JP2008216639A - Coating material - Google Patents
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本発明は、電子写真方式のプリンタやファクシミリ及び複写機などの画像形成装置に適用される定着ロールや金型表面保護膜などにおいて離型性と耐摩耗性が必要とされるコート材料に関するものである。 The present invention relates to a coating material that requires releasability and wear resistance in a fixing roll and a mold surface protective film applied to an image forming apparatus such as an electrophotographic printer, a facsimile machine, and a copying machine. is there.
従来、電子写真プロセスを利用した複写機等においては、記録シート上に形成された未定着トナー像を定着して永久画像にする必要があり、また、セメントや樹脂等を成形する際の金型においては、成形後に型離れを良くするために金型表面保護膜が必要であり、これらにフッ素樹脂コート材料が用いられている。 Conventionally, in a copying machine using an electrophotographic process, it is necessary to fix an unfixed toner image formed on a recording sheet to make a permanent image, and a mold for molding cement or resin In order to improve mold separation after molding, a mold surface protective film is required, and a fluororesin coating material is used for these.
しかし、離型性が良好なフッ素樹脂材料は、定着ローラにおいては紙の通過による摩耗が大きく、また金型表面保護膜においては材料の流動や型離れ時の摩耗が大きいため、耐摩耗性の改善が望まれていた。 However, the fluororesin material with good releasability has a large wear due to the passage of paper in the fixing roller, and the wear of the material on the mold surface protection film due to the flow of the material and a large amount of wear at the time of mold release. Improvement was desired.
耐摩耗性の改善するために材料配合が種々検討されており、タールエポキシ樹脂（中国塗料株式会社製、バンノ−５００）や各種メッキによる耐摩耗性の向上がなされているが、離型性との両立ができない。 Various material formulations have been studied to improve wear resistance, and wear resistance has been improved by tar epoxy resin (manufactured by China Paint Co., Ltd., Vanno-500) and various types of plating. Cannot be compatible.
離型性に優れた材料として、フッ素樹脂やフッ素樹脂にカーボン繊維を配合した材料が知られているが、耐摩耗性が不十分で、交換回数が多くなる問題があった。 As a material excellent in releasability, a fluororesin or a material in which a carbon fiber is blended with a fluororesin is known, but there is a problem in that the wear resistance is insufficient and the number of exchanges is increased.
フッ素樹脂が離型性に優れる理由は、フッ素樹脂が主に炭素原子とフッ素原子から分子が構成されているためである。フッ素原子は、電子と原子核の相互作用が強いため分極しにくい元素であるため、分子間力が小さく、フッ素樹脂の分子骨格である−ＣＦ2 −の分子間凝集エネルギーは−ＣＨ2 −に匹敵するほど小さく、各々７６０ｃａｌ、６８０ｃａｌである。同族元素の−ＣＣｌ2 −が３７８０ｃａｌであることからも、フッ素樹脂の分子間力が小さいことが理解できる。 The reason why the fluororesin is excellent in releasability is that the molecule is composed mainly of carbon atoms and fluorine atoms. Fluorine atoms are elements that are difficult to polarize due to strong interaction between electrons and nuclei, so the intermolecular force is small, and the intermolecular cohesive energy of —CF 2 —, the molecular skeleton of fluororesin, is comparable to —CH 2 —. It is so small that it is 760 cal and 680 cal, respectively. It can be understood that the intermolecular force of the fluororesin is small also from the fact that the homologous element —CCl 2 — is 3780 cal.
この性質から表面の分子を内部に引き付ける力である表面自由エネルギーは著しく小さく、各種液体に濡れにくく離型性に優れた材料となる（ふっ素樹脂ハンドブック、３〜６ページ）。 Because of this property, the surface free energy, which is the force that attracts surface molecules to the inside, is remarkably small, making it a material that is not easily wetted by various liquids and has excellent releasability (Fluorine Resin Handbook, pages 3-6).
このような離型性に優れたフッ素樹脂の耐摩耗性を改善するために、充てん材を添加することが行われる。充てん材は、３００℃以上のフッ素樹脂の焼成温度で分解しない性質が必要であるので、無機材料が用いられ、ガラスファイバ、グラファイト、ブロンズ、二硫化モリブデン、カーボン、カーボン繊維、セラミック、マイカなどが充てんされる。これらを、用途に応じて、単体もしくは適当に組合せて材料を作ることが通常行われている（ハンドブックシール、ゴム・プラスチック製品、１９〜２１ページ）。 In order to improve the wear resistance of such a fluororesin excellent in releasability, a filler is added. Since the filler must have the property of not decomposing at the firing temperature of fluororesin of 300 ° C. or higher, inorganic materials are used, such as glass fiber, graphite, bronze, molybdenum disulfide, carbon, carbon fiber, ceramic, mica, etc. Filled. It is usual to make these materials by combining them alone or appropriately depending on the application (handbook seal, rubber / plastic products, pages 19 to 21).
その反面、充てん材は、その化学構造から離型性を低下させる原因になる。そのため、耐摩耗性にも優れた離型層を簡易に作製できるコート材料に関しては充てん材を１０重量％以下で使用されることが多い。 On the other hand, the filler causes a decrease in mold release properties from the chemical structure. Therefore, the filler is often used at 10% by weight or less for a coating material that can easily produce a release layer having excellent wear resistance.
しかしながら、この方法においても、定着ロール表面の離型層や金型表面保護膜としての離型性と耐摩耗性を両立させることができなかった。 However, even with this method, it has been impossible to achieve both mold release properties and wear resistance as a release layer on the surface of the fixing roll and a mold surface protective film.
そこで、本発明の目的は、定着ロール表面の離型層や金型表面保護膜として、離型性が優れ、更に耐摩耗性にも優れたフッ素樹脂のコート材料を提供することにある。 Accordingly, an object of the present invention is to provide a fluororesin coating material having excellent releasability and excellent wear resistance as a release layer or mold surface protective film on the surface of a fixing roll.
本発明者等は、上記の各問題点に鑑み、種々検討した結果、繊維長が５０μｍ以下の黒鉛系のカーボン繊維と、融点近くの温度に加熱し、不活性ガス雰囲気中で電離性放射線を照射して架橋させた架橋ＰＴＦＥとを、テトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体（以下、ＰＦＡと略す）、テトラフルオロエチレン−ヘキサフルオロプロピレン共重合体（以下、ＦＥＰと略す）、テトラフルオロエチレン−パーフルオロメチルビニルエーテル（以下、ＭＦＡと略す）からなる群より選ばれた少なくとも１つのフッ素樹脂に混ぜた離型層を、円筒状コアロール上に形成させることにより、離型性は良好で、かつ耐摩耗性が飛躍的に向上できることを見出した。 As a result of various studies in view of the above-mentioned problems, the present inventors have heated graphite fiber having a fiber length of 50 μm or less and a temperature close to the melting point to emit ionizing radiation in an inert gas atmosphere. Irradiated and crosslinked PTFE is converted into tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (hereinafter abbreviated as PFA), tetrafluoroethylene-hexafluoropropylene copolymer (hereinafter abbreviated as FEP), tetrafluoro By forming a release layer mixed with at least one fluororesin selected from the group consisting of ethylene-perfluoromethyl vinyl ether (hereinafter abbreviated as MFA) on a cylindrical core roll, the release property is good. In addition, the present inventors have found that the wear resistance can be dramatically improved.
すなわち、請求項１の発明は、繊維長が５０μｍ以下の黒鉛系のカーボン繊維と、ポリテトラフルオロエチレン（ＰＴＦＥ）を融点近くの温度に加熱し、これを不活性ガス雰囲気中で電離性放射線を照射して架橋させた架橋ＰＴＦＥを含むフッ素樹脂からなることを特徴とするコート材料である。 That is, the invention of claim 1 heats graphite-based carbon fiber having a fiber length of 50 μm or less and polytetrafluoroethylene (PTFE) to a temperature close to the melting point, which is then subjected to ionizing radiation in an inert gas atmosphere. A coating material comprising a fluororesin containing crosslinked PTFE that has been crosslinked by irradiation.
請求項２の発明は、黒鉛系のカーボン繊維が、そのカーボン繊維と架橋ＰＴＦＥ及びフッ素樹脂との総重量の１〜５ｗｔ％含有する請求項１に記載のコート材料である。
The invention according to
請求項３の発明は、架橋ＰＴＦＥが、黒鉛系のカーボン繊維と架橋ＰＴＦＥ及びフッ素樹脂との総重量の１０〜３０ｗｔ％含有する請求項１又は２に記載のコート材料である。 The invention according to claim 3 is the coating material according to claim 1 or 2, wherein the crosslinked PTFE contains 10 to 30 wt% of the total weight of the graphite-based carbon fiber, the crosslinked PTFE and the fluororesin.
請求項４の発明は、フッ素樹脂は、融点近くの温度に加熱し、不活性ガス雰囲気中で電離性放射線を照射して架橋させたポリテトラフルオロエチレン（ＰＴＦＥ）を含み、ベースのフッ素樹脂として、テトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体（ＰＦＡ）、テトラフルオロエチレン−ヘキサフルオロプロピレン共重合体（ＦＥＰ）、テトラフルオロエチレン−パーフルオロメチルビニルエーテル（ＭＦＡ）からなる群より選ばれた少なくとも１つの樹脂からなる請求項１〜３のいずれかに記載のコート材料である。 According to a fourth aspect of the present invention, the fluororesin includes polytetrafluoroethylene (PTFE) crosslinked by irradiation with ionizing radiation in an inert gas atmosphere, heated to a temperature close to the melting point, , Tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), tetrafluoroethylene-hexafluoropropylene copolymer (FEP), and at least one selected from the group consisting of tetrafluoroethylene-perfluoromethyl vinyl ether (MFA) The coating material according to any one of claims 1 to 3, comprising one resin.
本発明によれば、繊維長が５０μｍ以下の黒鉛系のカーボン繊維と電離性放射線を照射して架橋させた架橋ＰＴＦＥを含むフッ素樹脂で形成される離型層を有する定着ロールや金型は、離型性と耐熱特性に優れ、さらに耐摩耗性に優れているので、定着ロールや金型の保護膜の寿命を延ばすことができる。更に、本発明のフッ素樹脂は、容易にコーティングできるので、経済性に優れるという利点もある。 According to the present invention, a fixing roll or a mold having a release layer formed of a fluorocarbon resin containing a graphite-based carbon fiber having a fiber length of 50 μm or less and a crosslinked PTFE crosslinked by irradiating with ionizing radiation, Since it has excellent releasability and heat resistance, and also has excellent wear resistance, it can extend the life of the protective film of the fixing roll and mold. Furthermore, since the fluororesin of the present invention can be easily coated, there is an advantage that it is excellent in economic efficiency.
以下、本発明の好適な一実施の形態を添付図面に基づいて詳述する。 A preferred embodiment of the present invention will be described below in detail with reference to the accompanying drawings.
図１において、円筒状のアルミニウム芯金１の表面をサンドブラストで粗面化し、耐熱タイプのプライマーを塗装すると共に焼き付けてプライマー層２を形成し、その上に本発明のコート材料を離型層３として形成するものである。
In FIG. 1, the surface of a cylindrical aluminum core 1 is roughened by sand blasting, and a primer of heat resistant type is applied and baked to form a
本発明は、このコート材料は、例えば、ポリテトラフルオロエチレン（ＰＴＦＥ）を融点近くの温度に加熱し、不活性ガス雰囲気中で電離性放射線を照射して架橋させた架橋ＰＴＦＥと、繊維長が５０μｍ以下の黒鉛系のカーボン繊維とを含み、これをテトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体（ＰＦＡ）、テトラフルオロエチレン−ヘキサフルオロプロピレン共重合体（ＦＥＰ）、テトラフルオロエチレン−パーフルオロメチルビニルエーテル（ＭＦＡ）からなる群より選ばれた少なくとも１つのフッ素樹脂に混ぜて形成され、このコート材料を、静電塗装やスプレー塗装にて、基材の表面に塗布したのち、電気炉等で焼き付けを行って離型層とするものである。 In the present invention, the coating material includes, for example, crosslinked PTFE obtained by heating polytetrafluoroethylene (PTFE) to a temperature close to the melting point and irradiating with ionizing radiation in an inert gas atmosphere, and a fiber length. And a graphite-based carbon fiber having a size of 50 μm or less, which is a tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), a tetrafluoroethylene-hexafluoropropylene copolymer (FEP), or a tetrafluoroethylene-perfluoromethyl. Formed by mixing with at least one fluororesin selected from the group consisting of vinyl ether (MFA), this coating material is applied to the surface of the substrate by electrostatic coating or spray coating, and then baked in an electric furnace or the like To form a release layer.
本発明において、基材としては、金属或いはガラスからなる円筒状ロールや金型が挙げられる。 In the present invention, examples of the base material include cylindrical rolls and dies made of metal or glass.
ＰＴＦＥへの電離性放射線の照射は、酸素濃度１０Ｔｏｒｒ以下の不活性ガス雰囲気で、その樹脂の融点近くの温度に加熱された状態で行われる。具体的には放射線の照射は、ＰＴＦＥの融点より１０℃〜３０℃高い温度で行なうことが好ましい。 Irradiation of ionizing radiation to PTFE is performed in an inert gas atmosphere having an oxygen concentration of 10 Torr or less and heated to a temperature near the melting point of the resin. Specifically, the irradiation with radiation is preferably performed at a temperature that is 10 ° C. to 30 ° C. higher than the melting point of PTFE.
ＰＴＦＥを含むフッ素樹脂類の多くは、２７０℃〜３３０℃の融点をもつ。例えば融点が３１０℃のポリテトラフルオロエチレンの場合、照射温度は３２０℃〜３４０℃が適当である。これにより、ＰＴＦＥが架橋剤なしで架橋させることができる。この時に用いる電離性放射線としては、γ線、電子線、Ｘ線、中性子線等が使用される。 Many of fluororesins including PTFE have a melting point of 270 ° C to 330 ° C. For example, in the case of polytetrafluoroethylene having a melting point of 310 ° C, the irradiation temperature is suitably 320 ° C to 340 ° C. Thereby, PTFE can be crosslinked without a crosslinking agent. As the ionizing radiation used at this time, γ-rays, electron beams, X-rays, neutron beams and the like are used.
電離性放射線を照射して架橋させた架橋ＰＴＦＥを、ＰＦＡ、又はＭＦＡ、ＦＥＰのどれか１つのベース樹脂中に混ぜる割合は、１０〜３０重量％が好ましい。 The proportion of the cross-linked PTFE that has been cross-linked by irradiation with ionizing radiation in the base resin of any one of PFA, MFA, and FEP is preferably 10 to 30% by weight.
また、このようなフッ素樹脂で形成される離型層の厚さは、５〜５０μｍの範囲が好ましい。また、離型層の表面粗さは、平均粗値Ｒａで０．３以下、最大粗値Ｒｚで４以下が好ましい。 Moreover, the thickness of the release layer formed of such a fluororesin is preferably in the range of 5 to 50 μm. Further, the surface roughness of the release layer is preferably 0.3 or less in terms of the average roughness Ra and 4 or less in terms of the maximum roughness Rz.
カーボン繊維は、１０００〜１５００℃程度で繊維化させる炭素系ではなく、２０００〜３０００℃程度の高温で繊維化する黒鉛系のカーボン繊維を用い、且つその繊維長さは５０μｍ以下であることが好ましい。 The carbon fiber is not a carbon fiber that is fiberized at about 1000 to 1500 ° C., but a graphite-based carbon fiber that is fiberized at a high temperature of about 2000 to 3000 ° C., and the fiber length is preferably 50 μm or less. .
これは炭素系のカーボン繊維を混和した場合には処理温度が低いため、繊維に依存する官能基により離型層にトナーが着くオフセット現象が発生し易く、離型性が悪くなるためである。 This is because when carbon-based carbon fibers are mixed, the processing temperature is low, and therefore, an offset phenomenon in which toner is attached to the release layer due to functional groups depending on the fibers is likely to occur, and the releasability is deteriorated.
これに対し、黒鉛結晶がより成長した構造を有する高弾性率繊維である黒鉛系のカーボン繊維では、このような離型性への影響が小さく、しかも耐摩耗性を向上できることを見出した。また、その繊維長さをより好ましくは１０〜３０μｍとすることにより、さらに、分散性が向上し弾性率が改善する。 On the other hand, it has been found that a graphite-based carbon fiber, which is a high-modulus fiber having a structure in which graphite crystals are further grown, has a small influence on the releasability and can improve wear resistance. Further, by setting the fiber length to more preferably 10 to 30 μm, the dispersibility is further improved and the elastic modulus is improved.
また、カーボン繊維が、カーボン繊維と架橋させた架橋ＰＴＦＥ及びフッ素樹脂との総重量の１〜５ｗｔ％以内であることが好ましい。 Moreover, it is preferable that the carbon fiber is within 1 to 5 wt% of the total weight of the crosslinked PTFE and the fluororesin crosslinked with the carbon fiber.
カーボン繊維は、高弾性率で耐引掻き摩耗性に優れた材料であるため、耐摩耗性を改善するために必須であるが、１ｗｔ％未満では耐摩耗性向上の効果が見られない。一方、カーボン繊維が、カーボン繊維と架橋させた架橋ＰＴＦＥとフッ素樹脂との総重量の５ｗｔ％を超える場合には、表面の平滑面が著しく損なわれ、未定着トナー層が離型層にトナーが着くオフセット現象が発生し、離型性が悪くなるためである。 Since carbon fiber is a material having a high elastic modulus and excellent scratch resistance, it is essential for improving the wear resistance. However, if it is less than 1 wt%, the effect of improving the wear resistance is not observed. On the other hand, when the carbon fiber exceeds 5 wt% of the total weight of the cross-linked PTFE cross-linked with the carbon fiber and the fluororesin, the smooth surface of the surface is remarkably impaired, and the unfixed toner layer becomes a toner in the release layer. This is because the offset phenomenon that arrives occurs and the releasability deteriorates.
カーボン繊維を混和させず架橋させたＰＴＦＥをＰＦＡに混和させた場合には、フッ素樹脂以外に混和していないため離型性に優れ、耐摩耗性に有効な架橋させたＰＴＦＥを混和しているが、耐摩耗性が不十分になる。これは紙の繰り返しの通過によって、離型層が徐々に引き剥がされるためと推定される。耐引掻き摩耗性が不十分と考えられる。 When PTFE crosslinked without carbon fiber is mixed with PFA, it is mixed with PTFE which is excellent in releasability and effective in abrasion resistance because it is not mixed with other than fluororesin. However, the wear resistance is insufficient. This is presumably because the release layer is gradually peeled off by repeated passage of paper. Scratch wear resistance is considered insufficient.
架橋させた架橋ＰＴＦＥを混和させず、架橋なしのＰＴＦＥをＰＦＡに混和させた場合には、フッ素樹脂以外に混和していないため離型性に優れるが、耐摩耗性に有効な材料を混和していないため耐摩耗性は劣る。 When cross-linked cross-linked PTFE is not mixed and non-cross-linked PTFE is mixed with PFA, it is excellent in releasability because it is not mixed with other than fluororesin, but a material effective for wear resistance is mixed. The wear resistance is poor.
架橋させた架橋ＰＴＦＥを、カーボン繊維と架橋ＰＴＦＥ及びフッ素樹脂との総重量の１０重量％以下で混和する場合には、摩擦係数が大きくなり、耐摩耗性が悪くなる。一方、架橋ＰＴＦＥを、カーボン繊維と架橋ＰＴＦＥ及びフッ素樹脂との総重量の３０重量％以上で混和する場合には、平滑面が得られず、離型層にトナーが着くオフセット現象が発生し、離型性が悪くなる。 When the cross-linked cross-linked PTFE is mixed at 10% by weight or less of the total weight of the carbon fiber, the cross-linked PTFE and the fluororesin, the friction coefficient is increased and the wear resistance is deteriorated. On the other hand, when the cross-linked PTFE is mixed with 30% by weight or more of the total weight of the carbon fiber, the cross-linked PTFE and the fluororesin, a smooth surface is not obtained, and an offset phenomenon occurs in which the toner adheres to the release layer. The release property becomes worse.
カーボン繊維の繊維長さを５０μｍより長くすると離型層表面に凹凸を生じやすくなり、離型性を低下させてしまう。カーボン繊維の長さは、５０μｍより小さければ小さいほど平滑性に有利である。 If the fiber length of the carbon fiber is longer than 50 μm, irregularities are likely to occur on the surface of the release layer, and the releasability is deteriorated. The length of the carbon fiber is more advantageous for smoothness as it is smaller than 50 μm.
以下、本発明の実施例と比較例について説明する。 Examples of the present invention and comparative examples will be described below.
３０ｍｍのアルミニウム四角板の表面をサンドブラストで粗面化し、耐熱タイプの金属用プライマー（ダイキン工業製、ＧＬＰ−１０３ＳＲ）を２μｍ厚となるように塗装し、１５０℃で１０分間焼き付け、７０℃で１０分間乾燥し、プライマー層を作製する。
The surface of a 30 mm aluminum square plate was roughened by sandblasting, and a heat-resistant metal primer (GLP-103SR, manufactured by Daikin Industries, Ltd.) was applied to a thickness of 2 μm, baked at 150 ° C. for 10 minutes, and 10 ° C. at 70 ° C. Dry for minutes to make a primer layer.
次いで、その上に、電離性放射線を照射して架橋させた架橋ＰＴＦＥと繊維長が５０μｍの黒鉛系のカーボン繊維を、ベース樹脂であるＰＦＡに、１５重量％と１重量％の割合で混ぜたフッ素樹脂を用いて離型層を作製した。 Subsequently, crosslinked PTFE crosslinked by irradiating with ionizing radiation and graphite-based carbon fiber having a fiber length of 50 μm were mixed with PFA as a base resin at a ratio of 15% by weight to 1% by weight. A release layer was prepared using a fluororesin.
（実施例２〜５）
架橋ＰＴＦＥと繊維長が５０μｍの黒鉛系のカーボン繊維の混合割合を、１５重量％と３重量％（実施例２）、１５重量％と５重量％（実施例３）、１０重量％と５重量％（実施例４）、２０重量％と５重量％（実施例５）と変えたフッ素樹脂を用いて離型層を作製した。
(Examples 2 to 5)
The mixing ratio of the crosslinked PTFE and the graphite-based carbon fiber having a fiber length of 50 μm is 15 wt% and 3 wt% (Example 2), 15 wt% and 5 wt% (Example 3), 10 wt% and 5 wt%. % (Example 4), 20% by weight and 5% by weight (Example 5) were used to produce a release layer.
（実施例６、７）
ベース樹脂を実施例１〜５のＰＦＡから、ＭＦＡ、ＦＥＰに変え、架橋ＰＴＦＥと繊維長が５０μｍの黒鉛系のカーボン繊維の混合割合を、２０重量％と３重量％として離型層を作製した。
(Examples 6 and 7)
The base resin was changed from PFA of Examples 1 to 5 to MFA and FEP, and a release layer was prepared by setting the mixing ratio of crosslinked PTFE and graphite-based carbon fiber having a fiber length of 50 μm to 20 wt% and 3 wt%. .
（比較例１）
カーボン繊維を混和させずに、架橋ＰＴＦＥを１５重量％となるようにベース樹脂としてのＰＦＡに混和させて離型層を作製した。
(Comparative Example 1)
A release layer was prepared by mixing crosslinked PTFE with PFA as a base resin so as to be 15% by weight without mixing carbon fiber.
（比較例２）
架橋ＰＴＦＥを１５重量％となるように、またカーボン繊維の混和量を１０重量％となるようにＰＦＡに混和させて離型層を作製した。
(Comparative Example 2)
A release layer was prepared by blending with PFA such that the cross-linked PTFE was 15% by weight and the amount of carbon fiber was 10% by weight.
（比較例３）
黒鉛系のカーボン繊維を用いずに炭素系のカーボン繊維を用い、実施例２と同様な混合割合で混和させて離型層を作製した。
(Comparative Example 3)
A release layer was prepared by mixing carbon-based carbon fibers at the same mixing ratio as in Example 2 without using graphite-based carbon fibers.
（比較例４）
架橋ＰＴＦＥを用いず、架橋なしのＰＴＦＥを用い、実施例２と同様な混合割合で混和させて離型層を作製した。
(Comparative Example 4)
A release layer was prepared by mixing PTFE without crosslinking and using PTFE without crosslinking at the same mixing ratio as in Example 2.
（比較例５）
架橋ＰＴＦＥと黒鉛系のカーボン繊維を、それぞれ３重量％、ＰＦＡに混和させて離型層を作製した。
(Comparative Example 5)
A release layer was prepared by mixing 3% by weight of crosslinked PTFE and graphite-based carbon fiber with PFA.
（比較例６）
架橋ＰＴＦＥを、ＰＦＡに５０重量％で混和させて離型層を作製した。
(Comparative Example 6)
Crosslinked PTFE was mixed with PFA at 50% by weight to prepare a release layer.
（比較例７）
繊維長さ７０μｍと長い黒鉛系のカーボン繊維を用い、実施例２と同様な混合割合で混和させて離型層を作製した。
(Comparative Example 7)
Using a long graphite fiber having a fiber length of 70 μm, the release layer was prepared by mixing at the same mixing ratio as in Example 2.
実施例１〜７及び比較例１〜３、比較例５〜７の架橋ＰＴＦＥは、ＰＴＦＥを、酸素濃度１０Ｔｏｒｒ以下の不活性ガス雰囲気で、その樹脂の融点近くの温度に加熱された状態として電離性放射線を照射して架橋させたものである。具体的には、ＰＴＦＥモールディングパウダー（旭硝子社製、Ｇ−１６３）を酸素濃度２Ｔｏｒｒの雰囲気中で、３４０℃の加熱温度のもとで、電子線を１００ｋＧｙ照射して行う。 The crosslinked PTFE of Examples 1 to 7 and Comparative Examples 1 to 3 and Comparative Examples 5 to 7 are ionized as PTFE is heated to a temperature near the melting point of the resin in an inert gas atmosphere having an oxygen concentration of 10 Torr or less. It has been crosslinked by irradiating with actinic radiation. Specifically, PTFE molding powder (G-163, manufactured by Asahi Glass Co., Ltd.) is irradiated with an electron beam at 100 kGy at a heating temperature of 340 ° C. in an atmosphere with an oxygen concentration of 2 Torr.
これにより、得られた架橋されたＰＴＦＥを、平均粒径が１０μｍになるまでジェットミルで粉砕して架橋ＰＴＦＥとする。 Thus, the obtained cross-linked PTFE is pulverized with a jet mill until the average particle size becomes 10 μm to obtain cross-linked PTFE.
この架橋ＰＴＦＥに、ＰＦＡ粉末（デュポン社製、ＭＰ１０２）等とカーボン繊維を表１に示した割合で混合させ、フッ素樹脂粉末を作製する。 This cross-linked PTFE is mixed with PFA powder (manufactured by DuPont, MP102) and carbon fiber in the proportions shown in Table 1 to produce a fluororesin powder.
この粉末を、接着層（プライマー層）を塗布したアルミニウム四角板（或いはロール）上に、３５ｋＶの電圧を印加しながら静電塗装する。 This powder is electrostatically coated while applying a voltage of 35 kV on an aluminum square plate (or roll) coated with an adhesive layer (primer layer).
静電塗装後、電気炉内で３５０℃の温度で３０分間焼成し、炉外で放冷した後、表面を研磨して、厚さ３０μｍで表面粗さがＲａで０．２以下、Ｒｚで２以下の離型層を形成した。同様な方法で加圧ロールも作製した。 After electrostatic coating, it is baked for 30 minutes at a temperature of 350 ° C. in an electric furnace, allowed to cool outside the furnace, and then the surface is polished to have a thickness of 30 μm and a surface roughness Ra of 0.2 or less, Rz Two or less release layers were formed. A pressure roll was also produced in the same manner.
以上のようにして得られたコート材料板を用いて、離型性を比較するために、接触角を調べた。フッ素樹脂の２４℃の水に対する接触角は１０８゜である。小さな値ほど離型性が悪い。実機のトナーの性状や離型材の使用により、実機に使用できる定着ローラ離型層の接触角は制約され、１００°以上が望ましい。上記接触角が１００°以上を特性良好、１００°未満を不良と判断した。 In order to compare the releasability using the coating material plate obtained as described above, the contact angle was examined. The contact angle of fluororesin with water at 24 ° C. is 108 °. The smaller the value, the worse the mold release. The contact angle of the fixing roller release layer that can be used in the actual machine is limited by the properties of the toner in the actual machine and the use of the release material, and is preferably 100 ° or more. The contact angle was judged to be good when the contact angle was 100 ° or more, and poor when it was less than 100 °.
また、コート材料板を組み込み、リングオンディスク摩耗評価する。リングの表面を表面粗さＲａが０．６μｍになるように研摩し、回転速度を５０ｍ／ｍｉｎで回転させる。その際の圧力は２ＭＰａに設定し、２００℃の周囲温度下で３ｈされ、前後の重量変化からコート材料の摩耗深さを評価した。定着ローラは摩耗すると、紙への圧力が弱くなり、トナーの定着が悪くなる。また、金型では寸法が変化する弊害がある。そのため、摩耗深さ２０μｍ以下を良好とし、２０μｍより大きな摩耗は不良と判定した。 In addition, a coating material plate is incorporated to evaluate ring-on-disk wear. The surface of the ring is polished so that the surface roughness Ra is 0.6 μm, and rotated at a rotation speed of 50 m / min. The pressure at that time was set to 2 MPa, and the pressure was set at 3 ° C. for 3 hours at an ambient temperature of 200 ° C., and the wear depth of the coating material was evaluated from the weight change before and after. When the fixing roller is worn, the pressure on the paper is weakened, and the fixing of the toner is deteriorated. In addition, there is an adverse effect that the dimensions change in the mold. Therefore, the wear depth of 20 μm or less was considered good, and wear larger than 20 μm was determined to be defective.
表１より、実施例１〜７はいずれも離型性、耐摩耗性のよい離型層が得られる。これに対して、比較例１はカーボン繊維を含まないため耐摩耗性が悪く、比較例２は黒鉛系のカーボン繊維の含有量が１０重量％と多いために離型性が悪く、比較例３は、炭素系のカーボン繊維を用いているために離型性が悪い。また比較例４は架橋しないＰＴＦＥを用いているために耐摩耗性が悪く、比較例５は、黒鉛系のカーボン繊維の含有量が３重量％と少ないために耐摩耗性が悪い。さらに比較例７は黒鉛系のカーボン繊維を用いているもの、繊維長が７０μｍを用いているために離型性が悪い。 From Table 1, in Examples 1 to 7, release layers having good release properties and wear resistance can be obtained. On the other hand, Comparative Example 1 does not contain carbon fibers and thus has poor wear resistance, and Comparative Example 2 has a large amount of graphite-based carbon fibers of 10% by weight, so that the releasability is poor. Has poor releasability due to the use of carbon-based carbon fibers. Comparative Example 4 has poor wear resistance because it uses PTFE that is not crosslinked, and Comparative Example 5 has poor wear resistance because the content of graphite-based carbon fibers is as small as 3% by weight. Further, Comparative Example 7 uses graphite-based carbon fibers, and the fiber length is 70 μm, so that the releasability is poor.
このように、本発明の離型層によれば、前述のように離型性及び耐摩耗性が良い理由として、離型層は電離性放射線を照射して架橋させて硬質ゴムのように柔軟性を有しかつ硬度を有する所謂架橋ＰＴＦＥと紙の繰り返しの通過などで加わる応力に耐えるために高弾性体である繊維長が５０μｍ以下の黒鉛系のカーボン繊維を、ＰＦＡのフィルム内に混和してなるものである。 As described above, according to the release layer of the present invention, as described above, the release layer and the abrasion resistance are good. As a result, the release layer is irradiated with ionizing radiation and crosslinked to be flexible like a hard rubber. In order to withstand the stress applied by repeated passage of paper and the so-called cross-linked PTFE, the carbon fiber of high elasticity and fiber length of 50 μm or less is mixed in the PFA film. It will be.
また本発明では、離型層の厚さが５μｍ〜１００μｍの範囲で製作する。その理由は、離型層の厚さが５μｍ以下の場合には、離型層が薄過ぎて均一な平滑面が得られないばかりか、充分な機械的な強度が得られず耐摩耗性が悪くなる。離型層３の厚さが１００μｍ以上になると、ヒータランプからの熱により離型層上の未定着トナー層を記録紙に付着する場合、ヒータランプからの熱が離型層の厚さにより熱伝導性が悪くなり、ヒータランプ熱が未定着トナー層に均一に伝達されないから、印刷むらになり記録紙の画質が悪くなる。 Moreover, in this invention, it manufactures in the range whose thickness of a mold release layer is 5 micrometers-100 micrometers. The reason is that when the thickness of the release layer is 5 μm or less, the release layer is too thin to obtain a uniform smooth surface, and sufficient mechanical strength cannot be obtained, resulting in wear resistance. Deteriorate. When the thickness of the release layer 3 is 100 μm or more, when the unfixed toner layer on the release layer adheres to the recording paper by the heat from the heater lamp, the heat from the heater lamp is heated by the thickness of the release layer. The conductivity deteriorates and the heater lamp heat is not uniformly transmitted to the unfixed toner layer, resulting in uneven printing and poor image quality of the recording paper.
なお、上述の実施例では、静電塗装により塗布した後、焼き付ける例を説明したがスプレー塗装を行う場合には、架橋ＰＴＦＥ粉末１５重量％と平均粒径０．４μｍのＰＦＡ重合粒子が分散されたＰＦＡディスパージョン（ダイキン工業社製、ＡＤ２ＣＲ）を粒子量で７５重量％混合し、この希釈粘度調整したディスパージョンを先のプライマー層の上に、スプレー塗装し、８０℃で１５分間乾燥後、２５０℃で３０分間２次乾燥し、更に３５０℃で３０分間の焼成を行って、定着ロール等を作製する。このようにして、最外層としての離型層（乾燥膜厚として３０μｍ）を形成する。 In the above-described embodiment, an example of baking after applying by electrostatic coating has been described. However, when spray coating is performed, 15% by weight of crosslinked PTFE powder and PFA polymer particles having an average particle size of 0.4 μm are dispersed. PFA dispersion (Daikin Kogyo Co., Ltd., AD2CR) was mixed at 75% by weight, and this dispersion viscosity-adjusted dispersion was spray-coated on the primer layer, dried at 80 ° C. for 15 minutes, Secondary drying is performed at 250 ° C. for 30 minutes, and further, baking is performed at 350 ° C. for 30 minutes to prepare a fixing roll or the like. In this way, a release layer (dry film thickness of 30 μm) is formed as the outermost layer.
１ アルミニウム芯金
２ プライマー層
３ 離型層
1
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013147224A1 (en) * | 2012-03-30 | 2013-10-03 | 住友電工ファインポリマー株式会社 | Resin-releasing jig |
| CN104718502A (en) * | 2012-08-02 | 2015-06-17 | 佳能株式会社 | Fixing member, method for producing same, fixing device and image forming device |
| WO2019225434A1 (en) * | 2018-05-22 | 2019-11-28 | ダイキン工業株式会社 | Polytetrafluoroethylene composition |
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| JP5810689B2 (en) | 2011-07-07 | 2015-11-11 | 富士ゼロックス株式会社 | Fixing apparatus and image forming apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013147224A1 (en) * | 2012-03-30 | 2013-10-03 | 住友電工ファインポリマー株式会社 | Resin-releasing jig |
| JPWO2013147224A1 (en) * | 2012-03-30 | 2015-12-14 | 住友電工ファインポリマー株式会社 | Resin releasability jig |
| US9339951B2 (en) | 2012-03-30 | 2016-05-17 | Sumitomo Electric Fine Polymer, Inc. | Resin-releasing jig |
| CN104718502A (en) * | 2012-08-02 | 2015-06-17 | 佳能株式会社 | Fixing member, method for producing same, fixing device and image forming device |
| EP2881800A4 (en) * | 2012-08-02 | 2016-06-15 | Canon Kk | Fixing member, method for producing same, fixing device and image forming device |
| US9465338B2 (en) | 2012-08-02 | 2016-10-11 | Canon Kabushiki Kaisha | Fixing member, method for manufacturing the same, fixing apparatus, and image forming apparatus |
| CN104718502B (en) * | 2012-08-02 | 2017-02-01 | 佳能株式会社 | Fixing member, method for producing same, fixing device and image forming device |
| WO2019225434A1 (en) * | 2018-05-22 | 2019-11-28 | ダイキン工業株式会社 | Polytetrafluoroethylene composition |
| CN112154183A (en) * | 2018-05-22 | 2020-12-29 | 大金工业株式会社 | Polytetrafluoroethylene composition |
| CN112154183B (en) * | 2018-05-22 | 2022-08-16 | 大金工业株式会社 | Polytetrafluoroethylene composition |
| CN115608590A (en) * | 2022-11-04 | 2023-01-17 | 江苏贝尔机械有限公司 | PTFE spraying process for storing inner wall of viscous material bin |
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