JP5073222B2 - Carbon fiber monofilament sheets and their applications - Google Patents
Carbon fiber monofilament sheets and their applications Download PDFInfo
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Description
本発明は、炭素繊維モノフィラメントを単糸として使用した炭素繊維製シートとその用途に関する。 The present invention relates to a carbon fiber sheet using a carbon fiber monofilament as a single yarn and its use.
炭素繊維は、金属等に比べて比重が小さく、弾性率が高く、熱伝導性があり、耐薬品性や耐熱性に優れ、生体適合性があり、導電性や電磁波シールド性などにも優れるという利点があるため、非常に幅広い用途に使用されている。 Carbon fiber has a lower specific gravity than metals, high modulus of elasticity, thermal conductivity, excellent chemical resistance and heat resistance, biocompatibility, and excellent conductivity and electromagnetic shielding properties. Due to its advantages, it is used in a very wide range of applications.
一般に、炭素繊維はマルチフィラメント糸として供給され、一方向繊維や織物にして使用されることが多く、繊維の引張強度や引張弾性率は大きいが、ループ強度や結節強度が小さく、折れやすいという欠点がある。そのため、布帛形成には、例えば特許文献１に示されるように、通常、１Ｋ〜２４Ｋ程度の繊維束としてプリプレグ製造用の織物などに使用されることが多く、炭素繊維モノフィラメントを、単糸として使用したり、厚さ１００μｍ以下のシート状に形成したりすることはなかった。
本発明は、このような炭素繊維を、モノフィラメント単独として使用し、全く新規なシート及び用途を開発することを課題とする。 An object of the present invention is to use such a carbon fiber as a monofilament alone to develop a completely new sheet and application.
本発明では、炭素繊維を、直径１０μｍ以下のモノフィラメントとして使用し、これを単糸として、１インチ間に５〜１５００本の密度で有する炭素繊維製シートとすることによって、上記課題を解決した。 In the present invention, the above-mentioned problems have been solved by using carbon fibers as monofilaments having a diameter of 10 μm or less and using them as single yarns to form carbon fiber sheets having a density of 5 to 1500 per inch.
かかる本発明では、厚さ２０μｍ以下というような従来になく極めて薄いシート（モノフィラメントを織編したもの、又は一方向に引き揃えてシート状としたもの等）を得ることが可能であり、かかる超薄シートは、黒色の炭素繊維モノフィラメントからなるため、周囲に同化して、通常では視認できなくなるという意味で、透明性あるシートとなるが、高強度、高弾性率、熱伝導性、Ｘ線透過性、熱線吸収能、吸着能など炭素繊維本来の性能を十分に発揮しうるものである。 In the present invention, it is possible to obtain a very thin sheet (those woven or knitted monofilament or sheet-shaped by aligning in one direction) having a thickness of 20 μm or less. The thin sheet is made of black carbon fiber monofilament, so it becomes assimilated to the surroundings and becomes invisible in the normal sense. However, it has high strength, high elastic modulus, thermal conductivity, and X-ray transmission. The carbon fiber's inherent properties such as properties, heat ray absorption ability and adsorption ability can be fully exhibited.
更に、かかるシートで補強した極薄強化プラスチックは、ＩＴ関連電子機器など超精密分野等で、用途展開が可能となる。例えば、炭素繊維で補強した強化プラスチックを、厚さ０．５ｍｍ以下、特に０．２ｍｍ以下という非常に薄いシートとして得ることも可能である。 Furthermore, the ultra-thin reinforced plastic reinforced with such a sheet can be used in ultra-precision fields such as IT-related electronic devices. For example, it is possible to obtain a reinforced plastic reinforced with carbon fibers as a very thin sheet having a thickness of 0.5 mm or less, particularly 0.2 mm or less.
なお、本発明で使用する炭素繊維モノフィラメントの直径は、１０μｍ以下であればよく、通常３μｍ以上、特に５〜１０μｍ、７〜８μｍ程度であるのが好ましい。 The diameter of the carbon fiber monofilament used in the present invention may be 10 μm or less, and is usually 3 μm or more, particularly about 5 to 10 μm or 7 to 8 μm.
かかる炭素繊維モノフィラメントを用いたシートは、織物であっても、編物であってもよく、レースやネット状のものであってもよい。また、モノフィラメントの一方向引き揃えによるものであってもよい。通常、炭素繊維モノフィラメントを単糸として、１インチ間に５〜１５００本の密度で有するようにするのが好ましく、特に８〜１０００本程度の密度であるのが好ましい。なお、透明性と補強性を兼ね備えたシートとしては、モノフィラメントの密度が、１インチ間に８〜２００本程度の密度であるのが好ましい。 The sheet using such carbon fiber monofilament may be a woven fabric, a knitted fabric, or a lace or net-like one. Further, the monofilament may be aligned in one direction. Usually, it is preferable to have a carbon fiber monofilament as a single yarn so as to have a density of 5 to 1500 per inch, and particularly preferably a density of about 8 to 1000. In addition, as a sheet | seat which has transparency and a reinforcement, it is preferable that the density of a monofilament is a density of about 8 to 200 per inch.
本発明の炭素繊維モノフィラメントからなるシートは、強化プラスチックの補強材として樹脂と複合化して有効に使用できるが、これは、炭素繊維モノフィラメントからなるシートに、例えば、エポキシ樹脂、不飽和ポリエステル、アクリル樹脂等の熱硬化性樹脂や、ナイロン、ポリオレフィン、ポリエステル等の熱可塑性樹脂を含浸させ、又は積層して、極薄のシート状の強化プラスチックとすることができるのである。また、そのプリプレグを用いてパイプ状など３次元形状を有する強化プラスチック製品を得ることも可能である。なお、かかる強化プラスチックの製造に当たっては、炭素繊維モノフィラメントを前記密度で一方向に引き揃えて、補強材として使用することもできる。 The sheet comprising the carbon fiber monofilament of the present invention can be effectively used by being combined with a resin as a reinforcing material for a reinforced plastic. It is possible to obtain a very thin sheet-like reinforced plastic by impregnation or lamination with a thermosetting resin such as nylon, polyolefin, or polyester. It is also possible to obtain a reinforced plastic product having a three-dimensional shape such as a pipe using the prepreg. In manufacturing such a reinforced plastic, carbon fiber monofilaments can be aligned in one direction at the above-mentioned density and used as a reinforcing material.
炭素繊維モノフィラメントを一方向に引き揃えたシートは、一層で使用しても、二層以上の積層材として使用してもよいが、二層以上積層する場合には、第一層と第二層のモノフィラメントの引き揃え方向が、３０〜９０度となるように角度変化させて積層することで、擬似等方的な強度を得ることができ、好ましい。更に、透明性ある製品を得るためには、二〜四層であるのが好ましい。 A sheet in which carbon fiber monofilaments are aligned in one direction may be used as a single layer or as a laminate of two or more layers. When two or more layers are laminated, the first layer and the second layer are used. It is preferable that the monofilaments are aligned at different angles so that the direction in which the monofilaments are aligned is 30 to 90 degrees, whereby quasi-isotropic strength can be obtained. Furthermore, in order to obtain a transparent product, it is preferable to have two to four layers.
本発明のシートは、炭素繊維からなるため、寸法安定性に優れ、機械的強度にも優れ、また、生体親和性、化学安定性、耐熱性、導電性など優れた特性を有するものである。しかも、炭素繊維を非常に細いモノフィラメントとして使用しているため、目視できないような超薄の布帛とすることができ、その結果、生体適合性繊維材料として、細胞成長を阻害せず、超高強度で、かつ柔軟性を有し、しかもその使用を目視的に感知させない状態で、非常に有効に使用可能となる。
また、本発明の厚さ２０μｍ以下というような超薄シート（布帛又は炭素繊維モノフィラメントの一方向引き揃え材）で補強した強化プラスチックは、厚さ０．５ｍｍ以下というような薄さでも、適度の強度を有し、しかも電導性、電波遮蔽性、熱線吸収能、Ｘ線透過性、熱伝導性、吸着能などの機能性あるシートとして、ＩＴ関連電子機器など超精密機器の分野等で、広く使用されるものとなる。
Since the sheet of the present invention is made of carbon fiber, it has excellent dimensional stability, excellent mechanical strength, and excellent properties such as biocompatibility, chemical stability, heat resistance, and conductivity. Moreover, since carbon fibers are used as very thin monofilaments, they can be made into an ultra-thin fabric that cannot be visually observed. As a result, the biocompatible fiber material does not inhibit cell growth and has an ultra-high strength. In addition, it is flexible and can be used very effectively without visually detecting its use.
Further, the reinforced plastic reinforced with an ultra-thin sheet (fabric or carbon fiber monofilament unidirectional alignment material) having a thickness of 20 μm or less according to the present invention is suitable even if the thickness is 0.5 mm or less. As a functional sheet with strength, electrical conductivity, radio wave shielding, heat ray absorption ability, X-ray permeability, thermal conductivity, adsorption ability, etc. To be used.
実施例１
直径７μｍの炭素繊維モノフィラメントを、経緯にそれぞれ１２本／インチの密度で平織組織の織物とした。この織物は、１０名のモニター確認によって、１０名全てがその存在を視認できなかった。
この織物を生体適合性ある癒着防止膜として使用した。
Example 1
Carbon fiber monofilaments having a diameter of 7 μm were made into plain woven fabrics with a density of 12 / inch each. As for this woven fabric, all 10 persons were not able to visually recognize the presence by 10 monitor confirmation.
This fabric was used as a biocompatible anti-adhesion membrane.
実施例２
直径７μｍの炭素繊維モノフィラメントを、経緯にそれぞれ２４本／インチの密度で平織組織の織物とした。
この織物に、シリコン樹脂を含浸して、厚さ０．２ｍｍの強化プラスチックとした。これは耐熱性ある電導シートとして効果的に使用できた。
Example 2
Carbon fiber monofilaments with a diameter of 7 μm were made into plain weave fabrics with a density of 24 / inch each.
This woven fabric was impregnated with silicon resin to obtain a reinforced plastic having a thickness of 0.2 mm. This could be effectively used as a heat-resistant conductive sheet.
実施例３
直径７μｍの炭素繊維モノフィラメントを、経緯にそれぞれ１ｍｍピッチ（１ｃｍ間に１０本）の密度で綾織組織の織物とした。この織物も、その存在を視認できない薄布となり、実施例１のものと同様、生体適合性ある癒着防止膜として使用できた。
更に、同様の炭素繊維モノフィラメントを使用して、経緯にそれぞれ０．５ｍｍピッチ（１ｃｍ間に２０本）及び０．２ｍｍピッチ（１ｃｍ間に５０本）の密度で、綾織物を製造した。これらは、シリコン樹脂を含浸して、強化プラスチックとして、実用化できた。
Example 3
Carbon fiber monofilaments having a diameter of 7 μm were made into a twill-woven fabric with a density of 1 mm pitch (10 per cm). This woven fabric also became a thin fabric whose presence could not be visually confirmed, and, like the fabric of Example 1, could be used as a biocompatible adhesion preventing film.
Furthermore, using the same carbon fiber monofilament, twill woven fabrics were manufactured at a density of 0.5 mm pitch (20 per cm) and 0.2 mm pitch (50 per 1 cm), respectively. These were impregnated with silicon resin and could be put into practical use as reinforced plastics.
実施例４
直径７μｍの炭素繊維モノフィラメントを、経緯にそれぞれ１ｍｍピッチ（１ｃｍ間に１０本）、０．５ｍｍピッチ（１ｃｍ間に２０本）、０．２ｍｍピッチ（１ｃｍ間に５０本）の密度で、平織物とし、それぞれに、母材樹脂として１５−２０重量％に溶剤希釈したアクリルポリウレタン樹脂（大日本塗料製のＶトップクリア）を含浸した後、常温で２０時間硬化させて、厚さ５９−８４μm の炭素繊維／樹脂極薄シートを得た。
本発明に従った布帛を補強材とした、極薄強化プラスチックは、ヤング率が大きく、熱伝導性（放熱性）にも優れていた。しかし、比較例の樹脂シートでは、良好な放熱性が得られなかった
なお、製造した強化プラスチックの種類を下記に示す。
. 平織物 強化プラスチック（樹脂シート）
. ピッチ（ｍｍ） 厚さ（μｍ）
. １ ５９、６０、６１、６５、６３、６７
. ０．５ ７１、７０、６９、７３、７５、７１
. ０．５ ７１、７０、６９、７３、７５、７１
. 布帛なし（比較例） ５０、４９、５１、４７、４８、４８
Example 4
Carbon fiber monofilaments with a diameter of 7 μm are plain fabrics with a density of 1 mm pitch (10 per 1 cm), 0.5 mm pitch (20 per 1 cm) and 0.2 mm pitch (50 per 1 cm), respectively. Each was impregnated with 15-20% by weight of acrylic polyurethane resin (V Top Clear, manufactured by Dainippon Paint) as a base resin, and then cured at room temperature for 20 hours to obtain a thickness of 59-84 μm. A carbon fiber / resin ultrathin sheet was obtained.
The ultrathin reinforced plastic using the fabric according to the present invention as a reinforcing material has a large Young's modulus and excellent thermal conductivity (heat dissipation). However, in the resin sheet of the comparative example, good heat dissipation was not obtained. The types of manufactured reinforced plastics are shown below.
. Plain woven reinforced plastic (resin sheet)
. Pitch (mm) Thickness (μm)
1 59, 60, 61, 65, 63, 67
0.5 71, 70, 69, 73, 75, 71
0.5 71, 70, 69, 73, 75, 71
No fabric (comparative example) 50, 49, 51, 47, 48, 48
実施例５
直径７μｍの炭素繊維モノフィラメントを０．５−０．１ｍｍピッチで一方向に引揃えたＵＤ材を用いて、母材樹脂としてエポキシ樹脂（ジャパン エポキシ レジン社製のエピコート８２８)、硬化剤として脂環式ポリアミン(ジャパン エポキシ レジン社製のエピキュア１１３）を３２ｐｈｒ及び柔軟剤を配合したものを、１０−１５重量％に溶剤希釈し、前記ＵＤ材に含浸させた後、４５℃にて４０分間保持することで、Ｂステージ化した炭素繊維モノフィラメントプリプレグを得た。このプリプレグを±９０度方向に４層積層させて、１６０℃、１−２ＭPaの低圧で真空バグ成形することにより、炭素繊維／樹脂極薄積層体を得た。
０．１ｍｍピッチ材による極薄積層体は、精密回転体の微小治具の補強部材として有用であった。
製造した積層体の種類を下記に示す。
. フィラメント引き揃え 積層体
. ピッチ（ｍｍ） 厚さ（μｍ）
. ０．５ １９０、１８０、２０８、２１０、１９９、２２０
. ０．２５ ２４１、２３２、２２８、２４０、２３９、２４３
. ０．１ ３０８、２９９、３１０、３１５、２８８、２８５
Example 5
Using a UD material in which carbon fiber monofilaments having a diameter of 7 μm are aligned in one direction at a pitch of 0.5 to 0.1 mm, an epoxy resin (Epicoat 828 manufactured by Japan Epoxy Resin Co., Ltd.) is used as a base resin, and an alicyclic ring is used as a curing agent. Formula Polyamine (Epicure 113 manufactured by Japan Epoxy Resin Co., Ltd.) blended with 32 phr and a softening agent is diluted with a solvent to 10 to 15% by weight, impregnated in the UD material, and then held at 45 ° C. for 40 minutes. Thus, a B-staged carbon fiber monofilament prepreg was obtained. Four layers of this prepreg were laminated in the direction of ± 90 degrees, and vacuum bag forming was performed at 160 ° C. and a low pressure of 1-2 MPa to obtain a carbon fiber / resin ultrathin laminate.
The ultra-thin laminate with a 0.1 mm pitch material was useful as a reinforcing member for a fine jig of a precision rotating body.
The kind of the laminated body manufactured is shown below.
. Filament aligned laminate
. Pitch (mm) Thickness (μm)
0.5 190, 180, 208, 210, 199, 220
0.25 241, 232, 228, 240, 239, 243
0.1 308, 299, 310, 315, 288, 285
実施例６
直径７μｍの炭素繊維モノフィラメントによる平織クロス（ピッチ：１ｍｍと２ｍｍ）１層を用いて、母材樹脂として１５−２０重量％に溶剤希釈したアクリルポリウレタン樹脂（大日本塗料製のＶトップクリア）を含浸後、常温で２０時間硬化させることで、厚さ５１μｍと５４μｍの炭素繊維モノフィラメント平織クロス／樹脂極薄シートを得た。
次表に示したヤング率（引張弾性率）にみられるように、樹脂のみの極薄シート（比較例）と比較して補強効果が認められた。また、ヘイズ値は何れも比較例同様、１０％以下を維持し透明性が確保されていた。
Example 6
One layer of plain weave cloth (pitch: 1mm and 2mm) made of carbon fiber monofilament with a diameter of 7μm, impregnated with acrylic polyurethane resin (V Top Clear made by Dainippon Paint) diluted with solvent to 15-20% by weight as the base resin Thereafter, curing was performed at room temperature for 20 hours to obtain a carbon fiber monofilament plain weave cloth / resin ultrathin sheet having a thickness of 51 μm and 54 μm.
As seen in the Young's modulus (tensile modulus) shown in the following table, a reinforcing effect was recognized as compared with an ultrathin sheet made of resin only (Comparative Example). Further, the haze value was maintained at 10% or less as in the comparative example, and transparency was ensured.
． 試験体 厚さ(μｍ) ヘイズ値(%) ヤング率(MPa)
炭素繊維モノフィラメント平織クロス 51 2.9 2120
（１ｍｍピッチ）／透明樹脂シート
炭素繊維モノフィラメント平織クロス 54 2.6 1290
（２ｍｍピッチ）／透明樹脂シート
透明樹脂シート（比較例） 64 2.2 1090
. Specimen thickness (μm) Haze value (%) Young's modulus (MPa)
Carbon fiber monofilament plain weave cloth 51 2.9 2120
(1mm pitch) / Transparent resin sheet
Carbon fiber monofilament plain weave cloth 54 2.6 1290
(2mm pitch) / Transparent resin sheet
Transparent resin sheet (comparative example) 64 2.2 1090
実施例７
直径7μmの炭素繊維モノフィラメントを０．５ｍｍピッチ又は０．３ｍｍピッチで一方向に引揃えたＵＤ材を用いて、１５−２０重量％に溶剤希釈したアクリルポリウレタン樹脂（ロックペイント製のマルチトップクリヤーMR）を含浸後、６０℃で１０時間硬化させることで、厚さ４９μｍ又は５１μｍのUD炭素繊維／樹脂極薄シートを得た。本極薄シートは０．５ｍｍピッチ又は０．３ｍｍピッチのUD炭素繊維モノフィラメント材を用いて補強しているため、その外観は透明性を維持しており、かつ次表に示した繊維軸方向の引張試験により得られたヤング率（引張弾性率）にみられるように、樹脂のみの極薄シート（比較例）と比較して補強効果が認められた。透明性についてもヘイズ値が示すとおり何れも確保されていた。
Example 7
Acrylic polyurethane resin (multi-top clear MR made by Rock Paint) diluted with solvent to 15-20% by weight using a UD material in which carbon fiber monofilaments with a diameter of 7 μm are aligned in one direction at a pitch of 0.5 mm or 0.3 mm. ) And then cured at 60 ° C. for 10 hours to obtain a UD carbon fiber / resin ultrathin sheet having a thickness of 49 μm or 51 μm. Since this ultra-thin sheet is reinforced with a UD carbon fiber monofilament material with a pitch of 0.5 mm or 0.3 mm, its external appearance is kept transparent, and the fiber axis direction shown in the following table is maintained. As seen in the Young's modulus (tensile modulus) obtained by the tensile test, a reinforcing effect was recognized as compared with the ultrathin sheet (comparative example) made only of resin. As for the transparency, any haze value was ensured.
. 試験体 厚さ(μm) ヘイズ値(%) ヤング率(MPa)
一方向炭素繊維モノフィラメント 49 3.8 1260
(0.5mmピッチ)／透明樹脂シート
一方向炭素繊維モノフィラメント 51 4.1 1780
(0.3mmピッチ)／透明樹脂シート
透明樹脂シート（比較例） 52 2.2 990
Specimen thickness (μm) Haze value (%) Young's modulus (MPa)
Unidirectional carbon fiber monofilament 49 3.8 1260
(0.5mm pitch) / Transparent resin sheet
Unidirectional carbon fiber monofilament 51 4.1 1780
(0.3mm pitch) / Transparent resin sheet
Transparent resin sheet (comparative example) 52 2.2 990
実施例８
直径7μmの炭素繊維モノフィラメントを０．５ｍｍピッチで一方向に引揃えたＵＤ材を第１層とし、第２層は第１層と直交（若しくは±３０〜４５度方向でも良い）するように引揃えることにより得られた炭素繊維モノフィラメント異方向引揃２層（同様に３層以上も可であるが極薄かつ透明性を確保するためには２〜４層が好ましい）積層材を用いて、１５〜２０重量％に溶剤希釈した透明アクリルポリウレタン樹脂（ロックペイント マルチトップクリヤーMR）を含浸製膜後、６０℃で１０時間硬化させることで、厚さ５５〜６２μｍの異方向引揃２層炭素繊維モノフィラメント／樹脂透明極薄シートを得た。繊維軸方向（０度方向）と繊維軸と直交方向（９０度方向）の引張試験を行った。それぞれの引張強度を次表に示す。この表に見られるように、一方向繊維／樹脂シート材は、強度に異方性が見られるのに対して、異方向引揃２層繊維／樹脂シート材には、０、９０度方向において強度に異方性が認められなかった。また、ヘイズ値についても比較例（実施例７の比較例−透明樹脂シート−参照）同様、１０％以下を維持し透明性が確保されていた。
Example 8
A UD material in which carbon fiber monofilaments having a diameter of 7 μm are aligned in one direction at a pitch of 0.5 mm is used as the first layer, and the second layer is drawn so as to be orthogonal to the first layer (or in the direction of ± 30 to 45 degrees). Using a laminated material obtained by aligning carbon fiber monofilaments in two different directions (similarly three or more layers are preferable, but 2 to 4 layers are preferable in order to ensure ultrathinness and transparency), After impregnating a transparent acrylic polyurethane resin (Rock Paint Multi-Top Clear MR) diluted with a solvent to 15 to 20% by weight and then curing at 60 ° C. for 10 hours, a double-layered carbon with a different orientation of 55 to 62 μm in thickness is obtained. A fiber monofilament / resin transparent ultrathin sheet was obtained. Tensile tests were conducted in the fiber axis direction (0 degree direction) and in the direction orthogonal to the fiber axis (90 degree direction). Each tensile strength is shown in the following table. As seen in this table, the unidirectional fiber / resin sheet material has anisotropy in strength, whereas the different direction aligned two-layer fiber / resin sheet material has a 0, 90 degree direction. There was no anisotropy in strength. Moreover, about the haze value, 10% or less was maintained and transparency was ensured similarly to the comparative example (refer comparative example of Example 7-transparent resin sheet-).
． 試験体 厚さ ヘイズ値 引張強度 引張強度
(μｍ) (%) (0度/MPa) (90度/MPa)
異方向引揃２層炭素繊維モノフィラメント 55 5.1 32.5 31.8
(0. 5mmピッチ)／透明樹脂シート
一方向炭素繊維モノフィラメント 49 3.8 35.8 7.8
(0.5mmピッチ)／透明樹脂シート
. Specimen thickness Haze value Tensile strength Tensile strength
(μm) (%) (0 degree / MPa) (90 degree / MPa)
Different direction assembling double layer carbon fiber monofilament 55 5.1 32.5 31.8
(0.5mm pitch) / Transparent resin sheet
Unidirectional carbon fiber monofilament 49 3.8 35.8 7.8
(0.5mm pitch) / Transparent resin sheet
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