JPWO2018025915A1 - Polishing jig - Google Patents

Abstract

A polishing jig comprising a laminate having a thermosetting resin layer and a thermoplastic resin layer, wherein the thermosetting resin layer contains an organic fiber aggregate, and the thermoplastic resin layer contains an organic fiber aggregate. And a polishing jig in which the thermosetting resin layer is disposed on both surfaces of the laminate. At this time, it is preferable that the laminate is a three-layer structure including the thermosetting resin layer, the thermoplastic resin layer, and the thermosetting resin layer in this order. This polishing jig has high flexural modulus and flexural strength.

Description

  The present invention relates to a polishing jig made of a laminate having a thermosetting resin layer and a thermoplastic resin layer. The present invention also relates to a method of manufacturing the polishing jig. Furthermore, the present invention relates to a polishing method using the above-mentioned polishing jig.

  Conventionally, in the process of manufacturing an aluminum substrate for a semiconductor wafer or a hard disk, there is a process of polishing the surface of the plate-like body. In this polishing step, a polishing jig is used to hold the plate-like body. Generally, the polishing jig has a plurality of through holes, and the plate-like body is held by the through holes. Then, the plate-like body is polished by driving the polishing jig.

  Heretofore, the present inventors have been polishing jigs made of a laminate having a base material layer and a resin layer, and the base material layer is made of an aggregate of organic fibers impregnated with a thermosetting resin, The resin layer is made of a thermosetting resin containing no organic fiber, and the laminate has a resin layer between a plurality of base layers and a polishing jig having a resin layer on both surfaces was reported (patented) Literature 1). However, when the plate-like body is polished using this polishing jig, there is a problem that fibers and foreign substances drop out of the jig during polishing and a scratch is generated on the plate-like body. Moreover, the production cost is high and the practical application is difficult.

  In order to solve such a problem, the present inventors are polishing jigs which consist of a laminated board which has a base material layer and a resin layer, and the above-mentioned base material layer is an organic fiber aggregate with which resin was impregnated. A polishing jig comprising a body, the resin layer containing a cyclic olefin polymer and no organic fiber, and the laminate having a resin layer between a plurality of base layers and a resin layer on both surfaces (Patent Document 2). This polishing jig is less likely to cause scratches on the plate-like body than the polishing jig described in Patent Document 1, and the manufacturing cost is also suppressed, but depending on the application, it has a bending elastic modulus and strength. There was a case that became insufficient.

  In recent years, the requirements for the performance and manufacturing cost of the polishing jig have been increasingly intensified, and a polishing jig having a high flexural modulus and flexural strength and which can be manufactured inexpensively has been desired.

International Publication No. 2015/056664 WO 2015/170556

  The present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a polishing jig which has high flexural modulus and flexural strength and can be manufactured inexpensively.

  The subject is a polishing jig comprising a laminate having a thermosetting resin layer and a thermoplastic resin layer; the thermosetting resin layer includes an organic fiber aggregate, and the thermoplastic resin layer is an organic fiber The problem is solved by providing a polishing jig which is characterized in that the thermosetting resin layer is disposed on both surfaces of the laminate without including an aggregate.

  At this time, it is preferable that the laminate is a three-layer structure including the thermosetting resin layer, the thermoplastic resin layer, and the thermosetting resin layer in this order.

  The thermoplastic resin layer preferably contains at least one polymer selected from the group consisting of polyolefins, polyesters and poly (meth) acrylates. Moreover, it is preferable that the said thermosetting resin layer contains an epoxy resin or a phenol resin.

  It is preferable that the fiber which comprises the said organic fiber assembly is at least 1 type of fiber selected from the group which consists of a polyarylate fiber, an aramid fiber, and a polyphenylene sulfide fiber. Moreover, it is preferable that the said organic fiber aggregate is a woven fabric or a knitted fabric.

  It is preferable that the total thickness of the said laminated board is 100-5000 micrometers. Moreover, in the laminated board, it is preferable that the total thickness of the thermoplastic resin layer is 0.2 to 10 times the total thickness of the thermosetting resin layer.

  It is preferable that the said laminated board is a three-layer structure, and the thickness of the said thermosetting resin layer of the surface is 0.05-5 times of the said thermoplastic resin layer of all center.

  The subject is a method for producing the polishing jig; a first step of impregnating the organic fiber aggregate with a thermosetting resin to obtain a prepreg, the prepreg obtained in the first step, and a thermoplastic resin And a second step of obtaining a laminate by laminating and heating and pressing the sheet consisting of the above-mentioned prepregs on both surfaces, and forming a through hole for holding the plate-like body to be polished in the laminate. It is also solved by providing the manufacturing method of a grinding jig provided with the 3rd process to do.

  A preferred embodiment of the present invention is a polishing method in which a plate-like body is held by the above-mentioned polishing jig and the plate-like body is polished.

  According to the present invention, it is possible to provide a polishing jig which has high flexural modulus and flexural strength and which can be manufactured inexpensively.

7 is a cross-sectional image of the polishing jig in Example 1. FIG. 2 is a plan view of a polishing jig in Example 1; 7 is a cross-sectional image of a polishing jig in Comparative Example 1; 7 is a cross-sectional image of a resin jig in Comparative Example 2; 7 is a cross-sectional image of a resin jig in Comparative Example 3;

  The present invention is a polishing jig comprising a laminate having a thermosetting resin layer and a thermoplastic resin layer, wherein the thermosetting resin layer includes an organic fiber aggregate, and the thermoplastic resin layer is an organic fiber aggregate. And a thermosetting resin layer is disposed on both surfaces of the laminate. A polishing jig satisfying the above-described configuration has high flexural modulus and flexural strength, and can be manufactured inexpensively.

  In the present invention, it is important that the thermosetting resin layer contains an organic fiber aggregate. By arranging such layers on both surfaces of the polishing jig, the flexural modulus and the flexural strength are improved.

  It is preferable that the fibers constituting the organic fiber assembly be at least one fiber selected from the group consisting of polyarylate fibers, aramid fibers and polyphenylene sulfide fibers. Among them, polyarylate fibers are more preferable because they are less in the amount of metal impurities such as Al, Mg, Ti and Si, and are excellent in the strength of the obtained polishing jig.

It is preferable that the organic fiber assembly is a woven or knitted fabric. In the case of a woven fabric, plain weave, twill weave, entangled weave, barbed weave, multiple weave, etc. may be mentioned. In the case of a knitted fabric, Russell, Tricot, Miranees, etc. may be mentioned. The fabric weight of the woven or knitted fabric is usually 5 g / m ² or more, and preferably 30 g / m ² or more from the viewpoint of improving the strength of the polishing jig. On the other hand, the fabric weight of the woven or knitted fabric is usually 500 g / m ² or less. The organic fiber assembly is more preferably a woven fabric from the viewpoint of obtaining a product with higher strength.

  It is preferable that the thermosetting resin layer contains an epoxy resin or a phenol resin. Among these, from the viewpoint of chemical resistance, it is more preferable to include an epoxy resin. As an epoxy resin, bisphenol-type epoxy resins, such as a bisphenol A-type epoxy resin; Novolak-type epoxy resins, such as a phenol novolak-type epoxy resin, etc. are illustrated. The thermosetting resin may contain a common curing agent or curing accelerator. Examples of the curing agent and the curing accelerator when the thermosetting resin is an epoxy resin include amine compounds.

  In the present invention, it is important that the thermoplastic resin layer does not contain an organic fiber aggregate. When the thermoplastic resin layer contains an organic fiber aggregate, a beard may be generated in the thermoplastic resin layer, or the organic fibers may be dropped from the thermoplastic resin layer, and foreign matter may adhere to the plate-like body. Or scratching occurs. At this time, as long as the effects of the present invention are not impaired, the thermoplastic resin layer may contain a slight amount of organic fibers. However, it is preferable that the thermoplastic resin layer contains no organic fiber at all, from the viewpoint of completely suppressing the generation of the whiskers in the thermoplastic resin layer and the detachment of the organic fiber from the resin layer.

  In the present invention, preferably, the thermoplastic resin layer contains at least one polymer selected from the group consisting of polyolefin, polyester and poly (meth) acrylate. Among them, polyolefins are more preferable, and cyclic olefin polymers are more preferable.

  Cyclic olefin polymers are polymers excellent in heat resistance, heat aging resistance, chemical resistance, weather resistance, solvent resistance, dielectric properties, rigidity and the like, and by using cyclic olefin polymers, strength and durability are obtained. It is possible to obtain an excellent polishing jig. Since the cyclic olefin polymer is non-crystalline, the dimensional accuracy of the obtained polishing jig is good. Further, since the cyclic olefin polymer is a thermoplastic resin, it can be melted by heating, and the productivity of the polishing jig is improved.

  The cyclic olefin polymer may be formed by polymerizing only an olefin monomer having an aliphatic cyclic skeleton, or an amount which is copolymerizable with the olefin monomer having an aliphatic cyclic skeleton It may be a copolymer with the body. The copolymerization amount of the other monomers is usually less than 50% by mass, preferably less than 30% by mass. The cyclic olefin polymer may be a resin composition containing a cyclic olefin polymer as a main component and other components. The main component is usually a component whose content is 50% by mass or more, preferably a component whose content is 80% by mass or more.

  The cyclic olefin polymer is a non-crystalline, transparent polymer having a saturated hydrocarbon ring structure in the main chain or side chain of the polymer, and specifically, JP-A-63-264646, JP-A A ring-opened polymer of a monomer having a norbornene ring disclosed in JP-A 64-1705, JP-A-1-168724, JP-A-1-168725, etc. and a hydrogenated product thereof, JP-A-60-168708 The addition polymer of a monomer having a norbornene ring and an α-olefin disclosed in Japanese Patent Laid-Open Publications, etc., cyclic olefins and cyclic dienes disclosed in JP-A-6-136057, JP-A-7-258362 and the like Addition polymers and their hydrogenated products, resin compositions containing cyclic olefin polymers and soft copolymers disclosed in WO 2006/025294, etc. It can gel. Such a resin composition is, for example, a trade name from Fuji Bakelite Co., Ltd. under the trade name "e-mateX", a trade name from Mitsui Chemical Co., Ltd. under the trade name "Appel", a name from "Topass", a trade name from Nippon Zeon Co., Ltd. They are sold under the names "Zeonex" and "Zeonor", and commercially available products can be easily obtained. Since these commercial products are often added with additives for improving durability and moldability, the resin before adding the additives is used from the viewpoint of preventing foreign substances from falling off during polishing. In some cases, it is preferable to mold. In some cases, it may be preferable to use a resin having a particularly reduced catalyst residue and residual volatile content.

  The resin layer preferably comprises a resin composition containing a cyclic olefin polymer and a soft copolymer. The impact resistance and abrasion resistance of the polishing jig can be further improved by the polishing jig having such a resin layer. The resin layer is particularly selected from at least two or more kinds selected from the group consisting of 100 parts by mass of a cyclic olefin polymer (A) having a glass transition temperature of 60 to 200 ° C., an olefin, a diene and an aromatic vinyl hydrocarbon 1 to 50 parts by mass of a soft copolymer (B) having a glass transition temperature of 0 ° C. or less, 0.001 to 1 parts by mass of a radical initiator (C), and a radically polymerizable functional group It is more preferable to consist of a resin composition formed by melt-kneading 0 to 1 part by mass of a polyfunctional compound (D) having two or more of them in a molecule.

  Hereinafter, the cyclic olefin polymer (A), the soft copolymer (B), the radical initiator (C) and the polyfunctional compound (D) having two or more radical polymerizable functional groups in the molecule will be described.

  First, the cyclic olefin polymer (A) will be described. The cyclic olefin polymer (A) used in the present invention preferably has a glass transition temperature of 60 to 200 ° C. From the viewpoint of further improving the heat resistance of the polishing jig, the temperature is preferably 80 ° C. or more, more preferably 100 ° C. or more. In addition, the glass transition temperature is preferably 200 ° C. or less because there is a risk of decomposition if the molding temperature is too high. The glass transition temperature in the present invention is a glass transition start temperature measured at a temperature rising rate of 10 ° C./min using a differential scanning calorimeter (DSC).

  The MFR (melt flow rate: measured at 230 ° C. and a 2.16 kg load) of the cyclic olefin polymer (A) is preferably 0.1 to 500 g / 10 min. When the MFR is less than 0.1 g / 10 minutes, the melt viscosity is too high, and the melt moldability of the obtained resin composition may be deteriorated. The MFR is more preferably 0.5 g / 10 min or more, still more preferably 1 g / 10 min or more. On the other hand, when the MFR exceeds 500 g / 10 min, the mechanical strength of the obtained resin composition may be reduced. The MFR is more preferably 200 g / 10 min or less, still more preferably 100 g / 10 min or less.

  The cyclic olefin polymer (A) is formed by polymerizing an olefin monomer having an aliphatic cyclic skeleton, and the polymer obtained may have an aliphatic cyclic skeleton, and the type thereof is not limited. The cyclic olefin polymer (A) is preferably a polymer obtained by polymerizing a cyclic olefin represented by the following formula [I] or [II].

(In the above formula [I], n is 0 or 1, m is 0 or a positive integer, q is 0 or 1, and R ^{1 to} R ¹⁸ and R ^a and R ^b are each independently R ^{15 to} R ¹⁸ may be bonded to each other to form a monocyclic or polycyclic ring, and the monocyclic or polycyclic ring has a double bond. And R ¹⁵ and R ¹⁶ or R ¹⁷ and R ¹⁸ may form an alkylidene group).

(In the formula [II], p and q are 0 or an integer of 1 or more, m and n are 0, 1 or 2, and R ^{1 to} R ¹⁹ each independently represent a hydrogen atom, a halogen atom, an aliphatic carbon And a carbon atom to which R ⁹ (or R ¹⁰ ) is bonded, which is a hydrogen group, an alicyclic hydrocarbon group, an aromatic hydrocarbon group or an alkoxy group, and a carbon atom to which R ¹³ or R ¹¹ is bonded May be bonded directly or via an alkylene group of 1 to 3 carbon atoms, and when n = m = 0, R ¹⁵ and R ¹² or R ¹⁵ and R ¹⁹ are bonded to each other to form a single ring or It may form a polycyclic aromatic ring.)

(A1), (a2), (a3) and (a4) which are shown below as a polymer formed by polymerizing cyclic olefin shown by the above-mentioned formula [I] or [II] are illustrated as a suitable thing .
(A1): random copolymer of ethylene and cyclic olefin represented by the above formula [I] or [II] (ethylene-cyclic olefin random copolymer)
(A2): ring-opened polymer or ring-opened copolymer of cyclic olefin represented by the above formula [I] or [II] (a3): hydride (a4) of (a2): (a1), (a2) ) Or graft modified products of (a3)

  Among these, ethylene-cyclic olefin random copolymer (a1), that is, a random copolymer of ethylene and a cyclic olefin represented by the above-mentioned formula [I] or [II] is preferably used. Such ethylene-cyclic olefin random copolymer (a1) is suitably used because it is excellent in abrasion resistance and a resin composition with a small amount of volatile component released can be obtained.

At this time, as the cyclic olefin represented by the above-mentioned formula [I] or [II] used as a raw material of the ethylene-cyclic olefin random copolymer (a1), preferred is from the viewpoint of heat resistance and easy availability. as, tetracyclo [4.4.0.1 ^2,5 .1 ^7,10] -3- dodecene and derivatives hydrocarbon group substituted thereto is illustrated, tetracyclo [4.4.0.1 ^2,5 .1 ⁷ as particularly suitable ^{, 10} ] -3-Dodecene is exemplified.

  The ethylene content in the ethylene-cyclic olefin random copolymer (a1) is preferably 40 to 85 mol% from the viewpoint of heat resistance, rigidity and the like. The ethylene content is more preferably 50 mol% or more. Further, the ethylene content is more preferably 75 mol% or less. On the other hand, the content of the cyclic olefin is preferably 15 to 60 mol%. The content of cyclic olefin is more preferably 25 mol% or more. Further, the content of cyclic olefin is more preferably 50 mol% or less.

  Next, the soft copolymer (B) will be described. The glass transition temperature of the soft copolymer (B) is preferably 0 ° C. or less. The glass transition temperature is preferably −10 ° C. or less, more preferably −20 ° C. or less. Moreover, normally, a glass transition temperature is -100 degreeC or more. The degree of crystallinity measured by the X-ray diffraction method is preferably 0 to 30%, more preferably 0 to 25%.

  It is preferable that the MFR (melt flow rate: measured at 230 ° C., 2.16 kg load) of the soft copolymer (B) is 0.01 to 200 g / 10 min. If the MFR is less than 0.01 g / 10 min, the melt viscosity is too high, and the melt moldability of the resulting resin composition may be deteriorated. The MFR is more preferably 0.05 g / 10 min or more, still more preferably 0.1 g / 10 min or more. On the other hand, when the MFR exceeds 200 g / 10 min, the mechanical strength of the obtained polishing jig may be reduced. The MFR is more preferably 150 g / 10 min or less, still more preferably 100 g / 10 min or less. Further, it is preferable to use one having an intrinsic viscosity [[] of 0.01 to 10 dl / g, preferably 0.08 to 7 dl / g, which is measured in 135 ° C. decalin.

The soft copolymer (B) is preferably obtained by polymerizing at least two or more monomers selected from the group consisting of olefins, dienes and aromatic vinyl hydrocarbons. At this time, as the soft copolymer (B), (b1), (b2), (b3) and (b4) shown below are exemplified as preferable ones.
(B1): A non-crystalline or low crystalline soft copolymer (b2) formed by polymerizing at least two or more monomers selected from the group consisting of ethylene and an α-olefin having 3 to 20 carbon atoms ): Soft copolymer obtained by polymerizing ethylene, α-olefin having 3 to 20 carbon atoms, and cyclic olefin (b3): non-conjugated diene, ethylene and α-olefin having 3 to 20 carbon atoms A soft copolymer (b4) formed by polymerizing at least two or more monomers selected from the group consisting of: a random or block copolymer of an aromatic vinyl hydrocarbon and a conjugated diene or a hydride thereof Some soft copolymer

  Next, the radical initiator (C) will be described. The type of radical initiator (C) is not particularly limited as long as it can be thermally decomposed by heating at the time of melt-kneading to generate radicals. Peroxides, azo compounds, redox initiators and the like can be mentioned. However, metal-containing ones are not preferable because metal residues are mixed in the polishing jig. Moreover, the thing containing a nitrogen element like an azo compound has a possibility that a nitrogen-containing compound may volatilize from a grinding jig, and may be unpreferable. Therefore, organic peroxides are preferably employed. The radical initiator (C) preferably decomposes at an appropriate rate at the time of melt-kneading, and the half-life temperature thereof is preferably 30 to 250 ° C. The one-minute half-life temperature is more preferably 50 ° C. or more and 200 ° C. or less.

  Examples of the organic peroxide used as the radical initiator (C) include ketone peroxides such as methyl ethyl ketone peroxide and cyclohexanone peroxide; 1,1-bis (t-butylperoxy) cyclohexane and 2,2-bis Peroxyketals such as (t-butylperoxy) octane; t-butylhydroperoxide, cumene hydroperoxide, 2,5-dimethylhexane-2,5-dihydroxyperoxide, 1,1,3,3- Hydroperoxides such as tetramethylbutyl hydroperoxide; di-tert-butyl peroxide, 2,5-dimethyl-2,5-bis (tert-butylperoxy) hexane, 2,5-dimethyl-2,5 -Dialkyl peroxides such as bis (t-butylperoxy) hexyne-3; diacyl peroxides such as lauroyl peroxide and benzoyl peroxide Oxides; t-butyl peroxy acetate, t- butyl peroxybenzoate, 2,5-dimethyl-2,5-bis (benzoyl peroxy) may be mentioned hexane peroxy esters such like.

  Next, the polyfunctional compound (D) having two or more radically polymerizable functional groups in the molecule will be described. Examples of the polyfunctional compound (D) include divinyl benzene, vinyl acrylate, vinyl methacrylate, triaryl isocyanurate, diaryl phthalate, ethylene dimethacrylate, and trimethylolpropane trimethacrylate.

  And a resin composition can be obtained by melt-kneading cyclic olefin polymer (A), a soft copolymer (B), a radical initiator (C), and a polyfunctional compound (D).

  It is preferable that the compounding quantity of a soft copolymer (B) is 1-50 mass parts with respect to 100 mass parts of cyclic olefin polymers (A). When the blending amount of the soft copolymer (B) is less than 1 part by mass, the improvement of the abrasion resistance becomes insufficient, and it is preferably 5 parts by mass or more. On the other hand, when the content of the soft copolymer (B) exceeds 50 parts by mass, the rigidity of the obtained laminate decreases, which may make it difficult to use as a polishing jig. It is below a mass part.

  It is preferable that the compounding quantity of a radical initiator (C) is 0.001-1 mass part with respect to 100 mass parts of cyclic olefin polymers (A). When the blending amount of the radical initiator (C) is less than 0.001 parts by mass, the crosslinking reaction does not proceed sufficiently and the improvement of the abrasion resistance becomes insufficient, and preferably 0.01 parts by mass or more. is there. On the other hand, when the compounding quantity of a radical initiator (C) exceeds 1 mass part, there exists a possibility that contamination resistance may deteriorate and it is 0.5 mass part or less suitably.

  It is preferable that the compounding quantity of a polyfunctional compound (D) is 0-1 mass part with respect to 100 mass parts of cyclic olefin polymers (A). The compounding of the polyfunctional compound (D) is optional and may not be compounded, but is preferably compounded in order to allow the crosslinking reaction to proceed efficiently. In that case, the preferable blending amount is 0.001 parts by mass or more, and more preferably 0.01 parts by mass or more. On the other hand, when the compounding quantity of a polyfunctional compound (D) exceeds 1 mass part, there exists a possibility that stain resistance may deteriorate, and it is 0.5 mass part or less suitably.

  The cyclic olefin polymer (A) used in the present invention is preferably an acid-modified cyclic olefin polymer from the viewpoint of adhesion to the substrate layer. Such an acid-modified cyclic olefin polymer can be produced by blending a cyclic olefin polymer (A) with a modifier so as to obtain a desired amount of acid modification, and graft polymerizing the polymer, or modifying the polymer in advance with a high modification rate It can also be prepared by preparing the product and then mixing this modified product with the unmodified cyclic olefin polymer. At this time, in the polymer contained in the resin layer, the content of the unit derived from the unsaturated carboxylic acid unit or the anhydride thereof is preferably 0.1 to 5% by mass. When the content is less than 0.1% by mass, excellent adhesion with the base material layer may not be obtained, and 0.2% by mass or more is more preferable. On the other hand, if the content exceeds 5% by mass, the contamination resistance may be poor, and the content is more preferably 3% by mass or less.

  As the modifier, unsaturated carboxylic acids are usually used. Specifically, (meth) acrylic acid, maleic acid, fumaric acid, tetrahydrophthalic acid, itaconic acid, citraconic acid, crotonic acid, isocrotonic acid, endocis-bicyclo [2.2.1] Unsaturated carboxylic acids such as hept-5-ene-2,3-dicarboxylic acid (nadic acid), derivatives of these unsaturated carboxylic acids such as unsaturated carboxylic acid anhydride, unsaturated carboxylic acid halide, Examples thereof include unsaturated carboxylic acid amides, unsaturated carboxylic acid imides, and ester compounds of unsaturated carboxylic acids.

  More specifically, examples of the unsaturated carboxylic acid derivatives include maleic anhydride, citraconic anhydride, malenyl chloride, maleimide, monomethyl maleate, dimethyl maleate, glycidyl maleate and the like.

  Among these modifiers, α, β-unsaturated dicarboxylic acids and α, β-unsaturated dicarboxylic acid anhydrides such as maleic acid, nadic acid and anhydrides of these acids are preferably used. These modifiers can also be used in combination of 2 or more types.

  Next, the thickness and the layer configuration of the laminate in the present invention will be described. The present invention is a polishing jig comprising a laminate having a thermosetting resin layer and a thermoplastic resin layer, wherein the thermosetting resin layer is disposed on both surfaces of the laminate. It is

  The total thickness of the laminate is preferably 100 to 5000 μm. If the total thickness is less than 100 μm, the strength and durability of the polishing jig may be reduced. The total thickness is more preferably 200 μm or more. On the other hand, if the total thickness exceeds 5000 μm, the manufacturing cost may increase. The total thickness is more preferably 3000 μm or less. Here, a method of thickening the thermosetting resin layer and / or the thermoplastic resin layer may be mentioned as a method of thickening the total thickness of the laminate. However, from the viewpoint of production cost, it is preferable to make the thermoplastic resin layer thicker than to make the thermosetting resin layer thicker.

  Regarding the relationship between the total thickness of the thermosetting resin layer and the total thickness of the thermoplastic resin layer, it is preferable that the total thickness of the thermoplastic resin layer is larger from the viewpoint of preventing the falling of fibers from the cut surface. On the other hand, from the viewpoint of the strength of the polishing jig, it is preferable that the total thickness of the thermosetting resin layer be larger. From the viewpoint of these balances, in the laminate, the total thickness of the thermoplastic resin layer is preferably 0.2 times or more of the total thickness of the thermosetting resin layer, and more preferably 0.4 times or more Preferably, it is more preferably 0.6 times or more. The total thickness of the thermoplastic resin layer is preferably 10 times or less of the total thickness of the thermosetting resin layer, more preferably 6 times or less, still more preferably 4 times or less, and 3 times or less Is particularly preferred.

The layer configuration of the laminate in the present invention is not particularly limited as long as the thermosetting resin layers are disposed on both surfaces of the laminate, but, for example, a three-layer structure, a five-layer structure, and a seven-layer structure shown below Body etc. are mentioned. Here, TS represents a thermosetting resin layer, and TP represents a thermoplastic resin layer.
Three-layer structure: TS / TP / TS
Five-layer structure: TS / TP / TS / TP / TS
7-layer structure: TS / TP / TS / TP / TS / TP / TS

  Among the above, the laminate is preferably a three-layer structure (TS / TP / TS) having a thermosetting resin layer, a thermoplastic resin layer and a thermosetting resin layer in this order. Here, when an external force for bending the polishing jig is applied, a compressive stress and a tensile stress are respectively generated in the thermosetting resin layers on both sides as a force repulsive to the external force. By setting the layer in which the compressive stress and the tensile stress are generated as a thermosetting resin layer containing an organic fiber aggregate having high flexural modulus and flexural strength, the flexural modulus and the flexural strength of the polishing jig are improved.

  In the case where the laminate is a three-layer structure, the thickness of the thermosetting resin layer on the surface is preferably 0.05 times or more that of the central thermoplastic resin layer, preferably 0.1 times or more. Is more preferable, and 0.2 or more times is more preferable. By thickening the thickness of the central thermoplastic resin layer with respect to the thickness of the thermosetting resin layer on the surface, the thermosetting resin layer is disposed further outside. By arranging the thermosetting resin layer further to the outside, expansion and contraction of the surface of the polishing jig by bending can be effectively restrained by the thermosetting resin layer having a high elastic modulus, and therefore the bending elastic modulus and the bending strength of the polishing jig are It improves more. The thickness of the thermosetting resin layer on the surface is preferably 5 times or less of that of the central thermoplastic resin layer, more preferably 3 times or less, and still more preferably 2 times or less. It is particularly preferred that it is 5 times or less.

  The method for producing the polishing jig of the present invention is not particularly limited, but the first step of obtaining a prepreg by impregnating an organic fiber aggregate with a thermosetting resin, and the prepreg obtained in the first step and a thermoplastic resin Forming a laminated sheet so that the prepreg is on both surfaces and heating and pressing to form a laminated plate, and a through hole for holding a plate-like body to be polished is formed in the laminated plate A manufacturing method comprising the third step is preferable.

  First, in the first step, an aggregate of organic fibers is impregnated with a thermosetting resin to obtain a prepreg. As the aggregate of organic fibers, those described above can be used.

  At this time, it is preferable to use an organic fiber assembly having a thickness of 10 to 300 μm from the viewpoint of the strength and durability of the obtained polishing jig. The thickness of the assembly is more preferably 20 μm or more. On the other hand, if the thickness of the assembly exceeds 300 μm, the production of the assembly may be difficult, and the flexibility may be insufficient to produce a prepreg. The thickness of the assembly is more preferably 200 μm or less.

  The method for impregnating the organic fiber aggregate with a thermosetting resin to produce a prepreg is not particularly limited. The method of immersing an organic fiber aggregate in the thermosetting resin in a container, the method of apply | coating a thermosetting resin on the surface of an organic fiber aggregate, etc. are illustrated. At this time, it is preferable to use a solution obtained by dissolving a thermosetting resin in a solvent. The immersion time and the amount of application can be appropriately set so that the thermosetting resin layer has a desired thickness. Among them, it is preferable to immerse the organic fiber assembly in the thermosetting resin in the container. It is preferable that the thermosetting resin is in a semi-cured state up to the second step in order to laminate the prepreg and the sheet made of a thermoplastic resin in the next second step and heat and press the sheet to form a laminate.

  Next, in a second step, the prepreg obtained in the first step and a sheet made of a thermoplastic resin are superimposed on each other such that the prepregs are on both surfaces, and heat and pressure are applied to obtain a laminate. At this time, the number of prepregs and sheets to be used is not particularly limited. For example, in the case of obtaining the above-described three-layer structure, the prepregs may be disposed on both surfaces, and the number of sheets in the center is not particularly limited.

  In the manufacturing method of the present invention, the total thickness of the laminate can be arbitrarily changed by changing the thickness and the number of sheets made of the thermoplastic resin to be used. Since the sheet is often cheaper than the prepreg, the manufacturing method of the present invention is highly advantageous in terms of cost.

  Next, in the third step, through holes for holding the plate-like body to be polished are formed in the laminate. A polishing jig can be obtained by forming one or more holes in the laminate. The formation method is not particularly limited, and the through holes may be formed in the laminate using a router machine or the like. At this time, the laminated plate may be formed into a predetermined size or shape, or a drive gear may be formed as needed.

  The plate-like body is held by the polishing jig of the present invention to polish the plate-like body. The polishing jig of the present invention has high flexural modulus and flexural strength. Therefore, it is possible to prevent the falling off of the foreign matter while preventing the breakage of the polishing jig. Moreover, it can suppress that a foreign material adheres to a plate-like object, or a scratch generate | occur | produces. The plate-like body to be polished is not particularly limited, and examples thereof include a semiconductor wafer, an aluminum disk or glass disk for a hard disk, a glass substrate for liquid crystal display, and the like.

[material]
(Polyarylate fiber woven fabric (WF))
The polyarylate fiber woven fabric is “Bectran HT-0235” (weight: 62 g / m ² , thickness: 116 μm) manufactured by Kuraray Co., Ltd. In the following description, this polyarylate fiber woven fabric may be abbreviated as "WF".

(Epoxy-impregnated woven fabric (WP))
A bisphenol A type epoxy resin as a thermosetting resin and an amine compound as a curing agent were added to a mixed solvent of toluene, methanol and methyl cellosolve and dissolved to prepare a varnish.

  The above varnish was placed in a container, and the polyarylate fiber woven fabric “Bectran HT-0235” was dipped in the varnish in the container. Thereafter, the polyarylate fiber woven fabric was dried to partially cure the varnish to obtain an epoxy-impregnated woven fabric (prepreg). The epoxy resin content (Rc) in the obtained epoxy-impregnated woven fabric was 58% by mass. Hereinafter, this epoxy-impregnated woven fabric may be abbreviated as "WP".

(Non-woven fabric (NF))
The non-woven fabric is the non-woven fabric “Beculus MBBK150FZSO” (weight: 150 g / m ² , thickness: 323 μm, density: 0.46 g / cm ³ ) manufactured by Kuraray Kura Flex Co., Ltd. This "Becrus MBBK150FZSO" is a non-woven fabric manufactured by a melt blow molding method, obtained by thermocompression bonding, and does not contain an adhesive. In the following description, this non-woven fabric may be abbreviated as "NF".

(Epoxy-impregnated nonwoven fabric (NP))
A bisphenol A type epoxy resin as a thermosetting resin and an amine compound as a curing agent were added to a mixed solvent of toluene, methanol and methyl cellosolve and dissolved to prepare a varnish.

  The above varnish was placed in a container, and the non-woven fabric "BECLUS MBBK150FZSO" was dipped in the varnish in the container. Thereafter, the non-woven fabric was dried to partially cure the varnish to obtain an epoxy-impregnated non-woven fabric. Hereinafter, this epoxy-impregnated nonwoven fabric may be abbreviated as "NP".

(Resin sheet (S))
100 parts by mass of the following cyclic olefin polymer (a), 11 parts by mass of ethylene / propylene random copolymer (b), 0.022 parts by mass of a radical initiator (c) and 0.022 parts by mass of a polyfunctional compound (d) The mixture was melt-kneaded with an extruder to obtain a resin composition. The said resin composition is marketed by Fuji Bakelite Co., Ltd. under the name of "FB-0422X1".

・ Cyclic olefin polymer (a)
Ethylene and tetracyclo [4.4.0.1 ^2,5 .1 ^7,10] -3- dodecene (hereinafter sometimes abbreviated as "TCD-3") and random copolymer (ethylene -TCD-3 random copolymer) . ^The intrinsic viscosity [.eta.] Measured in decalin at 135.degree. C. is 77.8 mass% (38 mol%), the ethylene content is 22.2 mass% (62 mol%), and the TCD-3 content measured by .sup.13 C-NMR The glass transition temperature (Tg) is 0.60 dl / g and is 105 ° C. The MFR (measured at 230 ° C. and a 2.16 kg load based on ASTM D1238) is 8.2 g / 10 min. The structural formula of TCD-3 is such that n = 0, m = 1 and R ⁷ , R ⁸ , R ⁹ , R ¹⁰ , R ¹¹ , R ¹² , R ¹³ , R ¹⁴ , R ¹⁵ , in the above formula [I]. In the case where R ¹⁶ , R ¹⁷ and R ¹⁸ are hydrogen atoms.

・ Soft copolymer (b)
Mitsui Chemical Co., Ltd. ethylene-propylene random copolymer "P-0880". The ethylene content is 80 mol%, the intrinsic viscosity [η] is 2.5 dl / g, and the glass transition temperature (Tg) is −54 ° C. MFR (measured at 230 ° C. and 2.16 kg load based on ASTM D1238) 0.4 g / 10 min, density 0.867 g / cm ³ , crystallinity about 10% measured by X-ray diffraction method is there.

・ Radical initiator (c)
Nippon Oil and Fats Co., Ltd. "Perhexin 25B". 2,5-Dimethyl-2,5-bis (t-butylperoxy) hexine-3 is a main component (90% or more). The one-minute half-life temperature is 194.3 ° C.

・ Multifunctional compound (d)
Divinylbenzene

  Then, the above resin composition, 2,5-dimethyl-2,5-di- (t-butylperoxin) -hexyne-3, and maleic anhydride were mixed to obtain a mixture. The content of the above resin composition in this mixture is 98.5% by mass, and the content of 2,5-dimethyl-2,5-di- (t-butylperoxine) is 0.5% by mass. The content of maleic anhydride was 1.0% by mass. The mixture was charged into a twin-screw extruder ("TEX30.alpha." Manufactured by Nippon Steel Co., Ltd.), melt-kneaded and reacted, and then pelletized to obtain pellets. 2, 5-Dimethyl-2, 5-di- (t-butylperoxin) -hexyne-3 was "Perhexin 25B" manufactured by NOF Corporation.

  The obtained pellet was introduced into an extruder for film formation, and resin sheets having a thickness of 1.0 mm, 0.55 mm, 0.50 mm, 0.35 mm and 0.11 mm were produced. Hereinafter, a resin sheet may be abbreviated as "S". Moreover, the numerical value described with the symbol S shows the thickness (mm) of the resin sheet.

[Evaluation]
(Evaluation of bending characteristics)
The bending characteristics of the obtained laminate were measured in accordance with JIS K7171. Specifically, the obtained laminate is cut into 1.0 mm × 25 mm × 20 mm (thickness × width × length) using “AG-10TB” manufactured by Shimadzu Corporation, and 10 test pieces are obtained. I got Then, using these test pieces, the flexural strength (MPa) and the flexural modulus (MPa) are measured at 25 ° C. at a test speed of 1 mm / min and the distance between supporting points of 16 mm, and the average value of 10 pieces is determined. The The bending characteristics in the weave direction of the woven fabric and the bending characteristics in the bias direction were measured for laminates prepared using prepreg or polyarylate fiber woven fabric. Moreover, about the laminated board produced using the nonwoven fabric, the bending characteristic of a flow direction and the bending characteristic of the direction perpendicular | vertical to the direction were each measured. Here, the flow direction of the non-woven fabric refers to the flow direction (Machine Direction: MD) of equipment when manufacturing the non-woven fabric.

Example 1
Between the press plates, epoxy impregnated woven fabric (WP), epoxy impregnated woven fabric (WP), resin sheet (S _0.50 ), epoxy impregnated woven fabric (WP), epoxy impregnated woven fabric (WP) in this order I piled up. That is, the sheet sandwiched between the press plates is, in order from the top, WP / WP / S _0.50 / WP / WP. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 5 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 1.5 MPa, the press plate was heated while maintaining this press pressure. After confirming that the temperature of the press plate reached 130 ° C., it was pressed at that press pressure and temperature for 1 hour. Thereafter, the press pressure was set to 7.5 MPa and the press plate was cooled with cooling water.

The cross section of the obtained laminate was observed using a laser microscope. FIG. 1 is a cross-sectional image of a laminate. In Figure 1, WP _a and WP _b are both indicate the thermosetting resin layer two epoxy impregnated fabric (WP) is bonded, S _a represents a thermoplastic resin layer composed of a resin sheet. As shown in FIG. 1, the resulting laminate in which a multilayer structure _{(WP a / S a / WP} b) composed of a thermoplastic resin layer made of a thermosetting resin layer and a resin sheet made of a prepreg there were.

When the thickness of the laminated board was measured, the thickness was 1023 μm. The thickness of each layer is as follows.
WP _a : 284 μm
S _a : 494 μm
WP _b : 245 μm

  The flexural properties of the resulting laminates were measured according to the method described above. The results are shown in Table 1.

  Moreover, the obtained laminated board was processed using the router machine, and the grinding | polishing jig was produced. A plan view of the obtained polishing jig 1 is shown in FIG. As shown in FIG. 2, the polishing jig 1 has a driving gear 2 on the outer periphery, and has five through holes 3 for holding a plate-like body to be polished.

  Then, the obtained polishing jig was mounted on a polishing apparatus, the plate-like body was held by the through holes, and the plate-like body was polished for 6 minutes by driving the polishing jig horizontally. The plate-like body to be polished in this test is an aluminum substrate having a thickness of 1.27 mm. The abrasive used in this test was "Disc Light" manufactured by Fujimi Incorporated.

  Using a wafer inspection apparatus “Candela 7100” manufactured by KLA-Tencor Corporation, scratches present on the polished surface of the aluminum substrate after polishing were confirmed. As a result, no scratch was observed on the polished surface of the aluminum substrate. Further, using the above-described apparatus, it was confirmed whether foreign matter was attached to the polished surface of the aluminum substrate after polishing. As a result, only a few foreign particles were found on the polished surface of the aluminum substrate.

Comparative Example 1
In the press plate, resin sheet ( _S0.11 ), polyarylate fiber woven fabric (WF), resin sheet ( _S0.11 ), polyarylate fiber woven fabric (WF), resin sheet (S _0.35 ) , Polyarylate fiber woven fabric (WF), resin sheet (S _0.11 ), polyarylate fiber woven fabric (WF), and resin sheet (S _0.11 ). That is, the sheets sandwiched between the press plates are, in order from the top, S _0.11 / WF / S _0.11 / WF / S _0.35 / WF / S _0.11 / WF / S _0.11 is there. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 5 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 3.5 MPa, the press plate was heated while maintaining this press pressure. Immediately after confirming that the temperature of the press plate reached 180 ° C., the press pressure was set to 7.5 MPa and the press plate was cooled with cooling water. The pressure was stopped when the temperature of the press plate returned to room temperature, and the laminate was removed from the press plate.

  The cross section of the obtained laminate was observed using a laser microscope. FIG. 3 is a cross-sectional image of a laminate. As shown in FIG. 3, the polyarylate fiber woven fabric (WF) was embedded in a sheet made of a thermoplastic resin. The thickness of the laminate was 876 μm. Moreover, according to the method mentioned above, the bending characteristic of the obtained laminated board was measured. The results are shown in Table 1.

Comparative example 2
The resin plate (S _0.11 ), nonwoven fabric (NF), nonwoven fabric (NF), resin sheet (S _0.55 ), nonwoven fabric (NF), nonwoven fabric (NF), resin sheet (S _{0. 11} ) repeated. That is, the sheets sandwiched between the press plates are S _0.11 / NF / NF / S _0.55 / NF / NF / S _0.11 in order from the top. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 5 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 3.5 MPa, the press plate was heated while maintaining this press pressure. Immediately after confirming that the temperature of the press plate reached 180 ° C., the press pressure was set to 7.5 MPa and the press plate was cooled with cooling water. The pressure was stopped when the temperature of the press plate returned to room temperature, and the laminate was removed from the press plate.

The cross section of the obtained laminate was observed using a laser microscope. FIG. 4 is a cross-sectional image of the polishing jig. In FIG. 4, S _b , S _c and S _d indicate layers formed of resin sheets, and F _a and F _b indicate layers formed of two non-woven fabrics. As shown in FIG. 4, the obtained laminate has a multilayer structure (S _b / NF _a / S _c / NF _b / S _d ) in which a base material layer and a resin layer are laminated.

When the thickness of the laminated board was measured, the thickness was 965 μm. The thickness of each layer is as follows.
S _b : 49 μm
NF _a : 196 μm
S _c: 448μm
NF _b : 206 μm
S _d : 66 μm

  Moreover, according to the method mentioned above, the bending characteristic of the obtained laminated board was measured. The results are shown in Table 1.

Comparative example 3
Between the press plates, eight sheets of epoxy impregnated woven fabric (WP) were stacked. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 5 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 1.5 MPa, the press plate was heated while maintaining this press pressure. After confirming that the temperature of the press plate reached 130 ° C., it was pressed at that press pressure and temperature for 1 hour. Thereafter, the press pressure was set to 7.5 MPa and the press plate was cooled with cooling water.

  The cross section of the obtained laminate was observed using a laser microscope. FIG. 5 is a cross-sectional image of a laminate. As shown in FIG. 5, in the obtained laminate, the woven fabric was buried in the thermosetting resin layer. The thickness of the laminate was 1051 μm. Moreover, according to the method mentioned above, the bending characteristic of the obtained laminated board was measured. The results are shown in Table 1.

Comparative example 4
Between the press plates, _one resin sheet (S ₁ ) was placed. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 15 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 3.5 MPa, the press plate was heated while maintaining this press pressure. After confirming that the temperature of the press plate reached 120 ° C., it was pressed at that press pressure and temperature for 1 hour. Thereafter, the press pressure was set to 7.5 MPa and the press plate was cooled with cooling water. The bending properties of the obtained plate were also measured according to the method described above. The results are shown in Table 1.

Comparative example 5
Between the press plates, eight sheets of epoxy impregnated non-woven fabric (NP) were stacked. Then, release films were disposed on the top and bottom surfaces. This was made into one set, and 5 sets were piled and pressed. Pressurization was started, and after confirming that the press pressure had reached 2.5 MPa, the press plate was heated while maintaining this press pressure. After confirming that the temperature of the press plate reached 130 ° C., it was pressed at that press pressure and temperature for 1 hour. Thereafter, the press pressure was set to 2.5 MPa and the press plate was cooled with cooling water. Moreover, according to the method mentioned above, the bending characteristic of the obtained laminated board was measured. The results are shown in Table 1.

1 polishing jig 2 gear 3 through hole

Claims (11)

A polishing jig comprising a laminate having a thermosetting resin layer and a thermoplastic resin layer;
The thermosetting resin layer contains an organic fiber assembly,
A polishing jig characterized in that the thermoplastic resin layer does not contain an organic fiber aggregate, and the thermosetting resin layer is disposed on both surfaces of the laminate.   The polishing jig according to claim 1, wherein the laminate is a three-layer structure including the thermosetting resin layer, the thermoplastic resin layer, and the thermosetting resin layer in this order.   The polishing jig according to claim 1, wherein the thermosetting resin layer contains an epoxy resin or a phenol resin.   The polishing jig according to any one of claims 1 to 3, wherein the thermoplastic resin layer contains at least one polymer selected from the group consisting of polyolefin, polyester and poly (meth) acrylate.   The polishing jig according to any one of claims 1 to 4, wherein the fibers constituting the organic fiber assembly are at least one fiber selected from the group consisting of polyarylate fibers, aramid fibers and polyphenylene sulfide fibers.   The polishing jig according to any one of claims 1 to 5, wherein the organic fiber assembly is a woven fabric or a knitted fabric.   The total thickness of the said laminated board is 100-5000 micrometers, The grinding | polishing jig | tool in any one of Claims 1-6.   The polishing jig according to any one of claims 1 to 7, wherein in the laminate, a total thickness of the thermoplastic resin layer is 0.2 to 10 times a total thickness of the thermosetting resin layer.   The said laminated board is a three-layer structure, and the thickness of the said thermosetting resin layer of the surface is 0.05-5 times of the said thermoplastic resin layer of all center, It is any one of Claims 1-8. Polishing jig. A method of manufacturing a polishing jig according to any one of claims 1 to 9;
A first step of impregnating the organic fiber assembly with a thermosetting resin to obtain a prepreg;
A second step of obtaining a laminate by laminating and heating and pressing the prepreg obtained in the first step and a sheet made of a thermoplastic resin so that the prepreg is on both surfaces;
And a third step of forming a through hole for holding a plate-like body to be polished in the laminated plate.   The polishing method which hold | maintains a plate-like body with the polishing jig in any one of Claims 1-9, and grind | polishes this plate-like body.

Images