JPH0813711B2 - High-density carbon material manufacturing method - Google Patents
High-density carbon material manufacturing methodInfo
- Publication number
- JPH0813711B2 JPH0813711B2 JP63004689A JP468988A JPH0813711B2 JP H0813711 B2 JPH0813711 B2 JP H0813711B2 JP 63004689 A JP63004689 A JP 63004689A JP 468988 A JP468988 A JP 468988A JP H0813711 B2 JPH0813711 B2 JP H0813711B2
- Authority
- JP
- Japan
- Prior art keywords
- container
- pressure
- impregnation
- carbon
- furfuryl alcohol
- 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.)
- Expired - Fee Related
Links
- 239000003575 carbonaceous material Substances 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 48
- 239000007788 liquid Substances 0.000 claims description 31
- 238000005470 impregnation Methods 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 11
- 239000013013 elastic material Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 この発明は高密度炭素材料の製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a high-density carbon material.
従来の技術 炭素材料は、構造材や機械材料として注目されるよう
になってきた。炭素材料は熱や電気の良導体であり、耐
熱性にすぐれ、特に高温での強度劣化などがないことか
ら高温用構造材料や機械用材料として使用されている。2. Description of the Related Art Carbon materials have attracted attention as structural materials and mechanical materials. Carbon materials are good conductors of heat and electricity, have excellent heat resistance, and have no strength deterioration especially at high temperatures, so they are used as structural materials for high temperatures and materials for machinery.
他方、炭素材料は多孔性であるため機械的強度が十分
ではなく、容易に酸化されて消耗するといった欠点をも
っている。このため、これまで多くの研究者が、できる
だけ高密度にすることによって、すぐれた特性の炭素材
料を開発しようと永年努力を重ねてきた。On the other hand, since the carbon material is porous, it has insufficient mechanical strength and is easily oxidized and consumed. For this reason, many researchers have been working for many years to develop carbon materials with excellent properties by making them as dense as possible.
一般的に炭素材料を高密度化するには、骨材粒子の充
填密度を大きくしたり、密度の高い骨材を用いたりして
いた。さらに気孔へのピッチ含浸処理を行うことなどが
考えられていた。たとえば、従来は耐圧容器内に含浸液
と炭素成形体を載置して加圧空気を利用して含浸液を直
接加圧する方法によって高密度炭素材料が製造されてい
た。その際に含浸液を80℃以上に加熱したうえで加圧空
気の圧力を20Kg/cm2以下も設定していた。Generally, in order to increase the density of a carbon material, the packing density of aggregate particles has been increased, or an aggregate having a high density has been used. Further, it has been considered to perform a pitch impregnation treatment on the pores. For example, conventionally, a high-density carbon material has been manufactured by a method in which an impregnating liquid and a carbon molded body are placed in a pressure vessel and the impregnating liquid is directly pressurized using pressurized air. At that time, the impregnating liquid was heated to 80 ° C or higher and the pressure of the pressurized air was set to 20 Kg / cm 2 or less.
発明が解決しようとする課題 しかし、加圧空気の圧力が20Kg/cm2以下では、粘度の
高い含浸液で含浸する場合、含浸効果が悪かった。However, when the pressure of the pressurized air is 20 kg / cm 2 or less, the impregnation effect is poor when impregnated with a highly viscous impregnating liquid.
この発明の目的は、効率よく高密度の炭素材料を製造
する方法を提供することである。An object of the present invention is to provide a method for efficiently producing a high density carbon material.
発明の要旨 前述の目的を達成するために、本発明は耐圧容器内に
圧力伝達液を収容する工程と、伸縮性材料製容器の内部
に300c.p.以上のフルフリルアルコール重合物及び多孔
性の炭素成形体を収容する工程と、伸縮性材料製容器を
減圧密閉する工程と、伸縮性材料製容器を耐圧容器内の
圧力伝達液中に浸漬する工程と、耐圧容器内の圧力伝達
液を加圧して伸縮性材料製容器内でフルフリルアルコー
ル重合物を炭素成形体に含浸させる工程と、その含浸工
程後に、含浸後の炭素成形体を伸縮性材料製容器及び耐
圧容器から取り出す工程と、その後に含浸後の炭素成形
体を焼成する工程を含むことを特徴とする高密度炭素材
料の製造方法を要旨としている。SUMMARY OF THE INVENTION In order to achieve the above-mentioned object, the present invention comprises a step of containing a pressure transmitting liquid in a pressure resistant container, and a furfuryl alcohol polymer of 300 c.p. The step of accommodating the carbon molded body of No. 1, the step of decompressing and sealing the stretchable material container, the step of immersing the stretchable material container in the pressure transfer liquid in the pressure resistant container, and the pressure transfer liquid in the pressure resistant container. A step of impregnating the carbon molded body with a furfuryl alcohol polymer in a stretchable material container under pressure, and a step of removing the impregnated carbon molded body from the stretchable material container and the pressure resistant container after the impregnation step, The gist is a method for producing a high-density carbon material, characterized by including a step of firing a carbon compact after impregnation.
実施例 炭素成形体に含浸液を含浸する際に、含浸時における
粘度が300c.p.以上の含浸液を使用する。この粘度の値
は好ましくは20℃で得られるようにする。油、アルコー
ルや水などの圧力伝達液を利用して含浸液に含浸圧力を
付与する。好ましくはラバープレス法で含浸し、かつ含
浸圧力を50Kg/cm2以上にする。Example When impregnating a carbon compact with an impregnating liquid, an impregnating liquid having a viscosity of 300 c.p. or more during impregnation is used. This viscosity value is preferably obtained at 20 ° C. An impregnating pressure is applied to the impregnating liquid using a pressure transmitting liquid such as oil, alcohol or water. Preferably, the impregnation is performed by a rubber press method, and the impregnation pressure is 50 Kg / cm 2 or more.
本発明において使用する炭素成形体の一例をあげれ
ば、アルミ蒸着用又はCZ用の黒鉛ルツボやヒータ、サセ
プタ用基材、液相成長用ボート、プラズマCVD用電極で
ある。An example of the carbon molded body used in the present invention is a graphite crucible or heater for aluminum vapor deposition or CZ, a substrate for susceptor, a boat for liquid phase growth, an electrode for plasma CVD.
含浸液は、熱処理によって炭化残留する成分を少なく
とも30％以上含むのが好ましい。含浸液としては、フル
フリルアルコール重合物を使用する。フルフリルアルコ
ール重合物は最適の熱硬化性樹脂である。It is preferable that the impregnating liquid contains at least 30% or more of the components remaining after carbonization by the heat treatment. A furfuryl alcohol polymer is used as the impregnating liquid. Furfuryl alcohol polymer is the most suitable thermosetting resin.
含浸圧力は20Kg/cm2以上、特に50kg/cm2以上が望まし
い。Impregnation pressure is 20 Kg / cm 2 or more, especially 50 kg / cm 2 or more.
含浸の際には、圧力伝達液（たとえば水、アルコール
や油）の中に伸縮性のある材料製の容器（たとえばラバ
ー製の容器）を浸漬し、その伸縮性材料製容器の中に含
浸液と炭素成形体を入れた状態で圧力伝達液の方から圧
力を加えて含浸圧力を含浸液に加える。含浸工程の前に
伸縮性材料製容器の中を減圧して、含浸効果を高める。
最善の含浸方法は含浸液をラバープレス法で含浸させる
方法である。During impregnation, dip a container made of an elastic material (for example, a rubber container) in a pressure transmission liquid (for example, water, alcohol, or oil), and then place the impregnated liquid in the elastic material container. With the carbon molded body being added, pressure is applied from the pressure transmitting liquid to the impregnating liquid. Prior to the impregnation step, the elastic material container is depressurized to enhance the impregnation effect.
The best impregnation method is to impregnate the impregnating liquid with a rubber press method.
図示例 表−１に示す４種類の炭素成形体を使用し、第１図に
示す冷間静水圧プレス式の含浸装置を使用して、それら
の炭素成形体にフルフリルアルコール重合物を含浸す
る。Illustrative Example Four types of carbon compacts shown in Table 1 are used, and the furfuryl alcohol polymer is impregnated into the carbon compacts using the cold isostatic pressing type impregnation device shown in FIG. .
第１図において、耐圧容器１内に圧力伝達液として水
２を収容し、その水２の中に伸縮性材料製の容器として
ラバー製容器３を浸漬する。そのラバー製容器３の中に
フルフリルアルコール重合物４を入れ、そこに炭素成形
体５を一緒に配置する。まずラバー製容器３内を10分間
で30torrまで減圧し、そのあと水２を加圧して300Kg/cm
2以上の含浸圧力をフルフリルアルコール重合物４に約
１分間付与し、フルフリルアルコール重合物４を炭素成
形体５に含浸させ、しかるのち10℃／時間の加熱速度で
200℃まで加熱してフルフリルアルコール重合物４を硬
化させ、さらに炉内で８℃／時間の加熱速度で950℃ま
で加熱することにより焼成し、最後に2300℃で純化処理
を行う。それにより、表−２に示すような高密度炭素材
料を得る。In FIG. 1, water 2 is contained as a pressure transmitting liquid in a pressure resistant container 1, and a rubber container 3 as a container made of a stretchable material is immersed in the water 2. The furfuryl alcohol polymer 4 is placed in the rubber container 3, and the carbon molded body 5 is placed together therewith. First, depressurize the inside of the rubber container 3 to 30 torr in 10 minutes, and then pressurize the water 2 to 300 Kg / cm.
An impregnation pressure of 2 or more is applied to the furfuryl alcohol polymer 4 for about 1 minute so that the furfuryl alcohol polymer 4 is impregnated in the carbon molded body 5, and then at a heating rate of 10 ° C./hour.
Furfuryl alcohol polymer 4 is cured by heating to 200 ° C., and is further baked in a furnace at a heating rate of 8 ° C./hour to 950 ° C., and finally purified at 2300 ° C. Thereby, a high density carbon material as shown in Table 2 is obtained.
ところで、一般に炭素成形体に対する含浸液の重要な
特性としては、 含浸液の粘度 含浸液の表面張力 基材との接触角 含浸液中に懸濁している不溶性物質の大きさと形 熱処理中の反応性 含浸液の炭化率 などが挙げられる。なかでも粘度、含浸圧力は含浸時間
を左右する因子として、また炭化率は含浸の効果を決定
する因子として特に重要である。By the way, generally, the important characteristics of the impregnating liquid for the carbon compact are the viscosity of the impregnating liquid, the surface tension of the impregnating liquid, the contact angle with the substrate, the size and shape of the insoluble substance suspended in the impregnating liquid, and the reactivity during heat treatment. Examples include the carbonization rate of the impregnating liquid. Among them, the viscosity and the impregnation pressure are particularly important as factors that influence the impregnation time, and the carbonization rate is particularly important as a factor that determines the effect of impregnation.
本発明で使用するフルフリルアルコール重合物は、常
温で液体であり、後処理操作も簡単であり、炭化率が高
いため、好適な含浸液である。上述した６項目のうち、
は適当な粘性のものを使用できる。またとは高圧
であればよく、は濾過することで無視できる。はフ
ルフリルアルコール重合物が熱硬化性樹脂であることか
ら低温で完結する。については表−３に示す通りであ
る。The furfuryl alcohol polymer used in the present invention is a suitable impregnating liquid because it is liquid at room temperature, the post-treatment operation is simple, and the carbonization rate is high. Of the above 6 items,
Can have a suitable viscosity. Also, and may be high pressure, and can be ignored by filtering. Is completed at a low temperature because the furfuryl alcohol polymer is a thermosetting resin. Is as shown in Table-3.
表−１の実施例2,3のサンプルについて含浸液の粘度
と含浸圧力を２つのパラメータとして実験を行った。粘
度は、30、200、250、300、350、700c.p.（20℃）の６
水準とし、含浸圧力は1500Kg/cm2で含浸した時の高密度
化に及ぼす影響を第２図に示す。An experiment was conducted on the samples of Examples 2 and 3 in Table 1 by using the viscosity of the impregnating liquid and the impregnating pressure as two parameters. Viscosity is 30, 200, 250, 300, 350, 700c.p. (20 ℃) 6
And level, the impregnation pressure is shown in Figure 2 the effect on densification when impregnated with 1500 Kg / cm 2.
第２図から明らかなように、低粘度30c.p.（20℃）の
場合は、フルフリルアルコール重合物が固化するまでに
揮発する量が多く、かさ密度の増加はあまり望めない。
これは表−３の結果を裏付けている。As is apparent from FIG. 2, in the case of a low viscosity of 30 c.p. (20 ° C.), the furfuryl alcohol polymer is volatilized in a large amount until it solidifies, and an increase in bulk density cannot be expected so much.
This supports the results in Table-3.
また、高粘度700c.p.（20℃）の場合は、300c.p.（20
℃）と、かさ密度はあまり変わらない。以上の様なこと
よりフルフリルアルコール重合物の粘度は350c.p.（20
℃）以上が妥当であることがわかった。If the viscosity is 700c.p. (20 ℃), 300c.p.
℃), the bulk density does not change much. From the above, the viscosity of the furfuryl alcohol polymer is 350 c.p.
It was found that the above temperature was appropriate.
【図面の簡単な説明】 第１図は本発明による高密度炭素材料の製造方法を実施
するための含浸装置の一例を示す概略説明図、第２図は
粘度とかさ密度の関係を示す図である。 １……耐圧容器 ２……水（圧力伝達液） ３……ラバー製容器（伸縮性材料製容器） ４……フルフリルアルコール重合物 ５……炭素成形体BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic explanatory view showing an example of an impregnation apparatus for carrying out the method for producing a high-density carbon material according to the present invention, and FIG. 2 is a view showing a relationship between viscosity and bulk density. is there. 1 ... Pressure resistant container 2 ... Water (pressure transmitting liquid) 3 ... Rubber container (contractile material container) 4 ... Furfuryl alcohol polymer 5 ... Carbon molding
Claims (1)
と、伸縮性材料製容器の内部に300c.p.以上のフルフリ
ルアルコール重合物及び多孔性の炭素成形体を収容する
工程と、伸縮性材料製容器を減圧密閉する工程と、伸縮
性材料製容器を耐圧容器内の圧力伝達液中に浸漬する工
程と、耐圧容器内の圧力伝達液を加圧して伸縮性材料製
容器内でフルフリルアルコール重合物を炭素成形体に含
浸させる工程と、その含浸工程後に、含浸後の炭素成形
体を伸縮性材料製容器及び耐圧容器から取り出す工程
と、その後に含浸後の炭素成形体を焼成する工程を含む
ことを特徴とする高密度炭素材料の製造方法。1. A step of accommodating a pressure transmitting liquid in a pressure resistant container, a step of accommodating a furfuryl alcohol polymer of 300 c.p. or more and a porous carbon molded body in a container made of a stretchable material, The process of vacuum-sealing the elastic material container, the step of immersing the elastic material container in the pressure transmitting liquid inside the pressure resistant container, and the step of pressurizing the pressure transmitting liquid inside the pressure resistant container inside the elastic material container The step of impregnating the carbon molded product with the furfuryl alcohol polymer, the step of removing the impregnated carbon molded product from the elastic material container and the pressure resistant container after the impregnation process, and then firing the impregnated carbon molded product. A method for producing a high-density carbon material, which comprises the step of:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63004689A JPH0813711B2 (en) | 1988-01-14 | 1988-01-14 | High-density carbon material manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63004689A JPH0813711B2 (en) | 1988-01-14 | 1988-01-14 | High-density carbon material manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01183482A JPH01183482A (en) | 1989-07-21 |
| JPH0813711B2 true JPH0813711B2 (en) | 1996-02-14 |
Family
ID=11590858
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63004689A Expired - Fee Related JPH0813711B2 (en) | 1988-01-14 | 1988-01-14 | High-density carbon material manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0813711B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMI20110401A1 (en) * | 2011-03-14 | 2012-09-15 | Petroceramics S P A | METHOD FOR INFILTRATION OF A POROUS MATERIAL WITH A SECOND MATERIAL AND ITS PLANT |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55162489A (en) * | 1979-05-31 | 1980-12-17 | Kurosaki Refractories Co | Method of impregnating material having open pores |
-
1988
- 1988-01-14 JP JP63004689A patent/JPH0813711B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01183482A (en) | 1989-07-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4564496A (en) | Method of making porous silicon carbide bodies | |
| JPH0140796B2 (en) | ||
| US3671385A (en) | Fibrous carbonaceous composites and method for manufacturing same | |
| US3089195A (en) | Process for producing a shaped graphite article | |
| US4080413A (en) | Porous carbon fuel cell substrates and method of manufacture | |
| US4532091A (en) | Method of producing permeable, porous molded bodies of silicon carbide | |
| US5925405A (en) | Method of manufacturing ceramic, metallic or ceramo-metallic, shaped bodies and layers | |
| CN113321208B (en) | Preparation method of high-compactness graphene film | |
| JPH0813711B2 (en) | High-density carbon material manufacturing method | |
| US4963396A (en) | Method for making an impregnated ceramic material | |
| US2972552A (en) | All carbon impervious graphite and carbon articles | |
| JP2660515B2 (en) | Graphite crucible | |
| JPH0813712B2 (en) | Carbon material | |
| GB1360887A (en) | Method of producing a carbon composite | |
| RU96122444A (en) | METHOD FOR PRODUCING CARBON MATERIAL | |
| JPH0297464A (en) | High density graphite molded body and production thereof | |
| JPH03295879A (en) | Method for impregnating metal into carbon material | |
| RU2167132C2 (en) | Method of preparing composite material | |
| JPS59174510A (en) | Manufacture of carbon molded body | |
| JP2579560B2 (en) | Oxidation-resistant treatment of carbon fiber reinforced carbon materials | |
| JPH0624847A (en) | High-density and high-strength carbonaceous material manufacturing method | |
| US4539229A (en) | Method of providing a shaped carbon article | |
| JP2660516B2 (en) | Graphite crucible for pulling silicon single crystal | |
| JPH05132373A (en) | Method for producing porous silicon carbide composite | |
| JP3651070B2 (en) | Method for producing glassy carbon with excellent machinability |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees | ||
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| R371 | Transfer withdrawn |
Free format text: JAPANESE INTERMEDIATE CODE: R371 |