JP2007190613A - Polishing film and manufacturing method thereof - Google Patents

Polishing film and manufacturing method thereof Download PDF

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Publication number
JP2007190613A
JP2007190613A JP2004032287A JP2004032287A JP2007190613A JP 2007190613 A JP2007190613 A JP 2007190613A JP 2004032287 A JP2004032287 A JP 2004032287A JP 2004032287 A JP2004032287 A JP 2004032287A JP 2007190613 A JP2007190613 A JP 2007190613A
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polishing
film
component
epoxy
polishing film
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Michihiro Ishii
倫裕 石井
Yoshinori Fujiwara
良則 藤原
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Bando Chemical Industries Ltd
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Bando Chemical Industries Ltd
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Priority to JP2004032287A priority Critical patent/JP2007190613A/en
Priority to PCT/JP2004/019038 priority patent/WO2005075148A1/en
Priority to TW93141465A priority patent/TW200537142A/en
Publication of JP2007190613A publication Critical patent/JP2007190613A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28Resins or natural or synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D11/00Constructional features of flexible abrasive materials; Special features in the manufacture of such materials

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Laminated Bodies (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a polishing film and a manufacturing method for it, having good productivity and polishing durability, and heightening the polishing rate. <P>SOLUTION: This polishing film includes a polyester base film and a polishing layer formed on the polyester base film and containing abrasive grain and a binder, wherein the binder is epoxy urethane obtained by reacting and curing a polyol component, an epoxy component and a crosslinking agent. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、光コネクタフェルールや高容量ハードディスク等の精密研磨に使用される研磨フィルム及びその製造方法に関し、特に光コネクタフェルールの接合端面の研磨の最終仕上げに最適な研磨フィルム及びその製造方法に関する。   The present invention relates to a polishing film used for precision polishing of optical connector ferrules, high-capacity hard disks and the like, and a method for manufacturing the same, and more particularly to a polishing film optimal for final finishing of a joining end surface of an optical connector ferrule and a method for manufacturing the same.

従来より、光ファイバー通信網において、光ファイバーの接続には取り外しの容易な光コネクタが広く使用されている。接続は、光ファイバーと該光ファイバーを被覆する被覆部(フェルール)からなる光コネクタフェルールの端面同士を直接突き合わせ(フィジカルコンタクト)て行われるため、接続部の光学特性(減衰等)は、光コネクタフェルール端面の研磨加工性状と精度に依存する。光コネクタフェルールは、細長筒状のジルコニア製フェルールの軸中心の微小貫通孔に光ファイバーが挿入され接着一体化されたものであり、半球状に精密研磨されたコネクタ端面同士を圧接して中心の光ファイバーを接続する。この中心の光ファイバー部が凹凸を有すると隙間が形成された状態で接続され、減衰が多くなり致命的な欠陥となる。
光コネクタフェルール端面の研磨加工は、粗仕上、中仕上、最終仕上との複数の研磨工程によって行われるが、最終仕上工程においては、ポリエステル基材上にシリカ砥粒がバインダー樹脂で固定された研磨フィルムを、研磨機の研磨定盤上に研磨パッドを介して裁置し、研磨フィルム表面に中仕上げされた光コネクタフェルール端面を押付けながら研磨定盤を回転させると同時に公転させることにより、中仕上げされた光コネクタフェルール端面を、所定の寸法、面粗さに研磨する。
この最終仕上などのように、精密研磨に好適な研磨フィルムとしては、シリコーン樹脂をバインダーとして使用したものが知られている(下記特許文献1、特許文献2、特許文献3、特許文献4、特許文献5)。
しかしながら、これらの先行文献に記載された研磨フィルムは、砥粒の固定が砥粒とバインダーたるシリコン樹脂との親和性のみに依存しており、研磨中に砥粒が脱落しやすいため(特に、砥粒濃度が75容量%程度を超えた場合等)、研磨速度に限界がある。また、バインダー自身が対摩耗性に優れた材料でないため研磨耐久性において不十分である。更に、ポリエステル基材と研磨層の接着部の応力緩和のため2週間程度の熟成を要し生産性の点でも問題がある。
特開平08−336758号公報 特開平10−071572号公報 特開平11−333731号公報 特開平11−333732号公報 特開2002−154061号公報
2. Description of the Related Art Conventionally, in an optical fiber communication network, an optical connector that can be easily detached has been widely used to connect an optical fiber. The connection is made by directly abutting (physical contact) the end faces of the optical connector ferrule composed of an optical fiber and a covering portion (ferrule) that covers the optical fiber. Depends on the polishing properties and accuracy. An optical connector ferrule is an optical fiber inserted into a minute through-hole at the center of an elongated cylindrical ferrule made of zirconia and bonded and integrated. Connect. If the central optical fiber part has irregularities, it is connected in a state where a gap is formed, resulting in increased attenuation and a fatal defect.
The polishing process of the optical connector ferrule end face is performed by a plurality of polishing processes including rough finishing, intermediate finishing, and final finishing. In the final finishing process, the silica abrasive grains are fixed on a polyester base material with a binder resin. The film is placed on the polishing platen of the polishing machine via a polishing pad, and the polishing platen is rotated and revolved at the same time while rotating the polishing platen while pressing the end face of the optical connector ferrule on the polishing film surface. The optical connector ferrule end face is polished to a predetermined size and surface roughness.
As this final finish and the like, as a polishing film suitable for precision polishing, those using a silicone resin as a binder are known (Patent Document 1, Patent Document 2, Patent Document 3, Patent Document 4, Patent Reference 5).
However, in the polishing films described in these prior documents, the fixing of the abrasive grains depends only on the affinity between the abrasive grains and the silicon resin as the binder, and the abrasive grains are likely to fall off during polishing (particularly, If the abrasive concentration exceeds about 75% by volume), the polishing rate is limited. Further, since the binder itself is not a material with excellent wear resistance, the polishing durability is insufficient. Furthermore, aging for about 2 weeks is required to relieve stress at the bonded portion between the polyester substrate and the polishing layer, and there is a problem in terms of productivity.
Japanese Patent Laid-Open No. 08-336758 JP-A-10-071572 Japanese Patent Laid-Open No. 11-333731 JP 11-333732 A JP 2002-154061 A

そこで、本発明は、上記従来の問題点に鑑み、生産性、研磨耐久性が良好であり、研磨速度を高めうる研磨フィルム及びその製造方法を提供するを課題とする。   Therefore, in view of the above-described conventional problems, an object of the present invention is to provide a polishing film that has good productivity and polishing durability and can increase the polishing rate, and a method for manufacturing the same.

上記課題を解決すべく、本発明は、ポリエステル基材フィルム上に、砥粒とバインダーとを備えてなる研磨層が設けられてなる研磨フィルムであって、
前記バインダーが、ポリオール成分とエポキシ成分と架橋剤を反応硬化させてなるエポキシウレタンであることを特徴とする研磨フィルムを提供する。
本発明の研磨フィルムは、バインダーとしてエポキシウレタンが採用されてなるので、ウレタンの耐摩耗性、接着性と、エポキシの接着性、高剛性との合体によって、バインダー自身の耐摩耗性、砥粒及びポリエステル基材との接着性が向上することから、研磨耐久性が向上すると共に、砥粒が強固に固定されて、研磨速度を高めうるものとなる。
また、熟成に長時間をかけなくともポリエステル基材との接着性が良好であることから、生産性も良好である。
更に、砥粒及びポリエステル基材との接着性の向上により、例えば、砥粒の含有率を75容量以上90容量程度まで上げることもでき、斯かる含有率とした場合には、より研磨速度を高めうる。
尚、エポキシウレタンの構造は、エポキシ成分とイソシアネートとが反応したオキサゾリンと、ポリオール成分とイソシアネートとが反応したポリウレタンと、過剰なイソシアネートが3量化したイソシアヌレートとが混在しているものと推定される。
In order to solve the above problems, the present invention is a polishing film comprising a polyester base film provided with a polishing layer comprising abrasive grains and a binder,
A polishing film is provided in which the binder is an epoxy urethane obtained by reaction-curing a polyol component, an epoxy component, and a crosslinking agent.
Since the polishing film of the present invention employs epoxy urethane as a binder, the wear resistance of the binder itself, abrasive grains and the combination of urethane abrasion resistance and adhesion, epoxy adhesion, and high rigidity. Since the adhesiveness with the polyester base material is improved, the polishing durability is improved and the abrasive grains are firmly fixed to increase the polishing rate.
Moreover, productivity is also good because the adhesiveness with the polyester base material is good without taking a long time for aging.
Furthermore, by improving the adhesiveness between the abrasive grains and the polyester base material, for example, the content of the abrasive grains can be increased to 75 to 90 volumes. Can be increased.
The structure of epoxy urethane is presumed to be a mixture of oxazoline in which an epoxy component and isocyanate are reacted, polyurethane in which a polyol component and isocyanate are reacted, and isocyanurate in which excess isocyanate is trimerized. .

また、本発明は、ポリエステル基材の片面に砥粒とバインダー成分とを含む塗布液を塗布し乾燥させて研磨層を形成する研磨フィルムの製造方法であって、ポリエステル基材に塗布液を塗布した後、該ポリエステル基材の非塗布面側に加熱体を接触させ、非塗布面側から加熱して乾燥させることを特徴とする研磨フィルムの製造方法を提供する。
斯かる方法によれば、上記利点を有する研磨フィルムを製造することができる。
尚、本発明に於いて、バインダー成分を含むとは、バイダーたる樹脂を含む場合及びバインダーたる樹脂を構成するモノマー等の原料を含む場合の双方を意味する。
The present invention also relates to a method for producing a polishing film in which a coating liquid containing abrasive grains and a binder component is applied to one side of a polyester substrate and dried to form a polishing layer, and the coating liquid is applied to a polyester substrate. Then, a heating body is brought into contact with the non-coated surface side of the polyester base material, and the method for producing an abrasive film is characterized by heating from the non-coated surface side and drying.
According to such a method, a polishing film having the above advantages can be produced.
In the present invention, the phrase “containing a binder component” means both a case where a binder resin is included and a case where a raw material such as a monomer constituting the binder resin is included.

以上のように、本発明の研磨フィルムは、生産性、研磨耐久性が良好であり、研磨速度を高めうる。   As described above, the polishing film of the present invention has good productivity and polishing durability, and can increase the polishing rate.

以下、本発明の好ましい形態について図面を参照しつつ説明する。
図1は、一実施形態の研磨フィルムを示す概略断面図である。図2は、断面及び上面を示す概略図である。
本実施形態の研磨フィルム1は、例えば、図1に示されるように、ポリエステル基材フィルム2上に、砥粒3aとバインダー3bとを備えてなる研磨層3が設けられて構成され、前記バインダー3bとして、ポリオール成分とエポキシ成分と架橋剤とを反応硬化させてなるエポキシウレタンが用いられてなる。
前記エポキシウレタンは、高硬度の弾性体の硬度表示に用いられるショアーD硬度(JIS)で20〜90が好ましく、40〜75が特に好ましい。ショアーD硬度が20〜90であれば、上記研磨耐久性と研磨速度の向上を高いレベルで図りうる。ショアーD硬度が20未満になると、柔軟すぎて研磨速度の高いレベルでの向上を図れない虞があり、更に、比較的耐久性が劣る傾向にある。また、90を超えると被研磨面にキズを生じる恐れがある。
Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings.
FIG. 1 is a schematic cross-sectional view showing an abrasive film according to one embodiment. FIG. 2 is a schematic view showing a cross section and a top surface.
For example, as shown in FIG. 1, the polishing film 1 of the present embodiment is formed by providing a polishing layer 3 including abrasive grains 3 a and a binder 3 b on a polyester base film 2, and the binder As 3b, an epoxy urethane obtained by reaction-curing a polyol component, an epoxy component, and a crosslinking agent is used.
The epoxy urethane is preferably from 20 to 90, particularly preferably from 40 to 75, in Shore D hardness (JIS) used for displaying the hardness of a high-hardness elastic body. When the Shore D hardness is 20 to 90, the polishing durability and the polishing rate can be improved at a high level. When the Shore D hardness is less than 20, there is a possibility that improvement at a high polishing rate cannot be achieved due to being too flexible, and further, durability tends to be relatively inferior. On the other hand, if it exceeds 90, the surface to be polished may be scratched.

前記ポリオール成分としては、ポリエチレンアジーペート、ポリカプロラクトン等のエステル型ポリオールや、ポリオキシプロピレングリコール(PPG)、ポリ(オキシテトラメチレン)グリコール等のエーテル型ポリオール等を挙げることができる。中でも、耐研磨液よりポリオキシプロピレングリコール(PPG)が好ましく、特に、官能基数が3近辺で分子量(数平均)が3000〜8000のPPGで、エチレンオキサイドをブロック状に付加した活性化PPGが、砥粒の保持やポリエステル基との接着に優れ且つ耐久性に優れるので好ましい。
尚、ポリオール成分の分子量は、GPC法(Gel Permeation Chromatography)で以下の条件で測定される。
装置:ウオーターズ社製2690型
カラム:東ソー社製 TSKgel MultiporeHXL−M 2本
東ソー社製 TSKgel G2000HHR 1本
標準物質:スチレン
温度:30℃
Examples of the polyol component include ester type polyols such as polyethylene adipate and polycaprolactone, and ether type polyols such as polyoxypropylene glycol (PPG) and poly (oxytetramethylene) glycol. Among them, polyoxypropylene glycol (PPG) is preferable to the anti-polishing liquid, and in particular, an activated PPG in which ethylene oxide is added in a block form with PPG having a functional group number of 3 and a molecular weight (number average) of 3000 to 8000, This is preferable because it is excellent in holding of abrasive grains and adhesion to a polyester group and is excellent in durability.
The molecular weight of the polyol component is measured by the GPC method (Gel Permeation Chromatography) under the following conditions.
Apparatus: 2690 type manufactured by Waters Co., Ltd. Column: TSKgel Multipore HXL-M 2 manufactured by Tosoh Corporation
1 TSKgel G2000HHR manufactured by Tosoh Corporation Standard material: Styrene Temperature: 30 ° C

前記エポキシ成分としては、ビスフェノールA−グリシジルエーテル型やポリオールグリシジルエーテル型を挙げることができ、汎用性、砥粒や基材との接着の点で、ビスフェノールA−グリシジルエーテルが好ましく用いられる。   Examples of the epoxy component include a bisphenol A-glycidyl ether type and a polyol glycidyl ether type, and bisphenol A-glycidyl ether is preferably used in terms of versatility and adhesion to abrasive grains and a substrate.

前記架橋剤としては、トリレンジイソシアネート(TDI)、ジフェニルメタンジイソシアネート(MDI)、ナフタレンジイソシアネート(NDI)、イソフォロンジイソシアネート(IPDI)等のイソシアネートを挙げることができ、反応性に富み、取り扱いが容易な点でジフェニルメタンジイソシアネート(MDI)が好ましい。フェニル基におけるイソシアネート基の位置が2,4’−のものと4,4’−のものとを80/20〜20/80(2,4’−/4,4’−)の重量比で混合した混合物が、形成されるエポキシウレタンの耐久性が増すため好ましい。液状で取り扱いが容易で、得られるエポキシウレタンの耐久性が高いという点で、2,4’−/4,4’−(重量比)は、60/40〜40/60がより好ましい。   Examples of the crosslinking agent include isocyanates such as tolylene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), naphthalene diisocyanate (NDI), and isophorone diisocyanate (IPDI), which are rich in reactivity and easy to handle. Diphenylmethane diisocyanate (MDI) is preferred. Mixtures of 2,4'- and 4,4'-isocyanate groups in the phenyl group in a weight ratio of 80/20 to 20/80 (2,4 '-/ 4,4'-) The resulting mixture is preferred because the durability of the epoxy urethane formed is increased. 60/40 to 40/60 is more preferable for 2,4 '-/ 4,4'- (weight ratio) in that it is liquid and easy to handle, and the resulting epoxy urethane has high durability.

前記ポリオール成分、エポキシ成分、硬化剤の好ましい組み合わせとしては、ポリオール成分が官能基数3で分子量4800のエチレンオキサイド付加PPGであり、エポキシ成分がビスフェノールA型エポキシ樹脂であり、硬化剤が、2,4’−/4,4’−(重量比)が47/53のMDI混合物である。   As a preferable combination of the polyol component, the epoxy component, and the curing agent, the polyol component is an ethylene oxide-added PPG having 3 functional groups and a molecular weight of 4800, the epoxy component is a bisphenol A type epoxy resin, and the curing agent is 2,4. '-/ 4,4'- (weight ratio) is a 47/53 MDI mixture.

前記架橋剤と反応するエポキシ成分及びポリオール成分の比率は、剛性と柔軟性のバランスより、重量比(エポキシ成分/ポリオール成分)で90/10〜10/90が好ましく、より好ましくは30/70〜70/30である。
エポキシ成分およびポリオール成分の比率が90より大きくなると、エポキシライクになって弾性が無くなったり、ウレタンライクになって砥粒の濃度を上げることが困難となる。
The ratio of the epoxy component that reacts with the crosslinking agent and the polyol component is preferably 90/10 to 10/90, more preferably 30/70 to 90 by weight ratio (epoxy component / polyol component), from the balance of rigidity and flexibility. 70/30.
If the ratio of the epoxy component and the polyol component is greater than 90, it becomes epoxy-like and loses elasticity, or it becomes urethane-like and it becomes difficult to increase the concentration of abrasive grains.

研磨フィルムの研磨層表面は、例えば、図1、2に示されるように、精密仕上の観点からJISB0601に規定する算術平均表面粗さが0.1μm(100nm)以下の平滑な研磨面5と、研磨粉を収容する溝6、特に幾何学模様を成す溝6とを有するものが好ましい。
斯かる構成によれば、研磨面にて極めて精密に、例えば、光コネクタフェルールに要求される半球状端面の表面粗さ4nm以下に研磨仕上げを行うことができると共に、フェルールのジルコニアやファイバー等の研磨粉を溝によって収容することができる。
前記幾何学模様は、直線状の溝の組合せで1辺長さが1μm〜300μmの三〜六角形の形状に形成され、各溝の幅は、0.1μm〜5μmが好ましい。尚、図2に幾何学模様の例を示す。
斯かる構成によれば、被研磨物の研磨粉(屑)を収容して保持できる。
尚、研磨粉は、通常、加工の工程中に研磨液とともに除去される。これによって、研磨粉による研磨能力の低下が抑制される。
The polishing layer surface of the polishing film is, for example, as shown in FIGS. 1 and 2, a smooth polishing surface 5 having an arithmetic average surface roughness of 0.1 μm (100 nm) or less as defined in JIS B0601 from the viewpoint of precision finishing, It is preferable to have a groove 6 for storing abrasive powder, particularly a groove 6 having a geometric pattern.
According to such a configuration, it is possible to polish the surface of the hemispherical end face required for an optical connector ferrule to a surface roughness of 4 nm or less extremely precisely on the polishing surface, and to make ferrule zirconia, fiber, etc. The abrasive powder can be accommodated by the groove.
The geometric pattern is a combination of linear grooves and is formed in a three to hexagonal shape with one side length of 1 μm to 300 μm, and the width of each groove is preferably 0.1 μm to 5 μm. FIG. 2 shows an example of a geometric pattern.
According to such a configuration, it is possible to store and hold the polishing powder (debris) of the object to be polished.
The polishing powder is usually removed together with the polishing liquid during the processing step. This suppresses a decrease in polishing ability due to the polishing powder.

前記ポリエステル基材としては、通常、ポリエチレンテレフタレートの2軸延伸したフィルム等が用いられる。
また、前記砥粒としては、ダイヤモンド、アルミナ、シリカ等の粒子が用いられる。
As the polyester substrate, a biaxially stretched film of polyethylene terephthalate or the like is usually used.
Moreover, as said abrasive grain, particles, such as a diamond, an alumina, a silica, are used.

前記研磨フィルムは、通常、ポリエステル基材フィルム上に砥粒とバインダー成分とを含む塗布液を塗布し、乾燥、反応硬化させて研磨層を形成した後、所定の円盤状に打ち抜いて得られるが、該研磨フィルムの製造方法としては、ポリエステル基材に塗布液を塗布した後、該ポリエステル基材の非塗布面側に加熱体を接触させ、ポリエステル基材側から加熱して乾燥させる方法が好ましい。
塗布後の乾燥をポリエステル基材側から加熱して行うことにより、塗布液の乾燥(即ち研磨層の形成)がポリエステル基材側から進むことから、溶剤が乾燥した表面を突き破って飛散するということが発生せず、基材から剥離し難い平滑な研磨層を形成することができる。
更に、例えば、幾何学模様を成す溝を有する研磨層を形成する場合には、溶剤が表面を突き破って飛散すると溝周辺が盛り上がった模様(研磨面を囲むスタジアムのような模様)ができ、また、ポリエステル基材から研磨層が剥離しやすく、摩耗耐久性の低い研磨フィルムとなる虞があるが、斯かる方法によれば、そのような虞もなく、平滑な研磨面と幾何学模様を成す溝とを有する表面を備えた研磨フィルムが得られる。
The abrasive film is usually obtained by applying a coating liquid containing abrasive grains and a binder component on a polyester base film, drying and reaction curing to form an abrasive layer, and then punching it into a predetermined disc shape. The method for producing the abrasive film is preferably a method in which a coating liquid is applied to a polyester substrate, a heating body is brought into contact with the non-coated surface side of the polyester substrate, and the polyester substrate is heated and dried. .
By drying from the polyester substrate side by drying after coating, the coating solution is dried (that is, forming the polishing layer) from the polyester substrate side, so that the solvent scatters through the dried surface. Thus, a smooth polishing layer that does not easily peel off from the substrate can be formed.
Furthermore, for example, when forming a polishing layer having grooves forming a geometric pattern, when the solvent breaks through the surface and scatters, a pattern in which the periphery of the groove is raised (pattern like a stadium surrounding the polishing surface) is formed. There is a risk that the polishing layer will be easily peeled off from the polyester base material, resulting in a polishing film with low wear durability. However, according to such a method, a smooth polishing surface and a geometric pattern are formed without such a risk. A polishing film having a surface with grooves is obtained.

以下、本発明の実施例について説明する。
実施例1
ポリオール成分として、末端にエチレンオキサイドを導入した1級化ポリプロピレングリコール(商品名「ハイパーライトE824」、住化バイエルウレタン社製、OH価=35mg/KOH)を80℃で1時間以上減圧脱泡して用い、イソシアネート成分(架橋剤)として、ジフェニルメタンジイソシアネート(MDI)(商品名「スミジュール」、住化バイエル社製)の2,4’−と4,4’−とを、重量比で2,4’−:4,4’−が47:53になるように混合した混合MDIを用いた。そして、このイソシアネート成分80重量部にエポキシ成分としてビスフェノールA型エポキシ樹脂(商品名「エポトートYD128」、東都化成社製)20重量部を混合してエポキシ成分含有イソシアネートを調製した。
次いで、上記エポキシ含有イソシアネート130重量部に上記1級ポリプロピレングリコール52重量部およびアミン系触媒(商品名「テスモラビットDB」、住化バイエルウレタン社製)1.3重量部を、常温で混合し(エポキシ成分/ポリオール成分=33.3/66.7)、この混合物に対し砥粒であるシリカの含有率が30重量%のオルガノシリカゾル(商品名「NPC−ST30」、日産化学社製、70重量%が溶剤)7600重量部を加え、混合分散させて、砥粒含有率(容量%)が85%の研磨層を形成するための塗布液(固形分含量22.9容量%)を調製した。
ポリエステル基材フィルムとして、幅300mmのPETフィルム(帝人デュポン社製HPE−75)をバーコータ式塗布機に供給し、上記塗布液を塗布し、ウエット状態でオーブン内の加熱体(100℃)上に裁置して1分間ポリエステル基材側から加熱して乾燥させ、次いで、温風を循環させて100℃で1分間1次キュアーした後、500mm長さに裁断し、更に、100℃で12時間アフターキュアーした後、冷めるまで常温で放置した。更に、直径110mmの円板状に打ち抜き加工して所望の研磨フィルムを得た。
尚、この研磨フィルムは、乾燥時の表面の収縮によって幾何学模様を成す溝が形成されていた。
この研磨フィルムを対象として、光干渉型表面測定機(日本ビーコ社製 NT−1100)にて表面粗さを測定し、算術平均粗さ(Ra)を求めた。別途、上記塗布液調製の際の砥粒(オルガノシリカゾル)を入れる前の混合物を型枠に注入し、型枠下面から100℃で加熱乾燥し、厚さ2mmのバインダー板を作成し、100℃で12時間アフターキュア後、常温で重ねて6mm厚にしてショアーD硬度計で硬度を測定した。
上記研磨フィルムより外径110mmに打抜き、光コネクタフェルール研磨機(セイコーインスツルメンツ社製 OFL−15)の研磨パッド上に裁置し、外径2.5mmのフェルールを12本セットで冶具に取り付け、12本全体で荷重1150+冶具重量330=1480gかけ、回転数:180rpmで光コネクタフェルールの研磨を行い、フェルール端面測定器(装置名「AC−3000」、NORLAND社製)によるフェルール研磨面の粗さ(Ra)が4nmより小さくなるまでの所要時間を研磨時間として測定した。
念のため研磨した光コネクタフェルールの表面粗さおよびファイバー部とフェルール部の段差を3次元形状測定機(装置名「AC−3000」、NORLAND社製)で測定した。
更に、研磨後のファイバー12本のスクラッチ傷の有無を「Video Fiber Microscope」(WESTOVER社製)により確認し、その本数をカウントした。
また、研磨フィルムの研磨層が摩減してポリエステル基材フィルムが露出したり、研磨層が剪断力に耐え切れず剥離したりすることによって生じる光コネクタフェルールの振動が発生するまでの12本セットでの繰返し研磨の回数を調べた。
これらの評価結果をまとめて表1に示す。
Examples of the present invention will be described below.
Example 1
As a polyol component, primary polypropylene glycol (trade name “Hyperlite E824”, manufactured by Sumika Bayer Urethane Co., Ltd., OH number = 35 mg / KOH) introduced with ethylene oxide at the terminal is degassed at 80 ° C. for 1 hour or more under reduced pressure. As an isocyanate component (crosslinking agent), 2,4′- and 4,4′- of diphenylmethane diisocyanate (MDI) (trade name “Sumijoule” manufactured by Sumika Bayer Co., Ltd.) Mixed MDI mixed so that 4 ′ −: 4,4′− was 47:53 was used. Then, an epoxy component-containing isocyanate was prepared by mixing 80 parts by weight of this isocyanate component with 20 parts by weight of a bisphenol A type epoxy resin (trade name “Epototo YD128”, manufactured by Tohto Kasei Co., Ltd.) as an epoxy component.
Next, 52 parts by weight of the above-mentioned primary polypropylene glycol and 1.3 parts by weight of an amine catalyst (trade name “Tesmorabit DB”, manufactured by Sumika Bayer Urethane Co., Ltd.) are mixed with 130 parts by weight of the above epoxy-containing isocyanate at room temperature ( Epoxy component / polyol component = 33.3 / 66.7), organosilica sol having 30% by weight of silica as abrasive grains with respect to this mixture (trade name “NPC-ST30”, manufactured by Nissan Chemical Co., Ltd., 70% by weight) 7600 parts by weight of solvent (% is solvent) was added and mixed and dispersed to prepare a coating solution (solid content 22.9% by volume) for forming a polishing layer having an abrasive grain content (volume%) of 85%.
As a polyester base film, a 300 mm wide PET film (HPE-75 manufactured by Teijin DuPont) is supplied to a bar coater type coating machine, and the above coating solution is applied to the heating body (100 ° C.) in an oven in a wet state. It is placed and heated for 1 minute from the polyester substrate side, dried, then circulated with warm air and subjected to primary curing at 100 ° C. for 1 minute, then cut to 500 mm length, and further at 100 ° C. for 12 hours. After after curing, it was left at room temperature until it cooled. Further, a desired abrasive film was obtained by punching into a disk shape having a diameter of 110 mm.
In this abrasive film, grooves forming a geometric pattern were formed by shrinkage of the surface during drying.
For this polishing film, the surface roughness was measured with an optical interference type surface measuring machine (NT-1100 manufactured by Nippon Beco Co., Ltd.), and the arithmetic average roughness (Ra) was determined. Separately, the mixture before adding the abrasive grains (organosilica sol) in preparing the coating solution is poured into a mold, and heated and dried at 100 ° C. from the lower surface of the mold to prepare a binder plate having a thickness of 2 mm. And after curing for 12 hours, it was piled up at room temperature to a thickness of 6 mm, and the hardness was measured with a Shore D hardness meter.
Punched to 110 mm outer diameter from the above polishing film, placed on a polishing pad of an optical connector ferrule polishing machine (OFL-15 manufactured by Seiko Instruments Inc.), and attached 12 sets of ferrules having an outer diameter of 2.5 mm to the jig. The entire surface is loaded with 1150 + jig weight 330 = 1480 g, the optical connector ferrule is polished at a rotation speed of 180 rpm, and the ferrule polished surface is roughened by a ferrule end face measuring device (device name "AC-3000", manufactured by NORLAND). The time required for Ra) to become smaller than 4 nm was measured as the polishing time.
As a precaution, the surface roughness of the polished optical connector ferrule and the level difference between the fiber portion and the ferrule portion were measured with a three-dimensional shape measuring machine (device name “AC-3000”, manufactured by NORLAND).
Further, the presence or absence of scratch scratches on the 12 fibers after polishing was confirmed by “Video Fiber Microscope” (manufactured by Westover), and the number was counted.
Also, a set of 12 pieces until the vibration of the optical connector ferrule generated when the polishing layer of the polishing film is worn away and the polyester base film is exposed or the polishing layer peels off without being able to withstand the shearing force. The number of times of repeated polishing was examined.
These evaluation results are summarized in Table 1.

実施例2
混合MDIに於ける2,4’−/4,4’−の比率を20/80に変えた以外は、実施例1と同様にして研磨フィルムを得、該研磨フィルムの特性評価及び光コネクタフェルールの研磨評価を行った。結果を表1に示す。
Example 2
A polishing film was obtained in the same manner as in Example 1 except that the ratio of 2,4 '-/ 4,4'- in the mixed MDI was changed to 20/80. Characteristic evaluation of the polishing film and optical connector ferrule Polishing evaluation was performed. The results are shown in Table 1.

実施例3
混合MDIに於ける2,4’−/4,4’の比率を50/50に変えた以外は、実施例1と同様にして研磨フィルムを得、該研磨フィルムの特性評価及び光コネクタフェルールの研磨評価を行った。結果を表1に示す。
Example 3
A polishing film was obtained in the same manner as in Example 1 except that the ratio of 2,4 ′-/ 4,4 ′ in the mixed MDI was changed to 50/50, and the characteristics of the polishing film were evaluated and the optical connector ferrule Polishing evaluation was performed. The results are shown in Table 1.

実施例4
エポキシ成分/ポリオール成分の比率を10/90に変えた以外は、実施例1と同様にして研磨フィルムを得、該研磨フィルムの特性評価及び光コネクタフェルールの研磨評価を行った。結果を表1に示す。
Example 4
A polishing film was obtained in the same manner as in Example 1 except that the ratio of the epoxy component / polyol component was changed to 10/90, and the characteristics of the polishing film and the polishing evaluation of the optical connector ferrule were evaluated. The results are shown in Table 1.

実施例5
エポキシ成分/ポリオール成分の比率を90/10に変えた以外は、実施例1と同様にして研磨フィルムを得、研磨フィルムの特性評価及び光コネクタフェルールの研磨評価を行った。結果を表1に示す。
Example 5
A polishing film was obtained in the same manner as in Example 1 except that the ratio of the epoxy component / polyol component was changed to 90/10, and the characteristics evaluation of the polishing film and the polishing evaluation of the optical connector ferrule were performed. The results are shown in Table 1.

比較例1
研磨層がシリコン系ポリマーと称されている市販の研磨フィルムを用い、実施例1と同様に研磨フィルムの評価および研磨性能の評価を行った。結果を表1に示す。
Comparative Example 1
The polishing film was evaluated and the polishing performance was evaluated in the same manner as in Example 1 using a commercially available polishing film whose polishing layer was referred to as a silicon-based polymer. The results are shown in Table 1.

比較例2
バインダーとして、ポリオール成分がポリプロピレングリコール(PPG)、イソシアネート成分がジフェニルメタンジイソシアネート(MDI)を、NCOインデックス1.2で反応させたエポキシ成分を含まないポリウレタンを用い、実施例1と同じポリエステル基材上にシリカ砥粒を50容量%で含有させた研磨層を形成して研磨フィルムを製作し、実施例1と同様に研磨フィルムの評価および研磨性能の評価を行った。結果を表1に示す。
Comparative Example 2
On the same polyester base material as in Example 1, a polyurethane that does not contain an epoxy component in which a polyol component is polypropylene glycol (PPG) and an isocyanate component is reacted with diphenylmethane diisocyanate (MDI) with an NCO index of 1.2 is used as a binder. A polishing layer containing 50% by volume of silica abrasive grains was formed to produce a polishing film. The polishing film was evaluated and the polishing performance was evaluated in the same manner as in Example 1. The results are shown in Table 1.

表1から明らかなように、実施例のものは、研磨可能回数が従来のシリコン系に比し1.5倍以上となっており、耐久性が向上したものと認められる。また、同水準の表面粗さのものを得るための研磨時間が90秒から60秒へと従来の約2/3に短縮されており、研磨速度も向上したものと認められ、しかも、ファイバーの接合面にスクラッチ傷が発生し難いものと認められる。
熟成時間は12時間で済み、従来のシリコン系に比し大幅な短縮で、生産性も向上したものと認められる。
As is apparent from Table 1, in the examples, the number of polishable times is 1.5 times or more that of the conventional silicon system, and it is recognized that the durability is improved. In addition, the polishing time for obtaining the same level of surface roughness has been shortened from 90 seconds to 60 seconds to about 2/3 of the conventional one, and it is recognized that the polishing speed has been improved. It is recognized that scratches are hardly generated on the joint surface.
The ripening time is 12 hours, and it is recognized that productivity is improved by a significant shortening compared to the conventional silicon system.

一実施形態の研磨フィルムを示す概略断面図。1 is a schematic cross-sectional view showing an abrasive film of one embodiment. 同実施形態の研磨フィルムの断面及び上面を示す概略斜視図。The schematic perspective view which shows the cross section and upper surface of the polishing film of the embodiment.

符号の説明Explanation of symbols

1・・・研磨フィルム、
2・・・ポリエステル基材フィルム
3・・・研磨層
1 ... Abrasive film,
2 ... Polyester base film 3 ... Polishing layer

Claims (8)

ポリエステル基材フィルム上に、砥粒とバインダーとを備えてなる研磨層が設けられてなる研磨フィルムであって、
前記バインダーが、ポリオール成分とエポキシ成分と架橋剤とを反応硬化させてなるエポキシウレタンであることを特徴とする研磨フィルム。
On a polyester base film, a polishing film provided with a polishing layer comprising abrasive grains and a binder,
A polishing film, wherein the binder is an epoxy urethane obtained by reaction curing of a polyol component, an epoxy component, and a crosslinking agent.
前記エポキシウレタンが、ショアーD硬度20〜90である請求項1記載の研磨フィルム。   The polishing film according to claim 1, wherein the epoxy urethane has a Shore D hardness of 20 to 90. 前記架橋剤が2,4’−ジフェニルメタンジイソシアネートと4,4’−ジフェニルメタンジイソシアネートとの混合物で、2,4’−ジフェニルメタンジイソシアネートと4,4’−ジフェニルメタンジイソシアネートとの重量比(2,4’−/4,4’−)が20/80〜80/20である請求項1又は2記載の研磨フィルム。   The crosslinking agent is a mixture of 2,4′-diphenylmethane diisocyanate and 4,4′-diphenylmethane diisocyanate, and the weight ratio of 2,4′-diphenylmethane diisocyanate to 4,4′-diphenylmethane diisocyanate (2,4 ′ − / The polishing film according to claim 1 or 2, wherein 4,4'-) is 20/80 to 80/20. 前記エポキシ成分と前記ポリオール成分との重量比(エポキシ成分/ポリオール成分)が10/90〜90/10である請求項1乃至3の何れか1項記載の研磨フィルム。   The abrasive film according to any one of claims 1 to 3, wherein a weight ratio of the epoxy component to the polyol component (epoxy component / polyol component) is 10/90 to 90/10. 前記ポリオール成分が、末端にエチレンオキサイド基を有する請求項1乃至4の何れか1項記載の研磨フィルム。   The polishing film according to any one of claims 1 to 4, wherein the polyol component has an ethylene oxide group at a terminal. 前記研磨層の表面が、JISB0601に規定する算術平均表面粗さ(クラック部を除く)で0.1μm以下の平滑な研磨面と、研磨粉を収容する溝とを有する請求項1乃至5の何れか1項記載の研磨フィルム。   The surface of the polishing layer has a smooth polishing surface having an arithmetic average surface roughness (excluding cracks) as defined in JISB0601 of 0.1 μm or less, and a groove for containing polishing powder. The polishing film according to claim 1. 前記溝が幾何学模様をなし、該幾何学模様が不定形な三〜六角形で、一辺の長さが1μm〜300μmであり、前記溝の幅が0.1μm〜5μmである請求項6記載の研磨フィルム。   The groove has a geometric pattern, the geometric pattern is an irregular three to hexagonal shape, one side has a length of 1 μm to 300 μm, and the width of the groove is 0.1 μm to 5 μm. Polishing film. ポリエステル基材の片面に砥粒とバインダー成分とを含む塗布液を塗布し乾燥させて研磨層を形成する研磨フィルムの製造方法であって、ポリエステル基材にポリオール成分とエポキシ成分と架橋剤とを含む塗布液を塗布した後、該ポリエステル基材の非塗布面側に加熱体を接触させ、ポリエステル基材側から加熱して乾燥させることを特徴とする研磨フィルムの製造方法。   A method for producing a polishing film in which a coating liquid containing abrasive grains and a binder component is applied to one side of a polyester substrate and dried to form a polishing layer. The polyester substrate includes a polyol component, an epoxy component, and a crosslinking agent. A method for producing a polishing film, comprising: applying a coating solution containing the coating material, bringing a heating body into contact with the non-coated surface side of the polyester base material, and heating and drying the polyester base material side.
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KR20170016443A (en) 2014-07-07 2017-02-13 반도 카가쿠 가부시키가이샤 Polishing film
US10543582B2 (en) 2014-07-07 2020-01-28 Bando Chemical Industries, Ltd. Abrasive film
KR20170039750A (en) 2014-08-21 2017-04-11 반도 카가쿠 가부시키가이샤 Polishing film
US10220488B2 (en) 2014-08-21 2019-03-05 Bando Chemical Industries, Ltd. Abrasive film
WO2016047535A1 (en) * 2014-09-26 2016-03-31 バンドー化学株式会社 Polishing pad and method for producing polishing pad
JPWO2016047535A1 (en) * 2014-09-26 2017-07-20 バンドー化学株式会社 Polishing pad and polishing pad manufacturing method
JP2021020314A (en) * 2014-09-26 2021-02-18 バンドー化学株式会社 Polishing pad and method for producing polishing pad
WO2022220161A1 (en) * 2021-04-15 2022-10-20 株式会社アドマテックス Ferrule polishing material

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