JPH06345553A - Method for bonding graphite material - Google Patents
Method for bonding graphite materialInfo
- Publication number
- JPH06345553A JPH06345553A JP5129887A JP12988793A JPH06345553A JP H06345553 A JPH06345553 A JP H06345553A JP 5129887 A JP5129887 A JP 5129887A JP 12988793 A JP12988793 A JP 12988793A JP H06345553 A JPH06345553 A JP H06345553A
- Authority
- JP
- Japan
- Prior art keywords
- graphite material
- phenol
- graphite
- resin
- formaldehyde resin
- 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
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高温で使用する黒鉛材
の接着法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a bonding method for graphite materials used at high temperatures.
【０００２】[0002]
【従来の技術】黒鉛材は、真空及び還元性の雰囲気では
３０００℃の高温まで使用できるために、高温炉の部
品、ヒーター等に切削された一体物で使用されてきた。
高温炉の部品等で、特別に荷重のかからない部分や高周
波誘導加熱に使用する場合等のようにどうしても一体物
を必要とする場合を除いて、黒鉛材について高温で剥離
しない接着方法があれば、黒鉛材の端材、折損不良品等
が生じたときにその黒鉛材を使って接着を行って接着品
とし、黒鉛材の端材、折損不良品等を廃棄することなく
有効に活用することができる。一方、膨張黒鉛の膨張倍
率が大きいために薄手のものしか得られない膨張黒鉛シ
ートも、接着による厚手化が望まれている。2. Description of the Related Art Graphite materials can be used up to a high temperature of 3000.degree. C. in a vacuum and a reducing atmosphere, so that they have been used as one piece cut into parts of a high temperature furnace, heaters and the like.
Except for the case where a unit is absolutely necessary such as a part that does not receive a load or when it is used for high-frequency induction heating in high temperature furnace parts, etc., if there is a bonding method that does not peel off at high temperatures for graphite materials, When a scrap material of graphite material or a defective breakage product is generated, the graphite material is used for adhesion to make a bonded product, and the scrap material of the graphite material, a broken damage product, etc. can be effectively utilized without being discarded. it can. On the other hand, it is desired that the expanded graphite sheet, which can be obtained only in a thin shape due to the large expansion ratio of expanded graphite, be made thick by adhesion.
【０００３】[0003]
【発明が解決しようとする課題】接着品としては、高温
炉用の断熱材として、炭素繊維フェルトと膨張黒鉛シー
トとを接着したもの等が検討されているが、この高温炉
用の断熱材は、炭素繊維フェルトと膨張黒鉛シートのよ
うに異種材質の組み合わせであることもあって、接合面
で剥離するという問題がある。本発明は、上記した従来
の問題点を解消し、高温でも剥離しない黒鉛材の接着法
を提供するものである。As an adhesive product, as a heat insulating material for a high temperature furnace, a material in which a carbon fiber felt and an expanded graphite sheet are bonded is being studied. The carbon fiber felt and the expanded graphite sheet may be a combination of different materials, which causes a problem of peeling at the joint surface. The present invention solves the above-mentioned conventional problems and provides a method for adhering a graphite material that does not separate even at high temperatures.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、黒鉛材の
接着方法特に接着剤及び接着特性について鋭意研究を重
ねた結果、本発明を完成するに至った。本発明は、数平
均分子量が２７０〜２８０で且つ２５℃における粘度が
１１０〜２５０センチポアズ（ｃＰ）のフェノール・ホ
ルムアルデヒド樹脂を黒鉛材の接合面に塗布し、接合面
を重ね合わせて硬化、炭化或いは更に黒鉛化する黒鉛材
の接着法に関する。The inventors of the present invention have completed the present invention as a result of earnest studies on a method of adhering a graphite material, particularly an adhesive and an adhesive property. In the present invention, a phenol / formaldehyde resin having a number average molecular weight of 270 to 280 and a viscosity at 25 ° C. of 110 to 250 centipoise (cP) is applied to a joint surface of a graphite material, and the joint surface is superposed and cured, carbonized or Further, it relates to an adhesion method of a graphite material which is graphitized.
【０００５】本発明において、フェノール・ホルムアル
デヒド樹脂の数平均分子量及び２５℃における粘度が上
記の範囲から外れるものを使用すると、接着後に高温で
剥離する危険がある。接着する黒鉛材の組み合わせにつ
いては特に制限はなく、同種のものでも異種のものでも
良い。フェノール・ホルムアルデヒド樹脂の黒鉛材の接
合面への塗布は一方の黒鉛材の接合面だけでも良く、両
方の黒鉛材の接合面でも良い。塗布後は接合面を重ね合
わせ、樹脂を硬化させる。次いで、炭化、更に使用条件
によっては黒鉛化まで行う。炭化処理は通常８００℃以
上、好ましくは１０００℃以上の不活性雰囲気で行う。
処理温度が低いと高温で剥離する恐れがある。不活性雰
囲気は、酸素を含まず、通常はヘリウム、アルゴン、窒
素、水素、ハロゲンからなる群より選ばれる少なくとも
１種又は２種以上の気体からなる雰囲気、真空の雰囲気
又は減圧された雰囲気を言う。黒鉛化は通常２５００℃
以上で行う。In the present invention, if a phenol-formaldehyde resin having a number average molecular weight and a viscosity at 25 ° C. outside the above range is used, there is a risk of peeling at a high temperature after adhesion. The combination of the graphite materials to be adhered is not particularly limited, and the same kind or different kinds may be used. The phenol / formaldehyde resin may be applied to the joint surface of the graphite material only on one joint surface of the graphite material or on both joint surfaces of the graphite materials. After application, the bonding surfaces are overlapped and the resin is cured. Next, carbonization and further graphitization are performed depending on the use conditions. The carbonization treatment is usually performed in an inert atmosphere at 800 ° C or higher, preferably 1000 ° C or higher.
If the treatment temperature is low, it may peel off at a high temperature. The inert atmosphere refers to an atmosphere that does not contain oxygen and is usually composed of at least one kind or two or more kinds of gas selected from the group consisting of helium, argon, nitrogen, hydrogen and halogen, a vacuum atmosphere or a reduced pressure atmosphere. . Graphitization is usually 2500 ℃
This is done.
【０００６】[0006]
【実施例】次に本発明の実施例を説明する。 実施例１、参考例１ フェノールとホルムアルデヒドとを(ａ)Ｃ6Ｈ6ＯＨ＋Ｃ
Ｈ2Ｏ→Ｃ6Ｈ4ＯＨ・ＣＨ2ＯＨ、(ｂ)Ｃ6Ｈ4ＯＨ・ＣＨ
2ＯＨ→(−Ｃ6Ｈ2ＯＨ・ＣＨ2−)n＋Ｈ2Ｏの反応によ
り、接着剤として表１に示す４種類のフェノール・ホル
ムアルデヒド樹脂を得た。この中、Ｎo.３の樹脂が本発
明で使用する樹脂である。厚さ３mmの膨張黒鉛シート
（日立化成工業製、ＨＧＰ−２０７）２枚をそれぞれ１
００cm平方に切断し、その両シートの接合面に前記フェ
ノール・ホルムアルデヒド樹脂を塗布し、重ね合わせた
後で室温から毎時１０℃の速度で昇温し、８０℃で５時
間保持して樹脂を硬化させた。次いで、窒素雰囲気下毎
時１０℃の速度で１０００℃まで昇温し、その温度で５
時間保持して樹脂を炭化させた。EXAMPLES Examples of the present invention will be described below. Example 1, Reference Example 1 Phenol and formaldehyde (a) C 6 H 6 OH + C
H 2 O → C 6 H 4 OH ・ CH 2 OH, (b) C 6 H 4 OH ・ CH
By the reaction of 2 OH → (-C 6 H 2 OH.CH 2- ) n + H 2 O, four kinds of phenol / formaldehyde resins shown in Table 1 were obtained as adhesives. Among them, the resin No. 3 is the resin used in the present invention. 2 x 3mm thick expanded graphite sheets (Hitachi Chemical Co., Ltd., HGP-207)
Cut it into squares of 00 cm, apply the above-mentioned phenol-formaldehyde resin to the joint surface of both sheets, and after overlapping, raise the temperature from room temperature at a rate of 10 ° C per hour and hold at 80 ° C for 5 hours to cure the resin. Let Then, the temperature was raised to 1000 ° C. at a rate of 10 ° C./hour under a nitrogen atmosphere, and the temperature was increased to 5 ° C.
Hold for time to carbonize the resin.
【０００７】[0007]
【表１】 [Table 1]
【０００８】実施例２、参考例２ 厚さ５０mmの炭素繊維フェルト(呉羽化学工業製、クレ
カＲ−２００)及び厚さ０．３mmの膨張黒鉛シート(日立
化成工業製、ＨＧＰ−２０７)を各々１００cm平方に切
断し、以下、実施例１と同じ方法で接着、硬化及び炭化
させて接着品を得た。 実施例３、参考例３ 厚さ１０mmの黒鉛材(日立化成工業製、ＰＤ−６００)の
２枚を各々１００cm平方に切断し、以下、実施例１と同
じ方法で接着、硬化及び炭化させて接着品を得た。Example 2, Reference Example 2 A carbon fiber felt having a thickness of 50 mm (Kureha Chemical Industry Co., Ltd., Creca R-200) and an expanded graphite sheet having a thickness of 0.3 mm (Hitachi Chemical Co., Ltd., HGP-207) were respectively used. It was cut into a 100 cm square, and thereafter bonded, cured and carbonized in the same manner as in Example 1 to obtain a bonded product. Example 3, Reference Example 3 Two pieces of a graphite material (PD-600 manufactured by Hitachi Chemical Co., Ltd.) having a thickness of 10 mm were cut into 100 cm squares, and then bonded, cured and carbonized in the same manner as in Example 1. I got an adhesive.
【０００９】比較例１ 実施例１におけるフェノール・ホルムアルデヒド樹脂の
代りにフルフリルアルコール初期縮合物(日立化成工業
製、ＶＦ−３０２)を用いた以外は実施例１と同じ方法
で接着品を得た。 比較例２ 実施例２におけるフェノール・ホルムアルデヒド樹脂の
代りにフルフリルアルコール初期縮合物(日立化成工業
製、ＶＦ−３０２)を用いた以外は実施例１と同じ方法
で接着品を得た。 比較例３ 実施例３におけるフェノール・ホルムアルデヒド樹脂の
代りにフルフリルアルコール初期縮合物(日立化成工業
製、ＶＦ−３０２)を用いた以外は実施例１と同じ方法
で接着品を得た。Comparative Example 1 An adhesive product was obtained in the same manner as in Example 1 except that a furfuryl alcohol initial condensate (VF-302 manufactured by Hitachi Chemical Co., Ltd.) was used in place of the phenol-formaldehyde resin in Example 1. . Comparative Example 2 An adhesive product was obtained in the same manner as in Example 1 except that a furfuryl alcohol initial condensation product (VF-302 manufactured by Hitachi Chemical Co., Ltd.) was used in place of the phenol-formaldehyde resin in Example 2. Comparative Example 3 An adhesive product was obtained in the same manner as in Example 1 except that the furfuryl alcohol initial condensation product (VF-302 manufactured by Hitachi Chemical Co., Ltd.) was used in place of the phenol-formaldehyde resin in Example 3.
【００１０】上記実施例及び比較例で得られた接着品を
１０００℃及び２８００℃に加熱して剥離の有無を目視
観察した。剥離していない場合は、接着品をマイクロカ
ッターで切断して幅１０mm、長さ１００mmの試験片を作
り、万能試験機で曲げ試験を行い、切断箇所を調べた。
この結果を次頁の表２に示す。The adhesive articles obtained in the above Examples and Comparative Examples were heated to 1000 ° C. and 2800 ° C., and the presence or absence of peeling was visually observed. When not peeled, the adhesive product was cut with a micro cutter to prepare a test piece with a width of 10 mm and a length of 100 mm, and a bending test was performed with a universal testing machine to examine the cut portion.
The results are shown in Table 2 on the next page.
【００１１】[0011]
【表２】 表２から明らかなように、実施例１、２及び３のＮo.３
のフェノール・ホルムアルデヒド樹脂(数平均分子量２
７０〜２８０、２５℃における粘度が１１０〜２５０ｃ
Ｐ)を接着剤に用いたものは、２８００℃でも剥離がな
く、母材の方から折れている。また、実施例２のように
異種材質の組み合わせでも２８００℃で剥離しない。[Table 2] As is clear from Table 2, Nos. 3 of Examples 1, 2 and 3
Phenol-formaldehyde resin (number average molecular weight 2
70-280, viscosity at 25 ° C is 110-250c
In the case of using P) as an adhesive, there is no peeling even at 2800 ° C., and the base material is broken. Further, even if a combination of different materials as in Example 2, it does not peel off at 2800 ° C.
【００１２】[0012]
【発明の効果】本発明の接着法によって接着した黒鉛材
は、２８００℃のような高温でも剥離がなく、必要な強
度のあるものが得られる。The graphite material adhered by the adhesion method of the present invention does not peel even at a high temperature such as 2800 ° C. and has a required strength.
Claims (1)
５℃における粘度が１１０〜２５０センチポアズのフェ
ノール・ホルムアルデヒド樹脂を黒鉛材の接合面に塗布
し、接合面を重ね合わせて硬化、炭化或いは更に黒鉛化
することを特徴とする黒鉛材の接着法。1. A number average molecular weight of 270 to 280 and 2
A method for adhering a graphite material, which comprises applying a phenol-formaldehyde resin having a viscosity of 110 to 250 centipoise at 5 ° C. to a joint surface of a graphite material, and superposing the joint surfaces to cure, carbonize or further graphitize.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5129887A JPH06345553A (en) | 1993-06-01 | 1993-06-01 | Method for bonding graphite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5129887A JPH06345553A (en) | 1993-06-01 | 1993-06-01 | Method for bonding graphite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06345553A true JPH06345553A (en) | 1994-12-20 |
Family
ID=15020804
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5129887A Pending JPH06345553A (en) | 1993-06-01 | 1993-06-01 | Method for bonding graphite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06345553A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7041210B2 (en) | 1997-03-25 | 2006-05-09 | Lifescan, Inc. | Method of filling an amperometric cell |
| WO2006114896A1 (en) * | 2005-04-22 | 2006-11-02 | Kureha Corporation | Adhesive agent for thermally insulating material and carbonized laminate for thermally insulating material using the same |
| CN102560712A (en) * | 2010-12-28 | 2012-07-11 | 上海杰远环保科技有限公司 | High heat conduction composite fiber and manufacture method thereof |
| WO2012165208A1 (en) | 2011-05-27 | 2012-12-06 | 東洋炭素株式会社 | Joint of metal material and ceramic-carbon composite material, method for producing same, carbon material joint, jointing material for carbon material joint, and method for producing carbon material joint |
| WO2013172286A1 (en) | 2012-05-15 | 2013-11-21 | 東洋炭素株式会社 | Method for producing (carbon material)-(ceramic material) joint, and (carbon material)-(ceramic material) joint |
-
1993
- 1993-06-01 JP JP5129887A patent/JPH06345553A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7041210B2 (en) | 1997-03-25 | 2006-05-09 | Lifescan, Inc. | Method of filling an amperometric cell |
| WO2006114896A1 (en) * | 2005-04-22 | 2006-11-02 | Kureha Corporation | Adhesive agent for thermally insulating material and carbonized laminate for thermally insulating material using the same |
| CN102560712A (en) * | 2010-12-28 | 2012-07-11 | 上海杰远环保科技有限公司 | High heat conduction composite fiber and manufacture method thereof |
| CN102560712B (en) * | 2010-12-28 | 2016-08-03 | 碳元科技股份有限公司 | A kind of high heat conduction composite fiber and manufacture method thereof |
| WO2012165208A1 (en) | 2011-05-27 | 2012-12-06 | 東洋炭素株式会社 | Joint of metal material and ceramic-carbon composite material, method for producing same, carbon material joint, jointing material for carbon material joint, and method for producing carbon material joint |
| WO2013172286A1 (en) | 2012-05-15 | 2013-11-21 | 東洋炭素株式会社 | Method for producing (carbon material)-(ceramic material) joint, and (carbon material)-(ceramic material) joint |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |