JPS6364963A - Carbon material and manufacture - Google Patents
Carbon material and manufactureInfo
- Publication number
- JPS6364963A JPS6364963A JP61205525A JP20552586A JPS6364963A JP S6364963 A JPS6364963 A JP S6364963A JP 61205525 A JP61205525 A JP 61205525A JP 20552586 A JP20552586 A JP 20552586A JP S6364963 A JPS6364963 A JP S6364963A
- Authority
- JP
- Japan
- Prior art keywords
- carbon material
- carbon
- graphitized
- resin
- particle size
- 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
- 239000003575 carbonaceous material Substances 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000011347 resin Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 21
- 229920001187 thermosetting polymer Polymers 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 18
- 239000005011 phenolic resin Substances 0.000 description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 238000000465 moulding Methods 0.000 description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229920001568 phenolic resin Polymers 0.000 description 7
- 239000000446 fuel Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 3
- 229910021397 glassy carbon Inorganic materials 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007849 furan resin Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
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) [Abstract] 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、炭素材及びその製造方法に関し、特にりん酸
型燃料電池セパレーター用炭素材及びその製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION "Field of Industrial Application" The present invention relates to a carbon material and a method for producing the same, and particularly to a carbon material for a phosphoric acid fuel cell separator and a method for producing the same.
「従来の技術」
りん酸型燃料電池は、りん酸を保持した電解質層とその
両側に配置した白金触媒を担持した多孔質電極基板を単
位セルとし、各単位セルをセパレーターを介して積層し
たものである。"Conventional technology" A phosphoric acid fuel cell is a unit cell consisting of an electrolyte layer holding phosphoric acid and a porous electrode substrate supporting a platinum catalyst placed on both sides of the electrolyte layer, and each unit cell is stacked with a separator in between. It is.
かかるセパレーターは、その両側面に形成する流通溝に
それぞれ供給される燃料ガスと酸化ガスを分離するため
の境界としての機能と単位セル間の接続導体としての機
能を必要とするため、その材料にはガス不透過性、電気
伝導性、機械的強度及び作動温度における耐りん酸性等
について優れた特性を有することが要求される。Such a separator needs to function as a boundary to separate the fuel gas and oxidizing gas supplied to the flow grooves formed on both sides of the separator, and as a connecting conductor between unit cells. is required to have excellent properties such as gas impermeability, electrical conductivity, mechanical strength, and phosphoric acid resistance at operating temperatures.
従来、この種のセパレーター材料としての炭素材の製造
方法としては、フェノール樹脂等の熱硬化性樹脂と黒鉛
粉末を混練し、熱ロールまたは熱プレスにて成形したの
ち、炭化処理する方法が例えば特開昭５９−１２７３７
７号公報及び特開昭６０−１５０５５９号公報に開示さ
れている。Conventionally, as a method for producing carbon materials as separator materials of this kind, there has been a method in which a thermosetting resin such as a phenol resin and graphite powder are kneaded, molded using a hot roll or hot press, and then carbonized. Kaisho 59-12737
No. 7 and Japanese Unexamined Patent Publication No. 150559/1983.
「発明が解決しようとする間ツ点」
前記特開昭５９−１２７３７７号公報及び特開昭６０−
１５０５５９号公報に記載されている方法により製造さ
れた炭素材は、ＩＩＩＩＮとしての熱硬化性樹脂の配合
割合が少ない場合は経時的にガス不遇過性が低下すると
いう問題があり、配合割合が多い場合は成形性が悪いた
め特殊な成形方法を必要とし、かつ焼成工程において亀
裂が入り易いという問題がある。"The shortcomings that the invention attempts to solve"
The carbon material produced by the method described in Publication No. 150559 has a problem in that gas inconvenience decreases over time when the proportion of the thermosetting resin as IIIN is low, and the proportion of the thermosetting resin as IIIN is high. However, since the moldability is poor, a special molding method is required, and cracks tend to occur during the firing process.
また、機械的強度が劣るため、電池を製造する際に破損
しやすいという作業性の問題等がある。In addition, since the mechanical strength is poor, there are problems with workability such as easy damage during battery manufacturing.
一方、フェノール樹脂等の熱硬化性樹脂そのものを板状
に成形したのち、焼成して炭素材とする方法も知られて
いる。しかし得られる炭素材はガス不透過性に優れたガ
ラス状の炭素質０ものであるが電気伝導性に問題がある
。On the other hand, a method is also known in which a thermosetting resin such as a phenol resin itself is formed into a plate shape and then fired to obtain a carbon material. However, the obtained carbon material is a glass-like carbonaceous material with excellent gas impermeability, but has a problem in electrical conductivity.
さらに、本発明者に係る特願昭６１−１１３２７０号に
は、熱硬化性樹脂３０〜９０重量％を結合材として、メ
ソカーボン小球体の黒鉛化物に配合し、これを板状に成
形し、炭化処理する炭素材の製造方法を提案しているが
、成形工程において細かい条件によるコントロールを必
要とするという問題点ををする。Furthermore, in Japanese Patent Application No. 113270/1983 filed by the present inventor, 30 to 90% by weight of a thermosetting resin is blended as a binder into a graphitized mesocarbon small sphere, and this is formed into a plate shape. Although we have proposed a method for producing carbon materials that undergoes carbonization treatment, there is a problem in that the molding process requires detailed control of conditions.
本発明は、前記の問題点に着目してなされたもので、成
形性が良く、ガス不遇過性、電気伝導性、機械的強度、
耐りん酸性等に優れ、かつ焼成の際に亀裂を生じない燃
料電池セパレーター用炭素材及びその製造方法を提供す
ることを目的とする。The present invention has been made in view of the above-mentioned problems, and has good moldability, gas-inhospitable property, electrical conductivity, mechanical strength, and
An object of the present invention is to provide a carbon material for a fuel cell separator that has excellent phosphoric acid resistance and does not cause cracks during firing, and a method for producing the same.
「問題点を解決するための手段」
本発明は、粒度が５０μｍ以下の、メンカーボン小球体
の黒鉛化物とガラス状炭素質とからなり、黒鉛質炭素が
５〜６０！Ｉ％である炭素材及びその製造方法である。"Means for Solving the Problems" The present invention consists of graphitized mencarbon small spheres and glassy carbon having a particle size of 50 μm or less, and the graphitic carbon contains 5 to 60 μm. I% carbon material and its manufacturing method.
以下に本発明について詳細に説明する。The present invention will be explained in detail below.
本発明において用いるメソカーボン小球体の黒鉛化物は
、石油系または石炭系のピッチを熱処理して得られるメ
ソカーボン小球体をろ過し、必要に応じて洗浄したのち
約２５００℃まで昇温加熱して黒鉛化したものである。The graphitized mesocarbon spherules used in the present invention are obtained by filtering the mesocarbon spherules obtained by heat-treating petroleum-based or coal-based pitch, washing if necessary, and heating the mesocarbon spherules to approximately 2500°C. It is graphitized.
このメソカーボン小球体の黒鉛化物の粒度は５０μｍ以
下であることが必要である。黒鉛化物の粒度が５０ＡＩ
＋ｍを超えると得られる炭素材の密度があがらず、ガス
不透過性、電気伝導性等の特性において満足したものに
ならない。The particle size of the graphitized mesocarbon spherules must be 50 μm or less. Particle size of graphitized material is 50AI
If it exceeds +m, the density of the carbon material obtained will not increase and the properties such as gas impermeability and electrical conductivity will not be satisfactory.
黒鉛化物の一部が凝集している時は粉砕機で粉砕したの
ち、分級して粒度を５０μｍ以下とするが通常は粉砕も
分級もしなくてよい。When a part of the graphitized material is agglomerated, it is crushed in a crusher and then classified to a particle size of 50 μm or less, but usually neither crushing nor classification is necessary.
本発明の炭素材は、前記メソカーボン小球体の黒鉛化物
とガラス状炭素質とからなり、黒鉛質炭素が５〜６０ｆ
ｆｉｆ１％のもので、りん酸型燃料電池のセパレーター
用材料として優れた機能を有している。The carbon material of the present invention is composed of a graphitized product of the mesocarbon small spheres and glassy carbon, and the graphitic carbon is 5 to 60 f.
It contains 1% fif and has an excellent function as a separator material for phosphoric acid fuel cells.
前記黒鉛質炭素が５重量％未膚のものは、電気伝導性が
不足し、６０重量％を超えるものは、ガス不遇過性、耐
りん酸性が低下するためりん酸型燃料電池のセパレータ
ー用材料として十分な性能を有するものが得られない。If the graphitic carbon content is less than 5% by weight, the electrical conductivity is insufficient, and if it exceeds 60% by weight, the gas inconvenience and phosphoric acid resistance decrease, so it is suitable for separator materials for phosphoric acid fuel cells. However, it is not possible to obtain a product with sufficient performance.
つぎに、本発明の製造方法について説明する。Next, the manufacturing method of the present invention will be explained.
本発明において用いる熱硬化性樹脂粉末は、フェノール
樹脂、フラン樹脂、キシレン樹脂等で、好ましくはフェ
ノール樹脂粉末であり、不活性ガス雰囲気下約１０００
℃の温度で炭化処理した時にガラス状炭素質になるもの
をいい、粒度５０μｍ以下、アスペクト比２以下である
ことが必要である０粒度５０μｍ、アスペクト比２を超
えると、得られる炭素材の密度があがらず、ガス不遇過
性、電気伝導性等の特性が満足すべきものにならない。The thermosetting resin powder used in the present invention is a phenol resin, a furan resin, a xylene resin, etc., preferably a phenol resin powder.
It refers to a material that becomes glassy carbonaceous when carbonized at a temperature of °C, and must have a particle size of 50 μm or less and an aspect ratio of 2 or less.If the particle size exceeds 50 μm and the aspect ratio is 2, the density of the resulting carbon material The temperature does not increase, and the properties such as gas inconvenience and electrical conductivity are not satisfactory.
また、本発明において用いる熱硬化性樹脂としては、好
ましくはフェノール樹脂であるが、その（ム、フラン樹
脂、キシレン樹脂、エポキシ樹脂、ポリイミド普封脂等
も使用可能である０通常、樹脂溶液または粉末状樹脂の
形で使用する。フェノール樹脂が好ましいのは成形体の
特性が優れていること、安価で取扱い易いこと等の理由
による。The thermosetting resin used in the present invention is preferably a phenol resin, but other resins such as phenol resin, furan resin, xylene resin, epoxy resin, polyimide resin, etc. can also be used. Usually, a resin solution or It is used in the form of a powdered resin.Phenol resins are preferred because they have excellent properties when molded, are inexpensive, and are easy to handle.
まず、熱硬化性樹脂溶液中にメンカーボン小球体の黒鉛
化物及び熱硬化性樹脂粉末を添加して良く混合したのち
、室温で放置して乾燥する。First, graphitized mencarbon spherules and thermosetting resin powder are added to a thermosetting resin solution, mixed well, and then left to dry at room temperature.
つぎに、前記混合物を熱ロールまたは熱プレス等を用い
て熱圧成形する。なお、望ましくは熱圧成形する前に前
記混合物を１００℃前後の温度で加熱して予備硬化し、
これを粉砕してから前記熱圧成形するのがよい、また、
前記樹脂溶液のかわりに粉末状樹脂を用い、これとメソ
カーボン小球体の黒鉛化物及び熱硬化性樹脂粉末を混合
して熱圧成形してもよい。Next, the mixture is hot-pressed using a hot roll, a hot press, or the like. Preferably, the mixture is pre-cured by heating at a temperature of around 100° C. before hot-pressing.
It is preferable to pulverize this and then carry out the above-mentioned hot press molding, and
A powdered resin may be used instead of the resin solution, and this may be mixed with a graphitized mesocarbon small sphere and a thermosetting resin powder, and the mixture may be hot-pressed.
つぎに、前記成形工程で製造された樹脂成形体を１５０
〜２００℃の温度に加熱して完全に硬化させたのち、約
１０００℃まで昇温加熱して炭化処理することにより炭
素材とする。Next, the resin molded body manufactured in the above molding process was
After completely curing by heating to a temperature of ~200°C, the material is heated to approximately 1000°C and carbonized to obtain a carbon material.
「実施例」 以下、実施例により本発明をさらに詳細に説明する。"Example" Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例１
不揮発分５６重量％、粘度１００ｃｐｓのフェノール樹
脂溶液（群栄化学■製ニレシトツブＰＬ−２２１１）と
、平均粒度が１０μｍであるメンカーボン小球体の黒鉛
化物及び平均粒度１５μ■、アスペクト比１．２のフェ
ノール樹脂粉末を、得られる炭素材中の黒鉛質炭素が２
０重量％になるように配合し、攪拌機にて均一に混合し
たのち、室温に放置して乾燥した。Example 1 A phenolic resin solution with a non-volatile content of 56% by weight and a viscosity of 100 cps (Nireshitotsubu PL-2211 manufactured by Gunei Chemical Co., Ltd.), a graphitized product of men carbon small spheres with an average particle size of 10 μm, and an average particle size of 15 μm and an aspect ratio of 1. The graphitic carbon in the carbon material obtained is 2.
The mixture was blended to a concentration of 0% by weight, mixed uniformly using a stirrer, and then left to dry at room temperature.
この混合物を乾燥機中で１時間加熱して予備硬化したの
ち粉砕した。この粉末を平板状の金型に供給し、熱プレ
スによりプレス温度１６０℃、プレス圧１００眩／−で
熱圧成形し、厚さ０．８ ｍ、幅３００■、長さ３００
籠の薄板にした。ついで、この薄板を１８０℃の温度で
１０時間加熱してフェノール樹脂を硬化させたのち、黒
鉛板に挟んで１０℃／時の昇温速度で１０００℃まで昇
温して炭化処理し炭素材を得た。This mixture was precured by heating in a dryer for 1 hour and then ground. This powder was supplied to a flat mold and hot pressed at a press temperature of 160°C and a press pressure of 100/- to form a mold with a thickness of 0.8 m, a width of 300 cm, and a length of 300 cm.
I made it into a thin board for the basket. Next, this thin plate was heated at a temperature of 180°C for 10 hours to harden the phenolic resin, and then placed between graphite plates and heated to 1000°C at a heating rate of 10°C/hour for carbonization treatment to form a carbon material. Obtained.
この炭素材の特性を第１表に示す、なお、成形時の成形
斑、炭化時の割れ等は発生しなかった。The properties of this carbon material are shown in Table 1. Furthermore, no molding spots during molding, no cracking during carbonization, etc. occurred.
実施例２
粉末状フェノール樹脂（群栄化学■製ニレシトツブＰ（
Ｇ） Ａ−２４００）と、実施例１と同じ黒鉛化物及び
フェノール樹脂粉末を、得られるＲｓ材中の黒鉛質炭素
が４０重量％になるように配合し、均一に混合したのち
、熱ロールを用いてロール温度１５０℃、ロール周速度
０．２ｍ／分でロール成形して厚さ０．８簡の薄板にし
た。この薄板を実施例１と同様に炭化処理して炭素材を
得た。この炭素材の特性を第１表に示す、なお、成形時
の成形斑、炭化時の割れ等は発生しなかった。Example 2 Powdered phenol resin (Nireshitotsubu P manufactured by Gunei Chemical Co., Ltd.)
G) A-2400), the same graphitized material and phenolic resin powder as in Example 1 were blended so that the graphitic carbon in the resulting Rs material was 40% by weight, and after uniformly mixing, a hot roll was applied. A thin plate having a thickness of 0.8 sheets was formed by roll forming at a roll temperature of 150° C. and a roll circumferential speed of 0.2 m/min. This thin plate was carbonized in the same manner as in Example 1 to obtain a carbon material. The properties of this carbon material are shown in Table 1. It should be noted that no molding spots during molding or cracking during carbonization occurred.
比較例１
実施例１と同じフェノール樹脂溶液、メソカーボン小球
体の黒鉛化物及びフェノール樹脂粉末を、得られる炭素
材中の黒鉛質炭素が７０重量０％になるように配合され
たものを実施例１と同様に処理して炭素材を得た。この
炭素材の特性を第１表に示す。Comparative Example 1 An example in which the same phenolic resin solution, graphitized mesocarbon small spheres, and phenolic resin powder as in Example 1 were blended so that the graphitic carbon in the obtained carbon material was 70% by weight. A carbon material was obtained by processing in the same manner as in 1. The properties of this carbon material are shown in Table 1.
比較例２
実施例２と同じ粉末状フェノール樹脂に平均粒度３００
μｍ、アスペクト比３のフェノール樹脂粉末３０重量％
を配合し黒鉛質炭素なしで実施例２と同様に処理して炭
素材を得たやごの炭素材の特性を第１表に示す。Comparative Example 2 The same powdered phenolic resin as in Example 2 with an average particle size of 300
μm, aspect ratio 3 phenolic resin powder 30% by weight
Table 1 shows the properties of the carbon material obtained by blending and processing in the same manner as in Example 2 without graphitic carbon.
第１表
「発明の効果」
以上述べた如く、本発明の炭素材は、球状をしたメソカ
ーボン小球体の黒鉛化物とガラス状炭素質とで構成した
ので、緻密で高強度ををし、りん酸型燃料電池のセパレ
ーター用材料として、ガス不透過性、電気伝導性、機械
的強度及び耐りん酸性の優れたものが得られた。また、
本発明の炭素材の製造方法は、球状をしたメソカーボン
小球体の黒鉛化物と熱硬化性樹脂粉末を骨材としている
ため、成形性に優れ、かつ焼成の際、亀裂や反り、を発
生しないので、安定して高品質の炭素材が製造できると
いう効果がある。Table 1 "Effects of the Invention" As stated above, the carbon material of the present invention is composed of graphitized spherical mesocarbon small spheres and glassy carbon, so it is dense, has high strength, and is phosphorescent. A separator material for acid fuel cells with excellent gas impermeability, electrical conductivity, mechanical strength, and phosphoric acid resistance was obtained. Also,
The carbon material manufacturing method of the present invention uses graphitized spherical mesocarbon spherules and thermosetting resin powder as aggregates, so it has excellent moldability and does not cause cracks or warping during firing. Therefore, there is an effect that a high quality carbon material can be produced stably.
Claims (2)
鉛化物とガラス状炭素質とからなり、黒鉛質炭素が５〜
６０重量％である炭素材。(1) Consists of graphitized mesocarbon small spheres and glassy carbonaceous material with a particle size of 50 μm or less, with 5 to 50% of graphitic carbon.
The carbon material is 60% by weight.
黒鉛化物と熱硬化性樹脂粉末と熱硬化性樹脂とを、得ら
れる炭素材中の黒鉛質炭素が５〜６０重量％になるよう
に配合し、混練し、加圧、加熱下で成形し、１５０〜２
００℃の温度に加熱して硬化したのち炭化処理すること
を特徴とする炭素材の製造方法。(2) Graphitized mesocarbon small spheres with a particle size of 50 μm or less, thermosetting resin powder, and thermosetting resin are blended so that the resulting carbon material contains 5 to 60% by weight of graphitic carbon. , kneaded, molded under pressure and heat,
A method for producing a carbon material, which comprises heating the material to a temperature of 0.000C to harden it, and then subjecting it to carbonization treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61205525A JPS6364963A (en) | 1986-09-01 | 1986-09-01 | Carbon material and manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61205525A JPS6364963A (en) | 1986-09-01 | 1986-09-01 | Carbon material and manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6364963A true JPS6364963A (en) | 1988-03-23 |
Family
ID=16508325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61205525A Pending JPS6364963A (en) | 1986-09-01 | 1986-09-01 | Carbon material and manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6364963A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63222072A (en) * | 1987-03-12 | 1988-09-14 | 住友金属工業株式会社 | Impermeable carbon material |
| JP2005281100A (en) * | 2004-03-30 | 2005-10-13 | Jfe Chemical Corp | Method for manufacturing carbon material, negative electrode material for rechargeable lithium-ion battery, negative electrode for rechargeable lithium-ion battery, and rechargeable lithium-ion battery |
-
1986
- 1986-09-01 JP JP61205525A patent/JPS6364963A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63222072A (en) * | 1987-03-12 | 1988-09-14 | 住友金属工業株式会社 | Impermeable carbon material |
| JP2005281100A (en) * | 2004-03-30 | 2005-10-13 | Jfe Chemical Corp | Method for manufacturing carbon material, negative electrode material for rechargeable lithium-ion battery, negative electrode for rechargeable lithium-ion battery, and rechargeable lithium-ion battery |
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