JPH0393613A - Pitch-based carbon film tape and production thereof - Google Patents
Pitch-based carbon film tape and production thereofInfo
- Publication number
- JPH0393613A JPH0393613A JP1227740A JP22774089A JPH0393613A JP H0393613 A JPH0393613 A JP H0393613A JP 1227740 A JP1227740 A JP 1227740A JP 22774089 A JP22774089 A JP 22774089A JP H0393613 A JPH0393613 A JP H0393613A
- Authority
- JP
- Japan
- Prior art keywords
- pitch
- tape
- carbon film
- based carbon
- sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000009987 spinning Methods 0.000 claims abstract description 10
- 238000004804 winding Methods 0.000 claims abstract description 10
- 238000010000 carbonizing Methods 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 238000007664 blowing Methods 0.000 abstract description 5
- 238000007711 solidification Methods 0.000 abstract description 3
- 230000008023 solidification Effects 0.000 abstract description 3
- 239000011295 pitch Substances 0.000 description 62
- 239000010408 film Substances 0.000 description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011302 mesophase pitch Substances 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 150000001454 anthracenes Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000003570 air Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、テープ状ピッチ系炭素フィルムおよびその製
造方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a tape-shaped pitch-based carbon film and a method for producing the same.
なお、本明細書においては、“炭化”なる概念は、狭義
の“炭化”のみならず、“黒鉛化”を含む広い概念を意
味するものとする。In this specification, the concept of "carbonization" means not only "carbonization" in a narrow sense but also a broader concept including "graphitization."
従来技術とその問題点 炭素フィルムの用途は、２つのグループに大別される。Conventional technology and its problems The uses of carbon films can be broadly divided into two groups.
（イ） その一つは、炭素フィルム強化炭素複合材料の
強化材としての用途である。従来、ディスクブレーキ、
ロケットノズルなどの部材などとしては、機械的性質、
耐熱特性、軽量性などに優れた炭素繊維強化炭素複合材
料が極めて有用であることが知られている。(b) One of them is its use as a reinforcing material for carbon film-reinforced carbon composite materials. Conventionally, disc brakes,
For components such as rocket nozzles, mechanical properties,
It is known that carbon fiber-reinforced carbon composite materials, which have excellent heat resistance and light weight, are extremely useful.
この様な炭素複合材料の製造方法のτつに、炭素繊維成
形物と熱可塑性樹脂とを交互にまたは適切・な割合で積
層させた後、含浸炭化或いはさらに黒鉛化する方法があ
る。One of the methods for producing such a carbon composite material is a method in which a carbon fiber molded product and a thermoplastic resin are laminated alternately or in an appropriate ratio, and then impregnated carbonization or further graphitization is performed.
この場合に、若し炭素フィルムを炭素繊維に代えて使用
することができれば、積層密度が増大し、且つ樹脂との
密着性が向上して、炭素複合材料の特性を飛躍的に改善
させ得るものと期待されている。In this case, if carbon film can be used in place of carbon fiber, the lamination density will increase and the adhesion to the resin will improve, dramatically improving the properties of the carbon composite material. It is expected that
（ロ） 他の一つは、二次電池の電極としての用途であ
る。二次電池は、充電により電力貯蔵機能を有するので
、今後その有用性は、より一層増大するものと考えられ
ている。(b) Another application is as an electrode for secondary batteries. Since secondary batteries have a power storage function when charged, their usefulness is expected to further increase in the future.
この様な二次電池の電極用炭素材としては、従来フィル
ム状のグラファイト層間にドナー型、アクセプター型ま
たは共有結合型のインターカラントが挿入されたフィル
ム状グラファイト層間化合物が知られている。As carbon materials for electrodes of such secondary batteries, film-like graphite intercalation compounds in which donor-type, acceptor-type, or covalently bonded intercalants are inserted between film-like graphite layers are conventionally known.
上記の炭素フィルム或いはグラファイトフィルムは、有
機高分子原料をフィルム化した後、縦横にローラー延伸
し、薄膜化した後、フィルムの熱処理により製造されて
いる。また、グラファイトフィルムの場合には、天然グ
ラファイトから削り出しにより、製造することもできる
。しかしながら、これの方法により製造された炭素フィ
ルムおよびグラファイトフィルムは、高価であるため、
実用的でないという問題点がある。The above-mentioned carbon film or graphite film is manufactured by forming an organic polymer raw material into a film, stretching the film with rollers lengthwise and crosswise to make it thin, and then heat-treating the film. Further, in the case of a graphite film, it can also be manufactured by cutting out natural graphite. However, carbon films and graphite films produced by this method are expensive, so
The problem is that it is not practical.
問題点を解決するための手段
本発明者は、上記の如き技術の現状に鑑みて思索を重ね
た結果、従来炭素フィルムの製造原料として使用された
ことのないピッチから炭素フィルムを製造することを着
想し、その実施を試みた。Means for Solving the Problems As a result of repeated speculations in view of the current state of technology as described above, the present inventor has devised the idea of manufacturing a carbon film from pitch, which has never been used as a raw material for manufacturing carbon films. I came up with an idea and tried to implement it.
しかるに、ピッチは、固化状態では、非常に脆くなるた
め、有機高分子原料の場合のように押出し法、チューブ
ラー法などの方法により、広幅のフィルムを製造するこ
とは、不可能である。すなわち、例えば、押出しにより
形成したフィルム状ピッチを固化後に延伸して薄膜化す
ることは出来ないので、溶融押出し時に引張伸長し、薄
膜化しなければならない。しかしながら、この際、ピッ
チの有する高い表面張力の故に、ネックダウンが著しく
、広幅のフィルムを形成することは、極めて困難である
ことが判明した。However, since pitch becomes extremely brittle in a solidified state, it is impossible to produce a wide film using methods such as extrusion and tubular methods, as in the case of organic polymer raw materials. That is, for example, since it is not possible to stretch a film-like pitch formed by extrusion into a thin film after solidification, it must be stretched during melt extrusion to become a thin film. However, in this case, it was found that due to the high surface tension of the pitch, neckdown was significant and it was extremely difficult to form a wide film.
本発明者は、さらに鋭意、研究を重ねた結果、スリット
型ノズルから溶融押出され、巻取のために牽引されつつ
あるシート状ピッチが十分に固イヒし始める前に、シー
ト状ピッチの幅方向両端面に特定方向の高速気流を吹付
けて、シート状ピッチを幅方向に広げる分力を作用させ
る場合には、広幅のテープ状ピッチ系ピッチフィルムが
得られることを見出した。そして、このテープ状ピッチ
系ピッチフィルムを不融化し、炭化することにより、ピ
ッチを原料とするテープ状ピッチ系炭素フィルムを得る
ことに初めて成功した。As a result of further intensive research, the present inventor discovered that before the sheet-like pitch that is being melted and extruded from the slit nozzle and being pulled for winding begins to harden sufficiently, the width direction of the sheet-like pitch is It has been found that a wide tape-like pitch-based pitch film can be obtained when a high-speed airflow in a specific direction is applied to both end faces to apply force that spreads the sheet-like pitch in the width direction. By making this tape-like pitch-based pitch film infusible and carbonizing it, we succeeded for the first time in obtaining a tape-like pitch-based carbon film using pitch as a raw material.
すなわち、本発明は、下記のテープ状ピッチ系炭素フィ
ルムおよびその製造方法を提供するものである：
■ 厚さが１０〜４０μｍのテープ状ピッチ系炭素フィ
ルム。That is, the present invention provides the following tape-like pitch-based carbon film and its manufacturing method: (1) A tape-like pitch-based carbon film having a thickness of 10 to 40 μm.
■ 紡糸用ピッチをスリット型ノズルから押出し、且つ
押出された面状ピッチを巻取装置に牽引して巻取り、該
ピッチを不融化し、炭化するテープ状ピッチ系炭素フィ
ルムの製造方法であって、牽引により幅が減少しつつあ
る該面状ピッチの幅方向両端面近傍に、且つスリット中
央点を通るスリット長さ方向の面に垂直な仮゜想面に対
称な方向に、該面状ピッチが十分に固化する前に、外向
成分および下向成分を有する気流を吹き付けてテープ状
ピッチフィルムを製造し、これを不融化し、炭化するこ
とを特徴とするテープ状ピッチ系炭素フィルムの製造方
法。(2) A method for producing a tape-like pitch-based carbon film, which comprises extruding pitch for spinning from a slit-type nozzle, pulling the extruded planar pitch into a winding device, winding it up, infusibleizing the pitch, and carbonizing the pitch. , near both end faces in the width direction of the planar pitch whose width is decreasing due to traction, and in a direction symmetrical to an imaginary plane perpendicular to the plane in the longitudinal direction of the slit passing through the center point of the slit. A method for producing a tape-shaped pitch-based carbon film, which comprises: producing a tape-shaped pitch film by blowing an air stream having an outward component and a downward component before the carbon is sufficiently solidified; .
■ 仮想面に対称に幅方向両端面近傍に少くとも２ケ所
からシート状ピッチの両面に気流を吹付ける請求項（２
）に記載のテープ状ピッチ系炭素フィルムの製造方法。■Claim (2) in which air currents are blown onto both sides of the sheet-like pitch from at least two locations near both end faces in the width direction symmetrically with respect to a virtual plane.
) The method for producing a tape-shaped pitch-based carbon film.
■ 吹付ける気流の温度が２００〜４００℃である請求
項（２）または（３）に記載のテープ状ピッチ系炭素フ
ィルムの製造方法。(2) The method for producing a tape-shaped pitch-based carbon film according to claim (2) or (3), wherein the temperature of the air stream to be blown is 200 to 400°C.
以下必要に応じて図面を参照しつつ、本発明をより詳細
に説明する。第１図は、本発明方法を実施するための紡
糸装置の概要を示す斜面図であり、第２図は、その正面
図である。また、第３図は、本発明で使用する紡糸装置
のノズルと気流吹出し口とを特に強調して示す概要断面
図である。The present invention will be described in more detail below with reference to the drawings as necessary. FIG. 1 is a perspective view showing an outline of a spinning apparatus for carrying out the method of the present invention, and FIG. 2 is a front view thereof. Moreover, FIG. 3 is a schematic cross-sectional view that particularly emphasizes the nozzle and air outlet of the spinning device used in the present invention.
本発明で使用するピッチは、石炭系および石油系の如何
を問わない。その性状も特に限定されるものではない。The pitch used in the present invention may be coal-based or petroleum-based. Its properties are also not particularly limited.
即ち、等方性ピッチ、メソフエーズピッチ（等方性ピッ
チを含んでいてもよい）の何れをも使用することができ
る。但し、黒鉛化ピッチを製造する場合には、メソフエ
ーズピッチを使用する。That is, either isotropic pitch or mesophase pitch (which may include isotropic pitch) can be used. However, when producing graphitized pitch, mesophase pitch is used.
本発明においては、第１図乃至第３図に示すように、溶
融したピッチを紡糸装置（１）に供給し、押出されたシ
ート状ピッチ（３）を巻取装置（５）に牽引して巻取る
。紡糸装置（１）は、スリット型ノズル（７）から出て
くるシート状ピッチ（３）の幅方向両端面近傍に向けて
且つスリット中央点（Ｃ）を通るスリット長さ方向に垂
直な仮想面（Ｐ）に対称な方向に、外向成分および下向
成分を有する気流を吹き付けるための少くとも２個の気
流吹出し口（９）、（９）を備えている。第３図に示す
装置においては、気流吹出し口は、第１図に示すように
、スリット型ノズル（７）の片面側に２個の気流吹出し
口（９）、（９）と、その反対側面に第１図と同様の配
置で２個の気流吹出し口（９′）、（９′）が設けられ
ている。第１図、第２図および第３図に示すように、ス
リット型ノズル（７）から出て巻取装置（５）に牽引さ
れつつあるシート状ピッチが十分に固化する前に、換言
すれば、スリット型ノズル（７）の直下に位置するシー
ト状ピッチ（３）の両端面部近傍に、気流を吹付けてシ
ート状ピッチを幅方向に広げる分力を作用させることに
より、シート状ピッチのネックダウン現象が抑制されて
、広幅のテープ状ピッチフィルム（１１）が得られる。In the present invention, as shown in FIGS. 1 to 3, molten pitch is supplied to a spinning device (1), and the extruded sheet-like pitch (3) is pulled to a winding device (5). Wind it up. The spinning device (1) spins a virtual plane perpendicular to the length direction of the slit toward the vicinity of both end faces in the width direction of the sheet pitch (3) coming out of the slit type nozzle (7) and passing through the slit center point (C). At least two airflow outlets (9), (9) are provided for blowing airflow having an outward component and a downward component in a direction symmetrical to (P). In the device shown in FIG. 3, the airflow outlets include two airflow outlets (9), (9) on one side of the slit-type nozzle (7), and two airflow outlets (9) on the opposite side, as shown in FIG. Two airflow outlets (9') and (9') are provided in the same arrangement as in FIG. As shown in FIGS. 1, 2 and 3, before the sheet-like pitch emerging from the slit-type nozzle (7) and being pulled by the winding device (5) is sufficiently solidified, in other words, By blowing airflow to the vicinity of both end surfaces of the sheet-like pitch (3) located directly below the slit-type nozzle (7) and applying force to spread the sheet-like pitch in the width direction, the neck of the sheet-like pitch is removed. The down phenomenon is suppressed, and a wide tape-like pitch film (11) is obtained.
吹付け気体は、５０〜１００ｍ／秒程度の高速度で吹付
けることが好ましく、また、吹付け量は、気流吹出し口
（９）１個当り０．４〜０．５Ｕ／分程度とすることが
好ましい。吹付け気流の気体としては、空気、窒素、ガ
ス燃焼廃ガスなどが使用される。その温度は、通常シー
ト状ピッチ（３）が巻取により延伸し得る温度である２
００〜４００℃程度であり、より好ましくは２５０〜３
５０℃程度である。気流吹出し口（９）は、シート状ピ
ッチ（３）の両端面部近傍に両面から気流が吹付けられ
るために、両端面部近傍に少なくとも２か所づつ、合計
少なくとも４か所に形戊することがより好ましい。It is preferable that the blown gas be blown at a high speed of about 50 to 100 m/sec, and the amount of blown gas should be about 0.4 to 0.5 U/min per air outlet (9). is preferred. Air, nitrogen, gas combustion waste gas, etc. are used as the gas for the blown air stream. The temperature is usually 2, which is the temperature at which the sheet-like pitch (3) can be stretched by winding.
The temperature is about 00 to 400°C, more preferably 250 to 3
The temperature is about 50°C. The airflow outlet (9) can be formed in at least four locations in total, at least two locations near both endfaces, so that airflow is blown from both sides near both endfaces of the sheet pitch (3). More preferred.
かくして得られた広幅のテープ状ピッチフィルム（通常
厚さ１２〜５０μｍ程度、幅２〜４５ｍｍ程度）は、炭
素繊維の製造に際して採用されている常法に準じて、不
融化され、炭化され、テープ状ピッチ系炭素フィルムと
なる。例えば、不融化は、酸素雰囲気中２８０〜３４０
℃程度の温度で行なわれる。不融化に要する時間は、シ
ート状ピッチが薄い程、短時間で完了することは言うま
でもない。また、不融化物の炭素化は、窒素、二酸化炭
素、アルゴンなどの雰囲気中で１０００〜２０００℃程
度の温度で行われる。不融化物の黒鉛化を行なう場合に
は、アルゴン雰囲気中で２０００〜３０００℃程度の温
度で行われる。The thus obtained wide tape-shaped pitch film (usually about 12 to 50 μm in thickness and 2 to 45 mm in width) is infusible and carbonized into a tape according to a conventional method used in the production of carbon fibers. It becomes a pitch-based carbon film. For example, infusibility is 280 to 340 in an oxygen atmosphere.
It is carried out at a temperature of about ℃. Needless to say, the thinner the sheet-like pitch is, the shorter the time required for infusibility to be completed. Further, carbonization of the infusible substance is performed at a temperature of about 1000 to 2000°C in an atmosphere of nitrogen, carbon dioxide, argon, or the like. When the infusible material is graphitized, it is carried out at a temperature of about 2000 to 3000° C. in an argon atmosphere.
最終的に得られるテープ状ピッチ系炭素フイルムの厚さ
は、通常１０〜４０μｍ程度である。アスベクト比（幅
／厚さ）は、通常１０〜ｉｏｏｏ程度の範囲内にあるが
、３０〜３００程度のものが最も製造し易い。アスペク
ト比が１０未満の場合には、公知の異形断面の炭素繊維
と性能的に余り大きな相違が無いものとなり、一方、ア
スペクト比が過大となる場合には、テープ状ピッチ系炭
素フィルムに歪みが生じ易く、好ましくない。The thickness of the tape-like pitch-based carbon film finally obtained is usually about 10 to 40 μm. The aspect ratio (width/thickness) is usually within a range of about 10 to iooo, but one with an aspect ratio of about 30 to 300 is easiest to manufacture. If the aspect ratio is less than 10, there will be no significant difference in performance from known carbon fibers with irregular cross sections.On the other hand, if the aspect ratio is too large, the tape-like pitch-based carbon film will be distorted. This is likely to occur and is not desirable.
本発明方法により製造されるテープ状ピッチ系炭素フィ
ルムは、製造条件に応じて、ラジアル型（断面の中心部
から表面部に一定の流れ方向を示すもの）、ランダム型
（断面に特定の流れ方向が認められないもの）、オニオ
ン型（断面がタマネギの様な重層構造を有するもの）な
どの断面配向構造を有している。The tape-shaped pitch-based carbon film produced by the method of the present invention can be of radial type (having a constant flow direction from the center of the cross section to the surface) or random type (having a specific flow direction in the cross section) depending on the manufacturing conditions. It has a cross-sectional orientation structure such as an onion-type (a layered structure with an onion-like cross-section).
発明の効果 本発明によれば、下記の様な顕著な効果が達成される。Effect of the invention According to the present invention, the following remarkable effects are achieved.
（ａ）ピッチを原料とするテープ状ピッチ系炭素フィル
ムが初めて製造可能となった。(a) For the first time, it has become possible to produce a tape-shaped pitch-based carbon film using pitch as a raw material.
（ｂ）気流の吹付けを行わない場合に比して、１．２〜
２倍程度の広幅のテープ状ピッチ系炭素フィルムが製造
できる。(b) Compared to the case where no airflow is sprayed, 1.2~
It is possible to produce a tape-shaped pitch-based carbon film that is about twice as wide.
（ｃ）炭素複合材料の強化用炭素フィルム、二次電池の
電極などとして優れた性能を発揮する。(c) Demonstrates excellent performance as carbon films for reinforcing carbon composite materials, electrodes for secondary batteries, etc.
実施例
以下に参考例及び実施例を示し、本発明の特徴とすると
ころをより一層明確にする。EXAMPLES Reference examples and examples are shown below to further clarify the features of the present invention.
参考例１
軟化点１００℃、キノリン不溶分０．２％、ベンゼン不
溶分３０％のコールタールピッチに２倍量の水素化アン
トラセン油を加え、４３０℃で６０分間加熱し、さらに
減圧下３００℃で水素化アントラセン油を除去して還元
ピッチを得た。Reference Example 1 Double amount of hydrogenated anthracene oil was added to coal tar pitch with a softening point of 100°C, 0.2% quinoline insoluble content, and 30% benzene insoluble content, heated at 430°C for 60 minutes, and further heated to 300°C under reduced pressure. The hydrogenated anthracene oil was removed to obtain reduced pitch.
次いで、この還元ピッチに窒素ガスを導入して、低分子
量戊分を除去し、４００℃で５時間熱重合して、軟化点
３１０℃、キノリン不溶分５０％、ベンゼン不溶分９８
％、メソフエーズ含有量９０％以上の紡糸用メソフェー
ズピッチを得た。Next, nitrogen gas was introduced into this reduced pitch to remove low molecular weight fractions, and thermal polymerization was carried out at 400°C for 5 hours to obtain a softening point of 310°C, a quinoline insoluble content of 50%, and a benzene insoluble content of 98%.
%, and a mesophase pitch for spinning with a mesophase content of 90% or more was obtained.
実施例１〜３
参考例１で得られた紡糸用メソフェーズピッチを原料と
し、第１図乃至第３図に示す形式のスリット型ノズルを
使用して、空気を吹付けつつシート状ピッチを製造し、
これを牽引下に巻き取って、テープ状ピッチ系ピッチフ
ィルムを得た。次いで、これを空気中で不融化処理し、
次いで窒素ガス中で１０００℃まで加熱して、テープ状
ピッチ系炭素フィルムを得た。Examples 1 to 3 Using the mesophase pitch for spinning obtained in Reference Example 1 as a raw material, sheet-like pitch was produced while blowing air using a slit-type nozzle of the type shown in Figs. 1 to 3. ,
This was wound up under traction to obtain a tape-like pitch-based pitch film. Next, this is treated to be infusible in air,
Next, it was heated to 1000° C. in nitrogen gas to obtain a tape-shaped pitch-based carbon film.
製造条件と得られたテープ状ピッチ系炭素フィルムの性
状を第１表に示す。Table 1 shows the manufacturing conditions and the properties of the obtained tape-like pitch-based carbon film.
比較例１
シート状ピッチの製造時に空気の吹付けを行わない以外
は実施例１と同様にして、テープ状ピッチ系炭素フィル
ムを得た。Comparative Example 1 A tape-like pitch-based carbon film was obtained in the same manner as in Example 1, except that air was not blown during production of the sheet-like pitch.
製造条件と得られたテープ状ピッチ系炭素フィルムの性
状を第１表に併せて示す。The manufacturing conditions and properties of the obtained tape-like pitch-based carbon film are also shown in Table 1.
第１図乃至第３図は、本発明方法を実施するに際し使用
するスリット型ノズルの概要を示す図面である。
（１）・・・紡糸装置
（３）・・・シート状ピッチ
（５）・・・巻取装置
（７）・・・スリット型ノズル
（９）・・・気流吹出し口
（１ｌ）・・・テープ状ピッチフィルム（以 上）
第
１
図
第
２
図
１１
第
３
図
５1 to 3 are drawings showing an outline of a slit-type nozzle used in carrying out the method of the present invention. (1)... Spinning device (3)... Sheet pitch (5)... Winding device (7)... Slit type nozzle (9)... Air flow outlet (1l)... Tape-shaped pitch film (above) Figure 1 Figure 2 Figure 11 Figure 3 Figure 5
Claims (4)
ィルム。(1) Tape-shaped pitch-based carbon film with a thickness of 10 to 40 μm.
つ押出された面状ピッチを巻取装置に牽引して巻取り、
該ピッチを不融化し、炭化するテープ状ピッチ系炭素フ
ィルムの製造方法であって、牽引により幅が減少しつつ
ある該面状ピッチの幅方向両端面近傍に、且つスリット
中央点を通るスリット長さ方向の面に垂直な仮想面に対
称な方向に、該面状ピッチが十分に固化する前に、外向
成分および下向成分を有する気流を吹き付けてテープ状
ピッチフィルムを製造し、これを不融化し、炭化するこ
とを特徴とするテープ状ピッチ系炭素フィルムの製造方
法。(2) Extruding spinning pitch from a slit-type nozzle, and pulling the extruded planar pitch to a winding device and winding it up;
A method for producing a tape-like pitch-based carbon film in which the pitch is infusible and carbonized, the length of the slit passing through the center point of the slit in the vicinity of both end faces in the width direction of the planar pitch whose width is decreasing due to traction. Before the planar pitch is sufficiently solidified, an airflow having an outward component and a downward component is blown in a direction symmetrical to an imaginary plane perpendicular to the plane in the horizontal direction to produce a tape-like pitch film, and this is made into a tape-like pitch film. A method for producing a tape-shaped pitch-based carbon film, which is characterized by melting and carbonizing.
所からシート状ピッチの両面に気流を吹付ける請求項（
２）に記載のテープ状ピッチ系炭素フィルムの製造方法
。(3) A claim in which air currents are blown onto both sides of the sheet-like pitch from at least two locations near both end faces in the width direction symmetrically with respect to a virtual plane (
2) The method for producing a tape-shaped pitch-based carbon film.
求項（２）または（３）に記載のテープ状ピッチ系炭素
フィルムの製造方法。(4) The method for producing a tape-shaped pitch-based carbon film according to claim (2) or (3), wherein the temperature of the air stream to be blown is 200 to 400°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1227740A JPH0393613A (en) | 1989-09-01 | 1989-09-01 | Pitch-based carbon film tape and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1227740A JPH0393613A (en) | 1989-09-01 | 1989-09-01 | Pitch-based carbon film tape and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0393613A true JPH0393613A (en) | 1991-04-18 |
Family
ID=16865627
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1227740A Pending JPH0393613A (en) | 1989-09-01 | 1989-09-01 | Pitch-based carbon film tape and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0393613A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0463170A1 (en) * | 1990-01-17 | 1992-01-02 | Osaka Gas Co., Ltd. | Process for producing a carbon film |
| CN102166481A (en) * | 2011-03-07 | 2011-08-31 | 中国矿业大学 | Method for preparing composite carbon membrane based on asphaltene components in coals |
| US8240687B2 (en) * | 2007-07-04 | 2012-08-14 | Honda Motor Co., Ltd. | Wheel suspension system for a steerable wheel |
-
1989
- 1989-09-01 JP JP1227740A patent/JPH0393613A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0463170A1 (en) * | 1990-01-17 | 1992-01-02 | Osaka Gas Co., Ltd. | Process for producing a carbon film |
| EP0463170A4 (en) * | 1990-01-17 | 1992-12-09 | Osaka Gas Company Limited | Process for producing carbonaceous composite material containing carbon film, molding base material, and carbon film |
| US5326510A (en) * | 1990-01-17 | 1994-07-05 | Osaka Gas Company Limited | Carbon composite material incorporating carbon film, forming material and process for producing the carbon film |
| US8240687B2 (en) * | 2007-07-04 | 2012-08-14 | Honda Motor Co., Ltd. | Wheel suspension system for a steerable wheel |
| CN102166481A (en) * | 2011-03-07 | 2011-08-31 | 中国矿业大学 | Method for preparing composite carbon membrane based on asphaltene components in coals |
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