脂が多くなり、機械強度が不十分で耐久性が悪くなる傾向にある。一方、繊維基材が８０質量％を超えると、熱硬化性樹脂が少なくなり、積層板の成形が難しくなる傾向にある。
Moreover, in this invention, it is preferable that a fiber base material is 40-80 mass% in a to-be-polished material holding material, and it is still more preferable that it is 60-75 mass%.
When the fiber base is less than 40% by mass, the thermosetting resin increases, and the mechanical strength is insufficient and the durability tends to deteriorate. On the other hand, when the fiber substrate exceeds 80% by mass, the thermosetting resin is reduced, and it tends to be difficult to mold the laminate.
また、全芳香族ポリエステル繊維基材を用いた繊維強化シートと、アラミド繊維基材等を用いた繊維強化シートとを組合せる場合には、繊維基材中における全芳香族ポリエステル繊維基材が１０質量％以上であることが好ましく、１５質量％以上が更に好ましく、３０質量％以上が特に好ましい。
繊維基材中、全芳香族ポリエステル繊維からなる繊維基材が１０質量％未満では、機械強度が上がらず、厚み精度も不十分となる傾向にある。
When a fiber reinforced sheet using a wholly aromatic polyester fiber substrate is combined with a fiber reinforced sheet using an aramid fiber substrate or the like, the total aromatic polyester fiber substrate in the fiber substrate is 10 It is preferably at least mass%, more preferably at least 15 mass%, particularly preferably at least 30 mass%.
If the fiber base material composed of wholly aromatic polyester fibers is less than 10% by mass in the fiber base material, the mechanical strength does not increase and the thickness accuracy tends to be insufficient.
また、本発明で用いる全芳香族ポリエステル繊維は、全芳香族ポリエステル系ポリマーから形成される。
全芳香族ポリエステル系ポリマーは、芳香族ジカルボン酸、芳香族ジオール及び／又は芳香族ヒドロキシカルボン酸やこれらの誘導体からなるもので、場合により、これらと、脂環族ジカルボン酸、脂環族ジオール、脂肪族ジオールやこれらの誘導体との共重合体も含まれる。ここで芳香族ジカルボン酸としては、テレフタル酸、イソフタル酸、４，４’−ジカルボキシジフェニル、２，６−ジカルボキシナフタレン、１，２−ビス（４−カルボキシフェノキシ）エタン等や、これらのアルキル、アリール、アルコキシ、ハロゲン基の核置換体が挙げられる。芳香族ジオールとしては、ヒドロキノン、レゾルシン、４，４’−ジヒドロキシジフェニル、４，４’−ジヒドロキシベンゾフェノン、４，４’−ジヒドロキシジフェニルメタン、４，４’−ジヒドロキシジフェニルエタン、２，２−ビス（４−ヒドロキシフェニル）プロパン、４，４’−ジヒドロキシジフェニルエーテル、４，４’−ジヒドロキシジフェニルスルホン、４，４’−ジヒドロキシジフェニルスルフィド、２，６−ジヒドロキシナフタレン、１，５−ジヒドロキシナフタレン等やこれらのアルキル、アリール、アルコキシ、ハロゲン基の核置換体が挙げられる。芳香族ヒドロキシカルボン酸としては、ｐ−ヒドロキシ安息香酸、ｍ−ヒドロキシ安息香酸、２−ヒドロキシナフタレン−６−カルボン酸、１−ヒドロキシナフタレン−５−カルボン酸等やこれらのアルキル、アリール、アルコキシ、ハロゲン基の核置換体が挙げられる。脂環族ジカルボン酸としては、トランス−１，４−ジカルボキシシクロヘキサン、シス−１，４−ジカルボキシシクロヘキサン等やこれらのアルキル、アリール、ハロゲン基の核置換体が挙げられる。脂環族及び脂肪族ジオールとしては、トランス−１，４−ジヒドロキシシクロヘキサン、シス−１，４−ジヒドロキシシクロヘキサン、エチレングリコール、１，４−ブタンジオール、キシリレンジオール等が挙げられる。
Further, the wholly aromatic polyester fiber used in the present invention is formed from a wholly aromatic polyester polymer.
The wholly aromatic polyester polymer is composed of an aromatic dicarboxylic acid, an aromatic diol and / or an aromatic hydroxycarboxylic acid or a derivative thereof, and in some cases, these may be an alicyclic dicarboxylic acid, an alicyclic diol, Copolymers with aliphatic diols and derivatives thereof are also included. Here, examples of the aromatic dicarboxylic acid include terephthalic acid, isophthalic acid, 4,4′-dicarboxydiphenyl, 2,6-dicarboxynaphthalene, 1,2-bis (4-carboxyphenoxy) ethane, and alkyls thereof. , Aryl, alkoxy, and halogen substituted groups of halogen groups. Aromatic diols include hydroquinone, resorcin, 4,4′-dihydroxydiphenyl, 4,4′-dihydroxybenzophenone, 4,4′-dihydroxydiphenylmethane, 4,4′-dihydroxydiphenylethane, 2,2-bis (4 -Hydroxyphenyl) propane, 4,4'-dihydroxydiphenyl ether, 4,4'-dihydroxydiphenyl sulfone, 4,4'-dihydroxydiphenyl sulfide, 2,6-dihydroxynaphthalene, 1,5-dihydroxynaphthalene, etc. and their alkyls , Aryl, alkoxy, and halogen substituted groups of halogen groups. Examples of aromatic hydroxycarboxylic acids include p-hydroxybenzoic acid, m-hydroxybenzoic acid, 2-hydroxynaphthalene-6-carboxylic acid, 1-hydroxynaphthalene-5-carboxylic acid, and their alkyl, aryl, alkoxy, and halogen. And a nuclear substituent of the group. Examples of the alicyclic dicarboxylic acid include trans-1,4-dicarboxycyclohexane, cis-1,4-dicarboxycyclohexane, and the like, and nuclear substitution products of these alkyl, aryl, and halogen groups. Examples of the alicyclic and aliphatic diols include trans-1,4-dihydroxycyclohexane, cis-1,4-dihydroxycyclohexane, ethylene glycol, 1,4-butanediol, and xylylenediol.
これらの組み合わせの中で、本発明において好ましい全芳香族ポリエステル系ポリマーとしては、例えば、（ａ）ｐ−ヒドロキシ安息香酸残基４０〜７０モル％と上記芳香族ジカルボン酸残基１５〜３０モル％と芳香族ジオール残基１５〜３０モル％からなるコポリエステル、（ｂ）テレフタル酸及び／又はイソフタル酸とクロルハイドロキノン、フェニルハイドロキノン、及び／又はハイドロキノンからなるコポリエステル、（ｃ）ｐ−ヒドロキシ安息香酸残基２０〜８０モル％と２−ヒドロキシナフタレン−６−カルボン酸残基２０〜８０モル％からなるコポリエステル等が挙げられる。 Among these combinations, the preferred wholly aromatic polyester polymer in the present invention includes, for example, (a) 40-70 mol% of p-hydroxybenzoic acid residue and 15-30 mol% of the aromatic dicarboxylic acid residue. And (b) a copolyester comprising terephthalic acid and / or isophthalic acid and chlorohydroquinone, phenylhydroquinone, and / or hydroquinone, (c) p-hydroxybenzoic acid And a copolyester composed of 20 to 80 mol% of a residue and 20 to 80 mol% of a 2-hydroxynaphthalene-6-carboxylic acid residue.
上記出発原料を用い、本発明で用いる全芳香族ポリエステル系ポリマーを得るには、そのままで、あるいは脂肪族又は芳香族モノカルボン酸又はそれらの誘導体、脂肪族アルコール又はフェノール類又はそれらの誘導体等によるエステル化により、重縮合反応を行う。重縮合反応としては、既知の塊状重合、溶液重合、懸濁重合等を採用することができ、得られたポリマーはそのままで、あるいは粉体状で不活性気体中、又は減圧下に熱処理して紡糸用試料とする。あるいは、一度押出機により造粒して用いてもよい。 In order to obtain the wholly aromatic polyester-based polymer used in the present invention using the above starting materials, as it is, or by aliphatic or aromatic monocarboxylic acid or derivatives thereof, aliphatic alcohol or phenols or derivatives thereof, etc. A polycondensation reaction is performed by esterification. As the polycondensation reaction, known block polymerization, solution polymerization, suspension polymerization, and the like can be employed. The obtained polymer is left as it is, or it is heat treated in a powdery inert gas or under reduced pressure. A sample for spinning is used. Alternatively, it may be granulated once by an extruder.
全芳香族ポリエステル系ポリマーには、本発明の目的を阻害しない範囲で、他のポリマーあるいは添加剤を含有させてもよい。 The wholly aromatic polyester-based polymer may contain other polymers or additives as long as the object of the present invention is not impaired.
本発明で用いる全芳香族ポリエステル系ポリマーには、紡糸に適した分子量範囲が存在する。この溶融紡糸条件に適する分子量に対応する物性値として「流動開始温度」を用いる。「流動開始温度」は、島津製作所製のフローテスターＣＦＴ−５００を用い、径１ｍｍ、長さ１０ｍｍのノズルで、圧力１００ｋｇ／ｃｍ２の状態で、芳香族ポリエステル試料を４℃／分で昇温し、試料がノズルを通って流動し、かつ４，８００パスカル秒の見かけ粘度を与える温度で定義される。
本発明において、溶融紡糸に適した芳香族ポリエステルの「流動開始温度」は、３０５〜３２５℃が好適である。
The wholly aromatic polyester polymer used in the present invention has a molecular weight range suitable for spinning. “Flow start temperature” is used as a physical property value corresponding to the molecular weight suitable for the melt spinning conditions. “Flow start temperature” is a temperature tester using a flow tester CFT-500 manufactured by Shimadzu Corporation, with a nozzle having a diameter of 1 mm and a length of 10 mm and a pressure of 100 kg / cm 2 and raising the temperature of the aromatic polyester sample at 4 ° C./min. And the temperature at which the sample flows through the nozzle and gives an apparent viscosity of 4,800 Pascal seconds.
In the present invention, the “flow start temperature” of the aromatic polyester suitable for melt spinning is preferably 305 to 325 ° C.
本発明に用いる全芳香族ポリエステル繊維の製造は、公知の溶融押出方法により行えばよい。 The wholly aromatic polyester fiber used in the present invention may be produced by a known melt extrusion method.
本発明では、被研磨物保持材に使用する繊維強化樹脂シートは、全芳香族ポリエステル繊維からなる織物または不織布を繊維基材として用いる。 In the present invention, the fiber reinforced resin sheet used for the workpiece holding material uses a woven fabric or a nonwoven fabric made of wholly aromatic polyester fibers as a fiber base material.
本発明において、芳香族ポリエステル繊維を織物として使用する場合、芳香族ポリエステル繊維の総繊度は５０〜４５０ｄｔｅｘであることが必要であり、１００〜３００ｄｔｅｘであることが好ましい。
総繊度が５０ｄｔｅｘ未満または４５０ｄｔｅｘを超えると、目標とする厚み、目付の織物にするには極端に密度を増やす、または減らす等が必要となり、織物の製造が難しくなる。
In the present invention, when the aromatic polyester fiber is used as a woven fabric, the total fineness of the aromatic polyester fiber needs to be 50 to 450 dtex, and preferably 100 to 300 dtex.
When the total fineness is less than 50 dtex or exceeds 450 dtex, it is necessary to extremely increase or decrease the density in order to obtain a target thickness and fabric weight, which makes it difficult to manufacture the fabric.
また、芳香族ポリエステル繊維を織物として使用する場合、芳香族ポリエステル繊維の単糸繊度は１０ｄｔｅｘ以下が好ましく、５ｄｔｅｘ以下がより好ましい。また、フィラメント数の範囲は３〜１０００が好ましく、１０〜８００がより好ましい。 Moreover, when using an aromatic polyester fiber as a woven fabric, the single yarn fineness of the aromatic polyester fiber is preferably 10 dtex or less, and more preferably 5 dtex or less. The range of the number of filaments is preferably 3 to 1000, more preferably 10 to 800.
一方、芳香族ポリエステル繊維を不織布として使用する場合、その繊度は１．０〜１０ｄｔｅｘであることが必要であり、１．５〜６．０ｄｔｅｘであることが好ましい。
繊度が１．０ｄｔｅｘ未満であると、繊維が細く機械特性、特に耐摩耗性に欠け、繊度が１０ｄｔｅｘを超えると、繊維同士が絡まりにくくなり不織布の製造が難しくなる。
On the other hand, when using an aromatic polyester fiber as a nonwoven fabric, the fineness is required to be 1.0 to 10 dtex, and preferably 1.5 to 6.0 dtex.
If the fineness is less than 1.0 dtex, the fibers are thin and lack mechanical properties, particularly wear resistance. If the fineness exceeds 10 dtex, the fibers are less likely to be entangled, making it difficult to produce a nonwoven fabric.
本発明における全芳香族ポリエステル繊維の強度は、１０．０ｃＮ／ｄｔｅｘ以上が好ましく、１２．０ｃＮ／ｄｔｅｘ以上がより好ましく、２０．０ｃＮ／ｄｔｅｘ以上が更に好ましい。
また、伸度は、５．０％以下が好ましく、３．５％以下がより好ましい。
更に、弾性率は、４００ｃＮ／ｄｔｅｘ以上が好ましく、５００ｃＮ／ｄｔｅｘ以上がより好ましい。
The strength of the wholly aromatic polyester fiber in the present invention is preferably 10.0 cN / dtex or more, more preferably 12.0 cN / dtex or more, and further preferably 20.0 cN / dtex or more.
Further, the elongation is preferably 5.0% or less, and more preferably 3.5% or less.
Furthermore, the elastic modulus is preferably 400 cN / dtex or more, and more preferably 500 cN / dtex or more.
繊維基材が織物の場合、その厚みは５０〜３００μｍ、目付は３０〜２００ｇ／ｍ２であることが必要であり、厚みは１００〜２５０μｍ、目付は５０〜１５０ｇ／ｍ２であることが好ましい。
厚みが５０μｍ未満では積層枚数が多くなりすぎて生産性が悪くなる傾向にあり、３００μｍを超えると厚み精度が悪くなる。
また、目付が３０ｇ／ｍ２未満では、繊維基材の機械強度が劣り、繊維強化樹脂シートの補強効果が不十分となる。一方、２００ｇ／ｍ２を超えると、繊維基材の空隙が少なく、熱硬化樹脂の含浸が難しくなり、繊維強化樹脂シートとして積層した際、他の繊維強化樹脂シートとの剥離が生じ、耐久性に劣るものとなる。
また、織組織は、平織物が好適である。
When the fiber substrate is a woven fabric, the thickness is required to be 50 to 300 μm, the basis weight is 30 to 200 g / m 2 , the thickness is preferably 100 to 250 μm, and the basis weight is preferably 50 to 150 g / m 2. .
If the thickness is less than 50 μm, the number of stacked layers tends to be too large, and the productivity tends to deteriorate, and if it exceeds 300 μm, the thickness accuracy deteriorates.
Moreover, if a fabric weight is less than 30 g / m < 2 >, the mechanical strength of a fiber base material will be inferior, and the reinforcement effect of a fiber reinforced resin sheet will become inadequate. On the other hand, when it exceeds 200 g / m 2 , there are few voids in the fiber base material and it is difficult to impregnate the thermosetting resin, and when laminated as a fiber reinforced resin sheet, peeling from other fiber reinforced resin sheets occurs, resulting in durability It becomes inferior to.
The woven structure is preferably a plain woven fabric.
一方、繊維基材が不織布の場合、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２であることが必要である。
厚みが８０μｍ未満では、積層枚数が多くなりすぎて生産性が悪くなる傾向にあり、１４０μｍを超えると、厚み精度が悪くなる。
また、目付が５０ｇ／ｍ２未満では、繊維基材の機械強度が劣り、繊維強化樹脂シートの補強効果が不十分となる。一方、１００ｇ／ｍ２を超えると、繊維基材の空隙が少なく、熱硬化樹脂の含浸が難しくなり、繊維強化樹脂シートとして積層した際、他の繊維強化樹脂シートとの剥離が生じ、耐久性に劣るものとなる。
On the other hand, when the fiber substrate is a nonwoven fabric, it is necessary that the thickness is 80 to 140 μm and the basis weight is 50 to 100 g / m 2 .
When the thickness is less than 80 μm, the number of stacked layers tends to be too large, and the productivity tends to deteriorate. When the thickness exceeds 140 μm, the thickness accuracy is deteriorated.
Moreover, if a fabric weight is less than 50 g / m < 2 >, the mechanical strength of a fiber base material will be inferior, and the reinforcement effect of a fiber reinforced resin sheet will become inadequate. On the other hand, when it exceeds 100 g / m 2 , there are few voids in the fiber base material, and it becomes difficult to impregnate the thermosetting resin, and when laminated as a fiber reinforced resin sheet, peeling from other fiber reinforced resin sheets occurs, and durability It becomes inferior to.
全芳香族ポリエステル繊維を不織布として用いる場合、短繊維をランダムに分散させたもので、上述の繊度、厚み及び目付を満たすように公知の方法で製造されたものでよい。短繊維の長さとしては０．１〜１０ｍｍが好ましい。短繊維の長さが０．１ｍｍ未満では繊維強化樹脂シートの補強効果が不十分となる傾向にあり、１０ｍｍを超えると分散性が低下する為、機械特性の斑や反りの発生が懸念される。 When using a wholly aromatic polyester fiber as a nonwoven fabric, short fibers are randomly dispersed and may be manufactured by a known method so as to satisfy the fineness, thickness, and basis weight described above. The length of the short fiber is preferably 0.1 to 10 mm. If the length of the short fiber is less than 0.1 mm, the reinforcing effect of the fiber reinforced resin sheet tends to be insufficient, and if it exceeds 10 mm, the dispersibility is lowered, and there is a concern about occurrence of mechanical property spots and warping. .
本発明において用いるアラミド繊維には、パラ系とメタ系があるが、パラ系を主成分としたアラミド繊維基材が好ましい。ここでパラ系アラミド繊維が好ましい理由は、パラ系アラミド繊維はメタ系アラミド繊維より繊維自体の引張り強度など力学的物性値が高く、被研磨物保持材の摩耗消耗を抑制してその寿命を延ばせるからである。また、パラ系アラミド繊維は、吸湿性がメタ系アラミド繊維より小さいので、水分のある研磨環境に好適である。
パラ系アラミド繊維としては、ポリｐ−フェニレンテレフタラミド繊維とポリｐ−フェニレンジフェニールエーテルテレフタラミド繊維が市販されており、これらが一般的である。
The aramid fiber used in the present invention includes a para type and a meta type, and an aramid fiber base material containing the para type as a main component is preferable. Here, the reason why the para-aramid fiber is preferable is that the para-aramid fiber has a higher mechanical property value such as tensile strength of the fiber itself than the meta-aramid fiber, and can suppress the wear consumption of the workpiece holding material and extend its life. Because. Moreover, since the para-aramid fiber has a hygroscopic property smaller than that of the meta-aramid fiber, it is suitable for a polishing environment with moisture.
As the para-aramid fiber, poly p-phenylene terephthalamide fiber and poly p-phenylene diphenyl ether terephthalamide fiber are commercially available, and these are common.
本発明に用いるアラミド繊維の製造は、公知の製造方法により行えばよい。 What is necessary is just to perform manufacture of the aramid fiber used for this invention by a well-known manufacturing method.
本発明において、アラミド繊維からなる繊維基材は、織物または不織布であり、本発明の主旨から、織物であることが好ましい。 In this invention, the fiber base material which consists of an aramid fiber is a woven fabric or a nonwoven fabric, and it is preferable that it is a woven fabric from the meaning of this invention.
本発明において、アラミド繊維を織物として使用する場合、その総繊度は５０〜４５０ｄｔｅｘであることが必要であり、１００〜３００ｄｔｅｘであることが好ましい。
総繊度が５０ｄｔｅｘ未満または４５０ｄｔｅｘを超えると、目標とする厚み、目付の織物にするには極端に密度を増やす、または減らす等が必要となり、織物の製造が難しくなる。
In this invention, when using an aramid fiber as a textile fabric, the total fineness needs to be 50-450 dtex, and it is preferable that it is 100-300 dtex.
When the total fineness is less than 50 dtex or exceeds 450 dtex, it is necessary to extremely increase or decrease the density in order to obtain a target thickness and fabric weight, which makes it difficult to manufacture the fabric.
また、アラミド繊維を織物として使用する場合、その単糸繊度は１０ｄｔｅｘ以下が好ましく、５ｄｔｅｘ以下がより好ましい。また、フィラメント数の範囲は３〜１０００が好ましく、１０〜８００がより好ましい。 Moreover, when using an aramid fiber as a woven fabric, the single yarn fineness is preferably 10 dtex or less, and more preferably 5 dtex or less. The range of the number of filaments is preferably 3 to 1000, more preferably 10 to 800.
一方、アラミド繊維を不織布として使用する場合、その繊度は１．０〜１０ｄｔｅｘであることが必要であり、１．５〜６．０ｄｔｅｘであることが好ましい。
繊度が１．０ｄｔｅｘ未満であると、繊維が細く機械特性、特に耐摩耗性に欠け、繊度が１０ｄｔｅｘを超えると、繊維同士が絡まりにくくなり不織布の製造が難しくなる。
On the other hand, when using an aramid fiber as a nonwoven fabric, the fineness is required to be 1.0 to 10 dtex, and preferably 1.5 to 6.0 dtex.
If the fineness is less than 1.0 dtex, the fibers are thin and lack mechanical properties, particularly wear resistance. If the fineness exceeds 10 dtex, the fibers are less likely to be entangled, making it difficult to produce a nonwoven fabric.
本発明におけるアラミド繊維の強度は、１０．０ｃＮ／ｄｔｅｘ以上が好ましく、１２．０ｃＮ／ｄｔｅｘ以上がより好ましく、２０．０ｃＮ／ｄｔｅｘ以上が更に好ましい。
また、伸度は、５．０％以下が好ましく、３．５％以下がより好ましい。
更に、弾性率は、４００ｃＮ／ｄｔｅｘ以上が好ましく、５００ｃＮ／ｄｔｅｘ以上がより好ましい。
The strength of the aramid fiber in the present invention is preferably 10.0 cN / dtex or more, more preferably 12.0 cN / dtex or more, and further preferably 20.0 cN / dtex or more.
Further, the elongation is preferably 5.0% or less, and more preferably 3.5% or less.
Furthermore, the elastic modulus is preferably 400 cN / dtex or more, and more preferably 500 cN / dtex or more.
アラミド繊維基材が織物の場合、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２であることが必要であり、厚みは１００〜２５０μｍ、目付は５０〜１５０ｇ／ｍ２であることが好ましい。
厚みが５０μｍ未満では積層枚数が多くなりすぎて生産性が悪くなる傾向にあり、３００μｍを超えると厚み精度が悪くなる。
また、目付が３０ｇ／ｍ２未満では、繊維基材の機械強度が劣り、繊維強化樹脂シートの補強効果が不十分となる。一方、２００ｇ／ｍ２を超えると、繊維基材の空隙が少なく、熱硬化樹脂の含浸が難しくなり、繊維強化樹脂シートとして積層した際、他の繊維強化樹脂シートとの剥離が生じ、耐久性に劣るものとなる。
また、織組織は、平織物が好適である。
If aramid fiber substrate fabric, a thickness of 50 to 300 [mu] m, it is necessary that the basis weight is 30 to 200 g / m 2, thickness 100 to 250 [mu] m, it is preferred basis weight is 50 to 150 g / m 2 .
If the thickness is less than 50 μm, the number of stacked layers tends to be too large, and the productivity tends to deteriorate, and if it exceeds 300 μm, the thickness accuracy deteriorates.
Moreover, if a fabric weight is less than 30 g / m < 2 >, the mechanical strength of a fiber base material will be inferior, and the reinforcement effect of a fiber reinforced resin sheet will become inadequate. On the other hand, when it exceeds 200 g / m 2 , there are few voids in the fiber base material and it is difficult to impregnate the thermosetting resin, and when laminated as a fiber reinforced resin sheet, peeling from other fiber reinforced resin sheets occurs, resulting in durability It becomes inferior to.
The woven structure is preferably a plain woven fabric.
アラミド繊維基材が不織布の場合、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２であることが必要である。
厚みが８０μｍ未満では、積層枚数が多くなりすぎて生産性が悪くなる傾向にあり、１４０μｍを超えると、厚み精度が悪くなる。
また、目付が５０ｇ／ｍ２未満では、繊維基材の機械強度が劣り、繊維強化樹脂シートの補強効果が不十分となる。一方、１００ｇ／ｍ２を超えると、繊維基材の空隙が少なく、熱硬化樹脂の含浸が難しくなり、繊維強化樹脂シートとして積層した際、他の繊維強化樹脂シートとの剥離が生じ、耐久性に劣るものとなる。
When the aramid fiber substrate is a nonwoven fabric, it is necessary that the thickness is 80 to 140 μm and the basis weight is 50 to 100 g / m 2 .
When the thickness is less than 80 μm, the number of stacked layers tends to be too large, and the productivity tends to deteriorate. When the thickness exceeds 140 μm, the thickness accuracy is deteriorated.
Moreover, if a fabric weight is less than 50 g / m < 2 >, the mechanical strength of a fiber base material will be inferior, and the reinforcement effect of a fiber reinforced resin sheet will become inadequate. On the other hand, when it exceeds 100 g / m 2 , there are few voids in the fiber base material, and it becomes difficult to impregnate the thermosetting resin, and when laminated as a fiber reinforced resin sheet, peeling from other fiber reinforced resin sheets occurs, and durability It becomes inferior to.
芳香族ポリエステル繊維不織布と同様に、アラミド繊維を不織布として用いる場合には、短繊維をランダムに分散させたもので、上述の繊度、厚み及び目付を満たすように公知の方法で製造されたものでよい。短繊維の長さとしては０．１〜１０ｍｍが好ましい。短繊維の長さが０．１ｍｍ未満では繊維強化樹脂シートの補強効果が不十分となる傾向にあり、１０ｍｍを超えると分散性が低下する為、機械特性の斑や反りの発生が懸念される。 Similar to the aromatic polyester fiber nonwoven fabric, when aramid fibers are used as the nonwoven fabric, short fibers are randomly dispersed and manufactured by a known method so as to satisfy the above-mentioned fineness, thickness and basis weight. Good. The length of the short fiber is preferably 0.1 to 10 mm. If the length of the short fiber is less than 0.1 mm, the reinforcing effect of the fiber reinforced resin sheet tends to be insufficient, and if it exceeds 10 mm, the dispersibility is lowered, and there is a concern about occurrence of mechanical property spots and warping. .
また、本発明において、熱硬化性樹脂は、エポキシ樹脂、ポリイミド樹脂、変性ポリイミド樹脂、フェノール樹脂、フェノールノボラック樹脂、クレゾールノボラック樹脂、メラミン樹脂、不飽和ポリエステル樹脂、環状オレフィン系重合体樹脂から選択されることが好ましい。特にエポキシ樹脂が好ましい。 In the present invention, the thermosetting resin is selected from an epoxy resin, a polyimide resin, a modified polyimide resin, a phenol resin, a phenol novolac resin, a cresol novolac resin, a melamine resin, an unsaturated polyester resin, and a cyclic olefin polymer resin. It is preferable. An epoxy resin is particularly preferable.
また、熱硬化性樹脂と熱可塑性樹脂を複合してもよい。あるいは樹脂中に、本発明の目的を阻害しない範囲で、着色剤など各種添加剤を含有させても良い。 Further, a thermosetting resin and a thermoplastic resin may be combined. Alternatively, various additives such as a colorant may be contained in the resin as long as the object of the present invention is not impaired.
また、本発明においては、被研磨物保持材中のチタン、マグネシウム、アルミニウム又はケイ素の金属元素含有量が各々２０ｐｐｍ以下であることが好ましく、１０ｐｐｍ以下であることがより好ましい。
上記金属元素が各々２０ｐｐｍを超えると、被研磨物を汚染し、製品歩留りを低下させる傾向にある。
In the present invention, the metal element content of titanium, magnesium, aluminum or silicon in the workpiece holding material is preferably 20 ppm or less, more preferably 10 ppm or less.
When each of the above metal elements exceeds 20 ppm, the object to be polished is contaminated and the product yield tends to be lowered.
本発明に係る繊維強化樹脂シートは、例えば、以下の方法により製造すればよい。すなわち、各繊維基材に、樹脂を含浸させ、乾燥させることにより、繊維強化シートを調製する。
具体的には、熱硬化性樹脂を用いる場合、熱硬化性樹脂を溶剤に溶解した樹脂組成物を調製し、それを前記繊維構造体に塗布後、バーコーターやクリアランスロールなどを用いて余分な樹脂組成物を掻き取ることにより、繊維強化シートを調製することができる。
What is necessary is just to manufacture the fiber reinforced resin sheet which concerns on this invention with the following method, for example. That is, each fiber base material is impregnated with a resin and dried to prepare a fiber reinforced sheet.
Specifically, when a thermosetting resin is used, a resin composition in which a thermosetting resin is dissolved in a solvent is prepared, and after applying it to the fiber structure, an extra portion is used using a bar coater or a clearance roll. A fiber reinforced sheet can be prepared by scraping off the resin composition.
次に、被研磨物保持材の成形は、繊維強化シートを、所望の順となるよう複数枚積層し、これらを接合することにより積層板とする。 Next, the material to be polished is molded by laminating a plurality of fiber reinforced sheets in a desired order and joining them to form a laminated plate.
複数枚の繊維強化シートを積層した後、これらを接合する方法としては、オートクレーブ成形法、圧縮成形法など公知の成形方法を採用することができ、目的とする形状や、熱硬化性樹脂や熱可塑性樹脂等の使用する樹脂の種類に応じて最適な成形方法を適用すれば良い。特に、オートクレーブ成形法と圧縮成形法が好ましく、繊維表面に付着した接着剤成分との化学結合を促進させ、前記繊維基材と樹脂との接着性向上をより効果的に発現させることができる。 After laminating a plurality of fiber reinforced sheets, a known molding method such as an autoclave molding method or a compression molding method can be employed as a method for joining them, and the desired shape, thermosetting resin or heat What is necessary is just to apply the optimal shaping | molding method according to the kind of resin to use, such as a plastic resin. In particular, an autoclave molding method and a compression molding method are preferable, and the chemical bond between the adhesive component attached to the fiber surface can be promoted, and the improvement in the adhesion between the fiber base material and the resin can be expressed more effectively.
得られた積層板を、平面研磨機の歯車と噛み合う駆動用ギアを外周に形成した円板状等の所望の形状に切削し、シリコンウエハなどの被研磨物を保持するための孔を１個から複数個形成することによって、本発明の被研磨物保持材が得られる。 The obtained laminated plate is cut into a desired shape such as a disk shape having a driving gear meshing with a gear of a surface polishing machine on the outer periphery, and one hole for holding an object to be polished such as a silicon wafer The material to be polished of the present invention is obtained by forming a plurality of materials.
以下に実施例を挙げて、本発明を具体的に説明する。
実施例及び比較例で作製した積層板の特性は、以下の方法により評価した。
The present invention will be specifically described below with reference to examples.
The properties of the laminates produced in the examples and comparative examples were evaluated by the following methods.
１）厚み精度
積層板を１０００ｍｍ×１０００ｍｍに成形し、周縁部８箇所と中央部１箇所の計９点をマイクロメーターで測定し、最大値と最小値の差で評価した。
1) Thickness accuracy The laminated plate was molded into 1000 mm × 1000 mm, a total of 9 points at the peripheral part and one central part were measured with a micrometer, and evaluated by the difference between the maximum value and the minimum value.
２）反り量
積層板を１０００ｍｍ×１０００ｍｍに成形し、水平板上に平置きしたときの端部の浮き上がり量の最大値で評価した。
2) Warpage amount The laminate was molded into 1000 mm x 1000 mm, and evaluated by the maximum value of the amount of lifting at the end when it was placed flat on a horizontal plate.
３）金属元素含有量
繊維基材を白金るつぼ中で炭化後、電気炉で灰化させ炭酸ナトリウム（Ｎａ２ＣＯ３）にてアルカリ融解させたものを超純水で定容し測定試料とした。ＩＣＰ発光分光分析装置（ＡＭＥＴＥＫ社製、ＣＩＲＯＳ ＣＣＤ）を用い、各金属元素の含有量を測定した。
3) Metal element content After carbonizing the fiber base material in a platinum crucible, it was ashed in an electric furnace and alkali-melted with sodium carbonate (Na 2 CO 3 ), and the volume was measured with ultrapure water to obtain a measurement sample. . The content of each metal element was measured using an ICP emission spectroscopic analyzer (CIROS CCD manufactured by AMETEK).
４）研磨試験
１０００ｍｍ×１０００ｍｍに成形した積層板を、直径１１インチの円盤状に加工すると共にその外周に複数枚の歯を形成し、更に直径３．５インチの保持孔を４個貫通加工して被研磨物保持材を作成した。ついで、この被研磨物保持材の保持孔に、被研磨物として直径３．５インチのアルミニウムハードディスクを嵌め込んだ状態で研磨装置に装着し、研磨装置を稼働させて研磨を行った。研磨を１００回繰り返し、計２０００枚の被研磨物の研磨を行った。
4) Polishing test A laminated plate molded to 1000 mm x 1000 mm was processed into a disk shape with an 11 inch diameter, a plurality of teeth were formed on the outer periphery, and four holding holes with a 3.5 inch diameter were further passed through. Thus, an object holding material was prepared. Next, an abrasive hard disk was fitted with a 3.5-inch diameter aluminum hard disk in the holding hole of the polished object holding material, and the polishing apparatus was operated to perform polishing. Polishing was repeated 100 times, and a total of 2000 workpieces were polished.
５）スクラッチ不良率
研磨試験後の被研磨物の表面状態を観察し、スクラッチの発生有無を調べ、不良率を求めた。
5) Scratch failure rate The surface state of the object to be polished after the polishing test was observed, the presence or absence of scratches was examined, and the failure rate was determined.
６）使用寿命
研磨試験時の被研磨物保持材の摩耗の程度で評価した。すなわち、使用可能な摩耗程度における使用可能なバッチ数を調べ、下記比較例３における使用可能なバッチ数を100としたときの指数で表した。
6) Service life Evaluation was made based on the degree of wear of the workpiece holding material during the polishing test. That is, the number of usable batches in the usable wear level was examined, and the index was expressed as an index when the number of usable batches in Comparative Example 3 below was defined as 100.
また、各繊維基材及び樹脂ワニスとして、以下のものを使用した。
１）基材１：全芳香族ポリエステル（ＬＣＰ）繊維織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、２２０ｄｔｅｘ／４８ｆ）、厚さ１５０μｍ、目付６０ｇ／ｍ２の平織織布）
２）基材２：全芳香族ポリエステル（ＬＣＰ）繊維織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、５６０ｄｔｅｘ／４８ｆ）、厚さ３５０μｍ、目付２５０ｇ／ｍ２の平織織布）
３）基材３：全芳香族ポリエステル（ＬＣＰ）繊維不織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、２．３ｄｔｅｘ×３ｍｍ）、厚さ１００μｍ、目付７０ｇ／ｍ２の湿式不織布）
４）基材４：全芳香族ポリエステル（ＬＣＰ）繊維不織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、０．８ｄｔｅｘ×３ｍｍ）、厚さ５０μｍ、目付３５ｇ／ｍ２の湿式不織布）
５）基材５：全芳香族ポリエステル（ＬＣＰ）繊維不織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、２．３ｄｔｅｘ×３ｍｍ）、厚さ１００μｍ、目付１８０ｇ／ｍ２の湿式不織布）
６）基材６：全芳香族ポリエステル（ＬＣＰ）繊維不織布（ＬＣＰ繊維（ＫＢセーレン社製、商品名：Ｚｘｉｏｎ、１１．７ｄｔｅｘ×３ｍｍ）、厚さ２００μｍ、目付１５０ｇ／ｍ２の湿式不織布）
７）基材７：アラミド繊維不織布（アラミド繊維（東レ・デュポン社製、商品名：Ｋｅｖｌｅｒ２９、１．７ｄｔｅｘ×３ｍｍ）、厚さ１００μｍ、目付７５ｇ／ｍ２の平織織布）
８）基材８：アラミド繊維不織布（アラミド繊維（東レ・デュポン社製、商品名：Ｋｅｖｌｅｒ２９、１．７ｄｔｅｘ×３ｍｍ）、厚さ２００μｍ、目付１６０ｇ／ｍ２の平織織布）
９）基材９：ガラス繊維織布（ガラス繊維（旭シュエ―ベル社製、商品名：Ａ２１１６／ＡＳ４５０）、厚さ１８０μｍ、目付２０９ｇ／ｍ２の平織織布）
１０）樹脂ワニス：硬化剤としてジシアンジアミド、硬化促進剤として２−エチル−４−メチルイミダゾールを配合したビスフェノールＡ型エポキシ樹脂ワニス
Moreover, the following were used as each fiber base material and resin varnish.
1) Substrate 1: Fully aromatic polyester (LCP) fiber woven fabric (LCP fiber (KB Selen Co., Ltd., trade name: Zxion, 220 dtex / 48f), thickness 150 μm, basis weight 60 g / m 2 plain woven fabric)
2) Substrate 2: Fully aromatic polyester (LCP) fiber woven fabric (LCP fiber (KB Selen, trade name: Zxion, 560 dtex / 48f), thickness 350 μm, basis weight 250 g / m 2 plain woven fabric)
3) Substrate 3: Totally aromatic polyester (LCP) fiber nonwoven fabric (LCP fiber (KB Selen Co., Ltd., trade name: Zxion, 2.3 dtex × 3 mm), thickness 100 μm, basis weight 70 g / m 2 wet nonwoven fabric)
4) Substrate 4: Fully aromatic polyester (LCP) fiber nonwoven fabric (LCP fiber (KB Selen Co., Ltd., trade name: Zxion, 0.8 dtex × 3 mm), thickness 50 μm, basis weight 35 g / m 2 wet nonwoven fabric)
5) Substrate 5: wholly aromatic polyester (LCP) fiber nonwoven fabric (LCP fiber (manufactured by KB Selen, trade name: Zxion, 2.3 dtex × 3 mm), wet nonwoven fabric having a thickness of 100 μm and a basis weight of 180 g / m 2 )
6) Substrate 6: wholly aromatic polyester (LCP) fiber nonwoven fabric (LCP fiber (trade name: Zxion, 11.7 dtex × 3 mm), 200 μm thick, 150 g / m 2 wet nonwoven fabric)
7) Substrate 7: Aramid fiber nonwoven fabric (Aramid fiber (trade name: Kevler 29, 1.7 dtex × 3 mm), 100 μm thickness, plain weave woven fabric with a basis weight of 75 g / m 2 )
8) Substrate 8: Aramid fiber nonwoven fabric (Aramid fiber (trade name: Kevler 29, 1.7 dtex × 3 mm), thickness 200 μm, plain weave woven fabric with a basis weight of 160 g / m 2 )
9) Substrate 9: Glass fiber woven fabric (glass fiber (manufactured by Asahi Shebel Co., Ltd., trade name: A2116 / AS450), thickness 180 μm, basis weight 209 g / m 2 plain woven fabric)
10) Resin varnish: Bisphenol A type epoxy resin varnish containing dicyandiamide as a curing agent and 2-ethyl-4-methylimidazole as a curing accelerator
（実施例１）
基材１に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＡを得た。
得られたプリプレグＡを８枚積層し、２枚の鏡面板に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０MＰａで加熱加圧成形を行い、積層板１を得た。
Example 1
A resin varnish was applied to the substrate 1, impregnated, and then semi-cured by drying to obtain prepreg A.
Eight prepregs A obtained were laminated, sandwiched between two mirror plates, heated and pressed at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 minutes, and a pressure of 3.0 MPa, and laminated. A plate 1 was obtained.
（実施例２）
基材３に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＢを得た。
得られたプリプレグＢを１２枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板２を得た。
(Example 2)
A resin varnish was applied to the substrate 3, and after impregnation, semi-curing was performed by drying to obtain a prepreg B.
Twelve prepregs B obtained were laminated, sandwiched between two mirror plates, heated and pressure-molded at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 min, and a pressure of 3.0 MPa. Plate 2 was obtained.
（実施例３）
基材７に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグCを得た。
両外層にプリプレグCを３枚ずつ、中間層にプリプレグＡを４枚、計１０枚のプリプレグを２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板３を得た。
Example 3
A resin varnish was applied to the base material 7, impregnated, and then semi-cured by drying to obtain prepreg C.
Three prepregs C on both outer layers, four prepregs A on the intermediate layer, a total of 10 prepregs sandwiched between two mirror plates, a heating rate of 2.0 ° C / min, a curing temperature of 175 ° C x 60 minutes Then, heat and pressure molding was performed at a pressure of 3.0 MPa to obtain a laminate 3.
（実施例４）
両外層にプリプレグＣを３枚ずつ、中間層にプリプレグＢを６枚、計１２枚のプリプレグを２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板４を得た。
Example 4
Three prepregs C on both outer layers, six prepregs B on the intermediate layer, a total of 12 prepregs are sandwiched between two mirror plates, heating rate 2.0 ° C / min, curing temperature 175 ° C x 60 minutes Then, heat-press molding was performed at a pressure of 3.0 MPa to obtain a laminate 4.
（実施例５）
基材８に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＤを得た。
両外層にプリプレグＤを２枚ずつ、中間層にプリプレグＢを４枚、計８枚のプリプレグを２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板５を得た。
(Example 5)
A resin varnish was applied to the substrate 8, impregnated, and then semi-cured by drying to obtain a prepreg D.
Two prepregs D on both outer layers, 4 prepregs B on the intermediate layer, a total of 8 prepregs sandwiched between 2 mirror plates, heating rate 2.0 ° C / min, curing temperature 175 ° C x 60 min Then, heat-press molding was performed at a pressure of 3.0 MPa to obtain a laminate 5.
（比較例１）
基材２に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＥを得た。
プリプレグＥを４枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板６を得た。
(Comparative Example 1)
A resin varnish was applied to the substrate 2, and after impregnation, semi-curing was performed by drying to obtain a prepreg E.
Four prepregs E are laminated, sandwiched between two mirror plates, and heated and pressed at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 minutes, and a pressure of 3.0 MPa. Obtained.
（比較例２）
基材４に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＦを得た。
プリプレグＦを３０枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板７を得た。
(Comparative Example 2)
A resin varnish was applied to the substrate 4, and after impregnation, semi-curing was performed by drying to obtain a prepreg F.
30 sheets of prepreg F are laminated, sandwiched between two mirror plates, and heated and pressed at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. for 60 minutes, and a pressure of 3.0 MPa. Obtained.
（比較例３）
基材６に樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＧを得た。
プリプレグＧを６枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板８を得た。
(Comparative Example 3)
A resin varnish was applied to the substrate 6, and after impregnation, semi-curing was performed by drying to obtain a prepreg G.
Six prepregs G are laminated, sandwiched between two mirror plates, heated and pressure-molded at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 minutes, and a pressure of 3.0 MPa. Obtained.
（比較例４）
基材５に樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＨを得た。
プリプレグＨを１１枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板９を得た。
(Comparative Example 4)
A resin varnish was applied to the substrate 5, and after impregnation, semi-curing was performed by drying to obtain a prepreg H.
Eleven prepregs H are laminated, sandwiched between two mirror plates, heated and pressure-molded at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 minutes, and a pressure of 3.0 MPa. Obtained.
（比較例５）
基材８に、樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＩを得た。
両外層にプリプレグＩを２枚ずつ、中間層にプリプレグＧを２枚、計６枚のプリプレグを２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板１０を得た。
(Comparative Example 5)
A resin varnish was applied to the substrate 8, and after impregnation, semi-curing was performed by drying to obtain a prepreg I.
Two prepregs I on both outer layers, two prepregs G on the middle layer, a total of six prepregs sandwiched between two mirror plates, heating rate 2.0 ° C / min, curing temperature 175 ° C x 60 mins The laminated plate 10 was obtained by heat and pressure molding at a pressure of 3.0 MPa.
（比較例６）
基材９に樹脂ワニスを塗布し、含浸後、乾燥により半硬化を行い、プリプレグＪを得た。
プリプレグＪを６枚積層し、２枚の鏡面板の間に挟み、昇温速度２．０℃／分、硬化温度１７５℃×６０分、圧力３．０ＭＰａで加熱加圧成形を行い、積層板１１を得た。
(Comparative Example 6)
A resin varnish was applied to the substrate 9, and after impregnation, semi-curing was performed by drying to obtain a prepreg J.
Six prepregs J are laminated, sandwiched between two mirror plates, heated and pressure-molded at a heating rate of 2.0 ° C./min, a curing temperature of 175 ° C. × 60 minutes, and a pressure of 3.0 MPa. Obtained.
これらの積層板について、物性及び評価結果を表１に併せて示す。 Table 1 shows the physical properties and evaluation results of these laminates.
表１の結果より、実施例の積層板は、厚み精度が良好で、反りが起こらず、耐久性にも優れたものであった。また、チタン、マグネシウム、アルミニウム又はケイ素の金属元素含有量が少なく、被研磨物保持材の表面のスクラッチの発生が殆ど無かった。
一方、比較例の積層板は、厚み精度、反り量、耐久性、スクラッチの発生すべてを満足するものではなかった。特に、比較例４の積層板は、使用により、剥離が生じ、耐久性に劣るものであった。
From the results in Table 1, the laminates of the examples had good thickness accuracy, no warpage, and excellent durability. Moreover, there was little metal element content of titanium, magnesium, aluminum, or silicon, and there was almost no generation | occurrence | production of the scratch of the surface of a to-be-polished material holding material.
On the other hand, the laminate of the comparative example did not satisfy all the thickness accuracy, warpage, durability, and generation of scratches. In particular, the laminate of Comparative Example 4 was peeled off due to use and was inferior in durability.
Claims (5)
（１）総繊度が５０〜４５０ｄｔｅｘの全芳香族ポリエステルマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（２）繊度が１．０〜１０ｄｔｅｘの全芳香族ポリエステルモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。 A workpiece holding material formed by laminating a plurality of fiber reinforced resin sheets impregnated with a thermosetting resin into a fiber base material, wherein the fiber reinforced resin sheet is a fiber according to the following (1) or (2) A polished article holding material comprising a fiber reinforced resin sheet used as a substrate.
(1) A woven fabric having a total fineness of 50 to 450 dtex and a total aromatic polyester multifilament having a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(2) A non-woven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of wholly aromatic polyester monofilament having a fineness of 1.0 to 10 dtex.
（ａ）総繊度が５０〜４５０ｄｔｅｘのアラミドマルチフィラメントからなる、厚みが５０〜３００μｍ、目付が３０〜２００ｇ／ｍ２である織物。
（ｂ）繊度が１．０〜１０ｄｔｅｘのアラミドモノフィラメントからなる、厚みが８０〜１４０μｍ、目付が５０〜１００ｇ／ｍ２の不織布。 The fiber reinforced resin sheet is formed by laminating three or more fiber reinforced resin sheets, and the outer fiber reinforced resin sheet is a fiber reinforced resin sheet using the following (a) or (b) as a fiber base material. 1. A workpiece holding material according to 1.
(A) A woven fabric having an aramid multifilament having a total fineness of 50 to 450 dtex and a thickness of 50 to 300 μm and a basis weight of 30 to 200 g / m 2 .
(B) A nonwoven fabric having a thickness of 80 to 140 μm and a basis weight of 50 to 100 g / m 2 made of an aramid monofilament having a fineness of 1.0 to 10 dtex.
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