JPS63264967A - Method for modifying carbon fiber - Google Patents
Method for modifying carbon fiberInfo
- Publication number
- JPS63264967A JPS63264967A JP62091984A JP9198487A JPS63264967A JP S63264967 A JPS63264967 A JP S63264967A JP 62091984 A JP62091984 A JP 62091984A JP 9198487 A JP9198487 A JP 9198487A JP S63264967 A JPS63264967 A JP S63264967A
- Authority
- JP
- Japan
- Prior art keywords
- carbon fibers
- present
- seconds
- carbon fiber
- carbon
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 31
- 239000004917 carbon fiber Substances 0.000 title claims description 30
- 238000000034 method Methods 0.000 title claims description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title description 9
- 239000008151 electrolyte solution Substances 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JDVIRCVIXCMTPU-UHFFFAOYSA-N ethanamine;trifluoroborane Chemical compound CCN.FB(F)F JDVIRCVIXCMTPU-UHFFFAOYSA-N 0.000 description 1
- ZHNUHDYFZUAESO-UHFFFAOYSA-N formamide Substances NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は炭素繊維の改質方法、さらに詳しくいえば表面
処理により樹脂等との接着性を大きくシ′、複合材とし
たときその強度を向上させるための炭素繊維の表面処理
方法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for modifying carbon fibers, and more specifically, a method for improving the adhesion with resins etc. by surface treatment, and increasing the strength when made into a composite material. The present invention relates to a method for surface treatment of carbon fibers to improve the surface of carbon fibers.
炭素繊維は、疎水性であり、また樹脂等との接着性も低
いので、これらを良くするため炭素繊維の表面処理方法
が、数多く提案さ机ている。Since carbon fibers are hydrophobic and have low adhesion to resins, etc., many surface treatment methods for carbon fibers have been proposed to improve these properties.
これらの方法のうち、炭素Ｉ＆維の導電性を利用した電
解処理方法が、工業的に有利であるとされ、この電解処
理法の一つとして、パルス給電による方法が提案されて
いる（特開昭６２−４５７７３号公報）。Among these methods, an electrolytic treatment method that utilizes the conductivity of carbon I and fibers is said to be industrially advantageous, and as one of these electrolytic treatment methods, a method using pulsed power supply has been proposed (Unexamined Japanese Patent Publication No. Publication No. 62-45773).
この方法は、電解質溶液としては、アルカリ性の水酸化
ナトリウム水溶液を使用しているものであるが、炭素繊
維の表面に結合する酸素量を増加させることは困難であ
る。Although this method uses an alkaline aqueous sodium hydroxide solution as the electrolyte solution, it is difficult to increase the amount of oxygen bonded to the surface of the carbon fibers.
炭素繊維とマトリックス樹脂との接着性は、炭素繊維の
結合状態に大きく影響される。すなわち、炭素繊維が電
解酸化されると、表面の炭素と酸素の結合状態は、
−Ｃ−Ｏ−１Ｃ＝０、−Ｃ−Ｏ−
などになっており、これらの結合状態になっているとエ
ポキシ樹脂との接着性がよく、待に第三番目の結合状態
だとアミンと反応してアミド結合を形成するので硬化剤
としてアミンを含むエポキシ樹脂との接着性がよい。The adhesiveness between carbon fibers and matrix resin is greatly influenced by the bonding state of the carbon fibers. In other words, when carbon fibers are electrolytically oxidized, the bonding states of carbon and oxygen on the surface are -C-O-1C=0, -C-O-, etc. It has good adhesion with epoxy resins, and since it reacts with amines to form amide bonds in the third bonding state, it has good adhesion with epoxy resins containing amines as curing agents.
このように、炭素繊維表面の酸素の最適の結合状態がマ
トリックス樹脂や、硬化剤の種類に応じで変化するので
、この結合形態を制御できる方法の開発が切望されてい
る。As described above, the optimal bonding state of oxygen on the surface of carbon fibers changes depending on the type of matrix resin and curing agent, so there is a strong desire to develop a method that can control this bonding form.
本発明は、マ） ＩＪツク入用脂との接着性を決定づけ
る炭素繊維の結合酸素量を増加させ、さらに、酸素結合
状態を制御しやすい電解処理方法の提供を目的とする。An object of the present invention is to provide an electrolytic treatment method that increases the amount of bonded oxygen in carbon fibers, which determines the adhesion with the oil used in IJ, and further allows easy control of the oxygen bonding state.
本発明者らは、炭素繊維の電解処理において、炭素繊維
の表面の酸素結合量を増加させる手段を種々検討した結
果、酸性電解質溶液中で断続的給電により電解処理をし
た場合に異常に結合酸素量が増加することを見出し本発
明をなすに至った。The present inventors investigated various means for increasing the amount of oxygen bonded on the surface of carbon fibers in electrolytic treatment of carbon fibers, and found that when electrolytic treatment was performed in an acidic electrolyte solution with intermittent power supply, the amount of bound oxygen was abnormally high. The present inventors have discovered that the amount increases and have come up with the present invention.
すなわち、本発明は、炭素繊維を陽極とし、酸性電解質
溶液中で、断続的に給電することを特徴とする炭素繊維
の電解処理方法を提供するものである。That is, the present invention provides a method for electrolytically treating carbon fibers, which is characterized in that carbon fibers are used as anodes and electricity is intermittently supplied in an acidic electrolyte solution.
本発明は表面処理すべき炭素繊維を陽極として、陰極は
、例えば、白金等を用いて、これらを酸性電解質溶液中
に浸して、電解処理することよりなるものである。In the present invention, the carbon fiber to be surface-treated is used as an anode, and the cathode is made of, for example, platinum, which is immersed in an acidic electrolyte solution and electrolytically treated.
本発明の方法に陽極として用いる炭素繊維は、連続繊維
でも不連続繊維でも使用でき、又、黒鉛繊維も使用でき
る。The carbon fiber used as an anode in the method of the present invention can be either continuous fiber or discontinuous fiber, and graphite fiber can also be used.
本発明の方法では、陰極に使用する電解質溶液に対して
耐腐蝕性の導電性材料、例えば、白金、炭素材料、金な
どが使用できる。In the method of the present invention, corrosion-resistant conductive materials such as platinum, carbon materials, gold, etc. can be used for the electrolyte solution used in the cathode.
本発明の電解質溶液として、酸性電解質が好適に使用で
きる。An acidic electrolyte can be suitably used as the electrolyte solution of the present invention.
本発明に用いる酸性電解質は、例えば、化学式％式％
Ｎａ２５Ｏ，などが使用で外、とくに、強酸電解質、例
えば、１１□ＳＯ１、ＨＮＯ，等が好適に使用できる。The acidic electrolyte used in the present invention includes, for example, the chemical formula % Na25O, and particularly strong acid electrolytes such as 11□SO1, HNO, etc. are preferably used.
本発明に強アルカリ電解質を使用すると、陰極表面に金
属陽イオンが集まり、電解能を落とし、その結果、炭素
ＭＪｔ維の表面の酸化反応が起こらなくなる。When a strong alkaline electrolyte is used in the present invention, metal cations gather on the cathode surface, lowering the electrolytic ability, and as a result, no oxidation reaction occurs on the surface of the carbon MJt fibers.
本発明の電解処理において使用する電圧は、１．５〜５
■、好ましくは、１．８〜３．３ｖが使用でき、５■を
越えると、陰極から水素が大量に発生し、危険であり、
又、均一酸化処理が、困難となることがあり、電解酸化
を制御することができなくなる。The voltage used in the electrolytic treatment of the present invention is 1.5 to 5
■Preferably, 1.8 to 3.3V can be used; if it exceeds 5■, a large amount of hydrogen will be generated from the cathode, which is dangerous.
Furthermore, uniform oxidation treatment may become difficult, and electrolytic oxidation cannot be controlled.
本発明の電解処理において使用する温度は通常１０°Ｃ
以上、好ましくは３０〜８０℃、特に好ましくは５０〜
７０℃において実施できる。The temperature used in the electrolytic treatment of the present invention is usually 10°C.
Above, preferably 30-80°C, particularly preferably 50-80°C
It can be carried out at 70°C.
本発明の電解処理は、電圧により異なるが、通電時間は
通常１秒〜５分、好ましくは、５〜６０秒、特に好まし
くは２０〜５０秒において実施できる。Although the electrolytic treatment of the present invention varies depending on the voltage, the current application time is usually 1 second to 5 minutes, preferably 5 to 60 seconds, and particularly preferably 20 to 50 seconds.
本発明の特徴の一つである断続的な給電は、通常一定時
間の間隔毎に通電を断つことにより実施する。Intermittent power supply, which is one of the features of the present invention, is usually carried out by cutting off power supply at regular time intervals.
この際、停電時間は、該停電時間中に電極表面付近の高
濃度の電解質陰イオンの濃度が下がる時間であることが
望ましく、通常１秒〜６０秒、とくに、よくかきまぜな
がら行う場合は、１秒程度の短時間で十分なことも多い
。At this time, the power outage time is preferably a time during which the concentration of high-concentration electrolyte anions near the electrode surface decreases, and is usually 1 second to 60 seconds, especially 1 second to 60 seconds, especially when stirring well. A short time of about seconds is often sufficient.
このかきまぜは、かきまぜ翼の形、電解質溶液の循環方
法などを種々変えることにより効率的に行うことができ
る。This stirring can be performed efficiently by variously changing the shape of the stirring blades, the method of circulating the electrolyte solution, etc.
本発明の電解処理は電流密度１５Ａ／ｘ２以下で好適に
実施できる。電流密度カ弓５Ａ／ＪＩ２を越えると炭素
繊維の強度が低下する。The electrolytic treatment of the present invention can be suitably carried out at a current density of 15 A/x2 or less. When the current density exceeds 5A/JI2, the strength of the carbon fiber decreases.
本発明の電解処理は、通電量１００クーロン以下で行う
のが、好ましい。１００クーロンを越えると、やはり炭
素繊維の強度が低下する。The electrolytic treatment of the present invention is preferably carried out at a current flow rate of 100 coulombs or less. If it exceeds 100 coulombs, the strength of the carbon fiber will still decrease.
本発明の電解処理方法は、断続給電により炭素繊維を、
短時間で効率的に表面処理できる。又、断続給電を繰り
返すことにより、炭素繊維の表面が次第に酸化されて親
水性になるため、通電時の初期電流値がこれに応じて大
ぎくなり、炭素繊維の表面の結合酸素量が増大する。そ
の結果、樹脂 “マトリックスに対する相溶性
が向上し、強度の犬きい複合材料を製造できる利点があ
る。The electrolytic treatment method of the present invention treats carbon fibers by intermittent power supply.
Surface treatment can be done efficiently in a short time. In addition, by repeating intermittent power supply, the surface of the carbon fiber is gradually oxidized and becomes hydrophilic, so the initial current value when energized increases accordingly, and the amount of bound oxygen on the surface of the carbon fiber increases. . As a result, the compatibility with the resin matrix improves, which has the advantage of making it possible to produce strong composite materials.
〔実施例〕 本発明を実施例によりさらに詳細に説明する。〔Example〕 The present invention will be explained in more detail with reference to Examples.
実施例１
硝酸の１ ｍｏｉ、／１水溶液中で、炭素繊、４ｉ （
４０００本のフィラメント束、ＵＣＣ社製Ｆ２５−１引
張強度１４４ｋｇ／ｌ漏２、弾性率１２．５ｔ／ａｕ二
）を陽極とし、白金板を陰極とし、６３°Ｃで、２■の
直流を３０秒通電し、次いで、３０秒停電し、さらに、
３０秒通電した。Example 1 Carbon fibers, 4i (
A bundle of 4000 filaments, UCC F25-1 tensile strength 144 kg/l leakage 2, elastic modulus 12.5 t/au 2) was used as an anode, a platinum plate was used as a cathode, and a DC current of 2 cm was applied at 63°C for 30 min. Power on for seconds, then power off for 30 seconds, and then
Power was applied for 30 seconds.
このときの時間−電流曲線は、第１図のとおりであった
。The time-current curve at this time was as shown in FIG.
実施例２
２■の直流を、３０秒通電：３０秒停電の断続給電を６
回繰り返したこと以外は、実施例１と同様な方法により
電解処理を行った。１回目から６回目の通電量は、順次
３．０６．３．２４．３．４２．３．６２．３．７６
．４．１０クーロンであり、総給電量は、２１．２クー
ロンであった。Example 2 2 ■ DC current for 30 seconds: Intermittent power supply with 30 seconds power outage 6
The electrolytic treatment was performed in the same manner as in Example 1, except that the treatment was repeated twice. The amount of current applied from the first to the sixth time is 3.06.3.24.3.42.3.62.3.76
．． 4.10 coulombs, and the total amount of power supplied was 21.2 coulombs.
実施例３
電解液を１２℃でかきまぜながら、２ｖの直流を５秒通
電、５秒停電の断続給電を６０回繰り返したこと以外は
、実施例１と同様な方法により電解処理を行った。総給
電量は、８．８クーロンであった。Example 3 Electrolytic treatment was carried out in the same manner as in Example 1, except that while stirring the electrolytic solution at 12° C., intermittent power supply of 2V DC was applied for 5 seconds and then interrupted for 5 seconds 60 times. The total amount of power supplied was 8.8 coulombs.
実施例４
硫酸の１ ｍｏｎ／（ｌ水溶液中で、炭素ｗＬ（４００
０本のフィラメント、ｕＣＣ社製Ｆ２５Ｗ）を陽極とし
、白金板を陰極とし、５５°Ｃで、２■の直流を３０秒
通電、３０秒停電の断続給電を６回繰り返した。総給電
量は、２０．１クーロンであった。Example 4 Carbon wL (400
Using a filament (F25W manufactured by uCC Co., Ltd.) as an anode and a platinum plate as a cathode, intermittent power supply was repeated six times at 55°C, with 2μ of direct current applied for 30 seconds and a power outage for 30 seconds. The total amount of power supplied was 20.1 coulombs.
比較例１
水酸化ナトリウムの５ｗｔ％水溶液中で、炭素繊＠（４
０００本のフィラメント束、ＵＣＣ社製Ｐ２５Ｗ）を陽
極とし、白金板を陰極とし、２０’Ｃでかぎまぜながら
、５Ｖの直流を１秒通電、１秒停電の断続給電を３０回
繰り返した。Comparative Example 1 In a 5 wt% aqueous solution of sodium hydroxide, carbon fiber @ (4
Using a bundle of 1,000 filaments (P25W manufactured by UCC) as an anode and a platinum plate as a cathode, intermittent power supply of 5V DC was applied for 1 second and then interrupted for 1 second while stirring at 20'C was repeated 30 times.
比較例２
２■の直流を３０秒通電、３０秒停電の断続給電を６回
繰り返したこと以外は、比較例１と同様な方法により電
解処理を行った。Comparative Example 2 Electrolytic treatment was carried out in the same manner as in Comparative Example 1, except that intermittent power supply of 2■ DC current for 30 seconds and 30 seconds of power outage was repeated six times.
比較例３
硝酸のｌｌｌ１ｏ１／１水溶液中で、炭素繊維（４００
０本のフィラメント束、ＵＣＣ社製ｐｚｓｗ）を陽極と
し、白金板を陰極とし、１２℃で、２ｖの直流を連続通
電し、電解処理を行った。８．８クーロンの総給電量に
なるまで、１５分２秒要した。このときの時間−電流曲
線を第２図に示す。Comparative Example 3 Carbon fiber (400
A bundle of 0 filaments (pzsw manufactured by UCC) was used as an anode, a platinum plate was used as a cathode, and 2V of direct current was continuously applied at 12° C. to perform electrolytic treatment. It took 15 minutes and 2 seconds to reach a total power supply of 8.8 coulombs. The time-current curve at this time is shown in FIG.
実施例５
実施例１で、使用した炭素繊維、実施例１〜実施例４で
電解処理した炭素Ｍ＆維並びに、比較例１〜比較例３で
電解処理した炭素繊維のそれぞれに、エポキシ樹脂（二
ピフー） ８２８）１００重量部に対し、三７フ化ホウ
素モノエチルアミン５重量部を含む樹脂組成物を含浸し
、１７０℃２時間で硬化させた。Example 5 In Example 1, the carbon fibers used in Example 1, the carbon M & fibers electrolytically treated in Examples 1 to 4, and the carbon fibers electrolytically treated in Comparative Examples 1 to 3 were coated with epoxy resin Pifu) 828) 100 parts by weight was impregnated with a resin composition containing 5 parts by weight of boron trifluoride monoethylamine, and cured at 170°C for 2 hours.
この硬化物の炭素繊維含量は６０重量％とじた。The carbon fiber content of this cured product was 60% by weight.
得られた硬化物の物性を第１表に示す。Table 1 shows the physical properties of the obtained cured product.
第１図及び１２図は本発明の電解処理方法における通電
形態を示す時間−電流曲線図を示す。
特許出願人 出光興産株式会社
代 理 人 阿 形 明光１図
（ＳｅＣ）FIGS. 1 and 12 are time-current curve diagrams showing the energization mode in the electrolytic treatment method of the present invention. Patent applicant: Idemitsu Kosan Co., Ltd. Representative: Agata Meiko 1 (SeC)
Claims (1)
に給電することを特徴とする炭素繊維の改質方法。1. A method for modifying carbon fibers, which comprises using carbon fibers as anodes and intermittently supplying electricity in an acidic electrolyte solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62091984A JPS63264967A (en) | 1987-04-16 | 1987-04-16 | Method for modifying carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62091984A JPS63264967A (en) | 1987-04-16 | 1987-04-16 | Method for modifying carbon fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63264967A true JPS63264967A (en) | 1988-11-01 |
Family
ID=14041743
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62091984A Pending JPS63264967A (en) | 1987-04-16 | 1987-04-16 | Method for modifying carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63264967A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007224459A (en) * | 2006-02-24 | 2007-09-06 | Toray Ind Inc | Method for producing surface-oxidized carbon fiber bundle |
| JP2019151949A (en) * | 2018-03-02 | 2019-09-12 | 国立大学法人岐阜大学 | Carbon fiber, and method for producing carbon fiber |
-
1987
- 1987-04-16 JP JP62091984A patent/JPS63264967A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007224459A (en) * | 2006-02-24 | 2007-09-06 | Toray Ind Inc | Method for producing surface-oxidized carbon fiber bundle |
| JP2019151949A (en) * | 2018-03-02 | 2019-09-12 | 国立大学法人岐阜大学 | Carbon fiber, and method for producing carbon fiber |
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