JPS5978914A - Manufacture of special carbonaceous material - Google Patents
Manufacture of special carbonaceous materialInfo
- Publication number
- JPS5978914A JPS5978914A JP57190056A JP19005682A JPS5978914A JP S5978914 A JPS5978914 A JP S5978914A JP 57190056 A JP57190056 A JP 57190056A JP 19005682 A JP19005682 A JP 19005682A JP S5978914 A JPS5978914 A JP S5978914A
- Authority
- JP
- Japan
- Prior art keywords
- coke
- calcined
- raw
- pitch coke
- pitch
- 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.)
- Granted
Links
Abstract
Description
【発明の詳細な説明】
本発明は高密度、高強度かつ高純度で高耐酸化の特殊炭
素材の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a special carbon material with high density, high strength, high purity, and high oxidation resistance.
詳言スれば、生ピツチコークスとか焼ピッチコークスと
の配合物を主組成とし、これらに粘結剤を添加して加熱
混練した後、常法により粉砕、成型、焼成を行ないさら
に必要に応じて黒鉛化することを特徴とするものである
。In detail, the main composition is a mixture of raw pitch coke and calcined pitch coke, and after adding a binder and kneading with heat, it is crushed, molded, and calcined by conventional methods, and further processed as necessary. It is characterized by graphitization.
本発明で得られる炭素材は、メカ二カMシール、パフキ
ング材等の機械用、放電加工用電極等の電気用、鋳型、
Mツボ、ヒーターなどの耐熱用、化学用、半導体用もあ
るいは原子力用などの広範囲の分野で、使用できるもの
である。The carbon material obtained by the present invention can be used for mechanical purposes such as mechanical M seals and puffing materials, for electrical purposes such as electrodes for electrical discharge machining, for molds,
It can be used in a wide range of fields, including heat-resistant applications such as M pots and heaters, chemical applications, semiconductor applications, and nuclear power applications.
従来、炭素材の骨材としては、か焼石油コークス、が焼
ピッチコークスおよびそれらにカーボンブラックを配合
したものが使用されてきた。Conventionally, calcined petroleum coke, calcined pitch coke, and combinations thereof with carbon black have been used as carbon material aggregates.
しかしながら、か焼石油コークス、か焼ピッチコークス
を主体とした炭素材は、ヒツチ含浸及び炭化焼成を繰返
して行なうことにより嵩比重と強度とを向上させていた
ため高価なものとなっていた。しかも、特にピッチ含浸
部分は難黒鉛化性であるため、黒鉛化処理温度を高くす
る必要があシ1機械加工性も悪くなる欠点があった。However, carbon materials mainly composed of calcined petroleum coke and calcined pitch coke have been expensive because their bulk specific gravity and strength have been improved by repeatedly performing hit impregnation and carbonization and calcination. Furthermore, since the pitch-impregnated portion is difficult to graphitize, it is necessary to increase the graphitization temperature, which also has the drawback of poor machinability.
このような従来法の欠点を解消すべく、本発明者らは先
に特願昭51−52910号(特開昭52−18809
8号)をもって、下記の通りの発明を特徴とする特許出
願をなしている。In order to eliminate such drawbacks of the conventional method, the present inventors previously filed Japanese Patent Application No. 51-52910 (Japanese Unexamined Patent Publication No. 52-18809).
No. 8), we have filed a patent application featuring the following invention.
すなわち、上記の本発明者らが提案[7た特許出願の特
許請求の範囲は、平均粒径が15ミクロン以下の生石油
コークスと、平均粒径が44ミクロン以下のか焼コ−ク
スとを主体とした配合物に粘結剤を添加して混練し、常
法により粉砕し型押し成形し焼成を行ない、さらに必要
に応じて黒鉛化することを特徴とする特殊炭素相の製造
方法である。That is, the claims of the patent application proposed by the present inventors [7] mainly include raw petroleum coke with an average particle size of 15 microns or less and calcined coke with an average particle size of 44 microns or less. This is a method for producing a special carbon phase, which is characterized by adding a binder to the mixture, kneading it, pulverizing it by a conventional method, press-molding it, sintering it, and further graphitizing it if necessary.
この発明は、生石油コークスがこれを主原料として続出
した炭素又は黒鉛製品は焼成時において、大きな収縮性
を有すること、並びにか焼コークスの焼成時における安
定性を有することに着眼してなされたものであり、生石
油コークスとか焼コークスを主体とした配合物を骨材と
し、これらにコールタールピッチ、石油ヒノLあるいは
フニノール樹脂、フランa刊旨、ポリエチレン(耐脂な
どの合成樹脂粘結剤を添加して混練し、と11、i−粉
砕したのちに型押し成形し焼成さらに必要に応じて黒鉛
化することにより、高密度がつ高強度の特殊炭素材が容
易に得られるものである。This invention was made based on the fact that carbon or graphite products, which have been produced using raw petroleum coke as the main raw material, have a large shrinkage property during firing, and that calcined coke has stability during firing. The aggregate is a mixture mainly composed of raw petroleum coke and calcined coke, and these are combined with coal tar pitch, petroleum Hino L or Funiol resin, Furan A publication, and polyethylene (grease-resistant and other synthetic resin binders). A special carbon material with high density and high strength can be easily obtained by adding and kneading, pulverizing, pressing, firing, and graphitizing if necessary. .
しかしながら、上記発明の主原料である生石油コークス
は、石油重質油の高温熱分解によって製造されているた
め、この石油重質油は、くり返しの高温熱分解等により
、この種の特殊炭素相の構成物質として必要な芳香族の
炭素化合物の含有量が少なく、その構成物質としでは好
1しくない脂肪族系の炭素化合物の含有量が比較的多い
。よって、これから得られる生石油コークスを使用して
特殊炭素材を製造した場合、生石油コークスとコールク
−ルピッチとの境界面における、混線時又は、焼成時の
相容性が悪いことが判明した。However, raw petroleum coke, which is the main raw material of the above invention, is produced by high-temperature pyrolysis of heavy petroleum oil. The content of aromatic carbon compounds, which are necessary as constituent substances, is small, and the content of aliphatic carbon compounds, which are not desirable as constituent substances, is relatively large. Therefore, when a special carbon material is manufactured using raw petroleum coke obtained from the raw petroleum coke, it has been found that the compatibility between the raw petroleum coke and the coal cool pitch is poor at the time of crosstalk or during calcination.
寸だ、石油重質油を出発原料としているため、イオウ、
チタン、バナジウム等灰分の含有量が比較的多いことよ
り、次に示すような欠点が生ずることも判明した。Because the starting material is heavy petroleum oil, sulfur,
It has also been found that the relatively high content of ash such as titanium and vanadium causes the following drawbacks.
すなわち、イオウ等の化合物が介在することにより、均
一な黒鉛の構造の形成が一部阻害されること、並びにこ
の種の特殊炭素材の用途として最近注目されその需要が
増大している半導体製重用lレツホや治具などにおいて
は、灰分などの不純物が混入婆れていることは極力避け
なけハばならず、又、耐酸化性を低トさせる原因の一つ
である、バナジウム等が含有されているため、必要以上
の高純度化処理をする必要があった。In other words, the presence of compounds such as sulfur partially inhibits the formation of a uniform graphite structure, and the use of this type of special carbon material has recently attracted attention and its demand is increasing for heavy-duty semiconductor manufacturing. l In retsuho and jigs, it is essential to avoid contamination with impurities such as ash as much as possible, and vanadium, etc., which is one of the causes of low oxidation resistance, must be avoided. Therefore, it was necessary to perform purification treatment higher than necessary.
そこで、本発明者らは、上記生石油コークスに代えてこ
れらの欠点を有しないこの種の原料と1〜で、生ヒツチ
コークス及びか焼ピッチコークスを用いることを思いつ
き、微粒子状の生ピツチコークス及びか焼ヒツチコーク
スを用いた特殊炭素材の製造方法を改良工夫した。Therefore, the present inventors came up with the idea of using raw hitch coke and calcined pitch coke in place of the raw petroleum coke described above, which do not have these drawbacks. We have improved the method for producing special carbon materials using burnt hitch coke.
これにより、従来法の欠点をすべて解消することのでき
る特殊炭素材の製造方法を提供するものである。This provides a method for producing a special carbon material that can eliminate all the drawbacks of conventional methods.
以[5、本発明を実施例などに基いて詳細に説明する。Hereinafter, the present invention will be described in detail based on examples and the like.
すなわち、本発明は、前記特許請求の範囲に記載の通り
、平均粒子径が15ミクロン以下の生ピツチコークスと
、平均粒子径が44ミクロン以下のか焼ピッチコークス
とを主体とした配合物に粘結材として、コールクールピ
ッチを添加して混練し、常法により粉砕し成型し焼成を
付ない坏1)に必要に応じて黒鉛化することを特徴とす
る特殊炭素材の製造方法を提供するものである。That is, as described in the above claims, the present invention provides a blend consisting mainly of raw pitch coke with an average particle diameter of 15 microns or less and calcined pitch coke with an average particle diameter of 44 microns or less, and a caking agent. The present invention provides a method for producing a special carbon material, which comprises adding coal cool pitch, kneading it, crushing it by a conventional method, molding it, and graphitizing it as needed without calcination (1). be.
ぞして、本発明の特徴とするところは、特殊炭素材の1
:、原料として、生ピツチコークスと、か焼ピッチコー
クスとを使用−4ることにより、両原朱1の微粒子とコ
ールタールピッチとの杜若性などを改善し黒鉛の構造の
j陶1−1素材内の均一性を一段と向上さセることによ
り、先のつ1′、明の生石油コークスとか焼コークスと
の組合せ原車)では得られなかった高耐酸化性及び高強
度かつ高密で、高純度の特殊炭素材を得ることに成功l
〜だものである。Therefore, the feature of the present invention is that one of the special carbon materials is
: By using raw pitch coke and calcined pitch coke as raw materials, the firmness etc. of the fine particles of Ryohara Shu 1 and coal tar pitch are improved, and the material with a graphite structure is created. By further improving the uniformity within the coke, we are able to produce high oxidation resistance, high strength, high density, and Succeeded in obtaining special carbon material with high purity
~ is something.
本発明で使用される生ピツチコークスは、石炭の高温乾
留により回収されたコールタールをディレートコ−カー
によりコークス化温度に加熱し、製造されるものである
。The raw pitch coke used in the present invention is produced by heating coal tar recovered by high-temperature carbonization of coal to a coking temperature in a dilate coker.
石炭の高温乾留では、灰分の大半は石炭コークスに残り
、回収されたコールタ−1しには灰分は殆んど含有され
ない。したがつてこのコールタールをノベインダー用に
調整したコールタールピッチバインダーは、低灰分であ
りかつ黒鉛構造を形成する物質として好ましい芳香族の
炭素化合物に富んでいる。In high-temperature carbonization of coal, most of the ash remains in the coal coke, and the recovered coulter 1 contains almost no ash. Therefore, the coal tar pitch binder prepared from this coal tar for Novinder has a low ash content and is rich in aromatic carbon compounds which are preferable as substances forming graphite structures.
丑だ、コールタールから得られた生ヒツチコークスは、
力lレザイナーによりか焼され、か焼ピッチ] −りy
、 トなる。よって、コールタールピッチ、生ヒツチコ
ークス、か焼ピンチコークスはともに非常に似かまった
構造を示す。生ピツチコークスとか焼ヒツチコークスに
コールタールヒツチを添加混合する加熱混合の過程にお
(/′1て、両コークス微粒子とパインターピッチの境
界面でのなじみは生石油コークスの場合に比較し非常に
よくなる。つ甘り、生ピツチコークス中の芳香族系炭素
化合物などが混線中あるいは焼成時に留出し、すなわち
+11容が起り、各粒子の境界面における結合は強固な
ものとなり、よシ均一かつ高密度、高強度の炭素材が得
られるものである。Raw hitch coke obtained from coal tar is
Calcined by force l resiner, calcined pitch] -riy
, Tonaru. Therefore, coal tar pitch, raw hitch coke, and calcined pinch coke all exhibit very similar structures. During the heating and mixing process of adding and mixing coal tar hitch to raw pitchcoke and calcined hitch coke (/'1), the compatibility at the interface between the fine particles of both cokes and pinter pitch is much better than in the case of raw petroleum coke. In other words, aromatic carbon compounds in the raw pitchcoke are distilled out during mixing or during firing, resulting in a +11 volume, and the bonding at the interface between each particle becomes strong, resulting in a more uniform and dense coke. A high-strength carbon material can be obtained.
1だ、生ヒツチコークス、か焼ピッチコークスのいずれ
にもイオウ等の灰分も少ないため、欠陥の少ない黒鉛構
造形成は容易に行なえる。First, since both raw hitch coke and calcined pitch coke have low ash content such as sulfur, it is easy to form a graphite structure with few defects.
また、本発明のように灰分のきわめて少ない生ピンチコ
ークスとか焼ピッチコークスとを主原料として、特殊炭
素材を製造す乙と、高純度、高耐酸化性のものが得られ
る。Furthermore, as in the present invention, a special carbon material is produced using raw pinch coke and calcined pitch coke with extremely low ash content as main raw materials, and a material with high purity and high oxidation resistance can be obtained.
このように本発明によれば、非常に欠陥の少ない高密度
でかつ高強度、また高純度で高耐酸化性の特殊炭素相が
得られる。As described above, according to the present invention, a special carbon phase having high density, high strength, high purity, and high oxidation resistance with very few defects can be obtained.
なお1本発明において生ピツチコークスの平均粒度を、
15ミクL1ン以下にする用j出は、生ピツチコークス
の平均粒度が15ミクロン以上になると、粒子自身が収
縮を起こすため高密度でかつ高強度の炭素材又は黒鉛累
月か得られないからである。In addition, in the present invention, the average particle size of raw pitch coke is
The reason why the average particle size of raw pitch coke is less than 15 microns is because if the average particle size of raw pitch coke exceeds 15 microns, the particles themselves will shrink, making it impossible to obtain a high-density and high-strength carbon material or graphite material. be.
他方、か焼ヒソナコークスの平均粒径を44ミクロン以
下にする理由は、これ以上の粒径になると組織の均一な
収縮が阻害され、高密でかつ高強度のものが得られなく
なるからである。On the other hand, the reason why the average particle size of the calcined Hisona coke is set to 44 microns or less is that if the particle size is larger than this, uniform contraction of the structure will be inhibited, making it impossible to obtain a highly dense and high-strength coke.
次に、本発明の実施例について説明する。Next, examples of the present invention will be described.
実施例1
平均粒径5ミクロンの生ピツチコークス80部と平均粒
径44ミクロンのか焼ピッチコークス20部との配合物
にコールタールピンチ52部を添加しニーダ−中で22
0℃で1時間加熱混練した。この混線物を常法によシ粉
砕し、成形し、焼成し、黒鉛化した。かくして得られた
製品の物性及び特性値は前記の表に示す通りである。Example 1 52 parts of coal tar pinch was added to a blend of 80 parts of raw pitch coke with an average particle size of 5 microns and 20 parts of calcined pitch coke with an average particle size of 44 microns, and the mixture was heated in a kneader for 2 hours.
The mixture was heated and kneaded at 0°C for 1 hour. This mixed wire material was pulverized by a conventional method, molded, fired, and graphitized. The physical properties and characteristic values of the product thus obtained are as shown in the table above.
実施例2
平均粒径1(1ミクロンの生ピツチコークス80部と平
均粒径48ミクυンのか焼ピンチコークス20部との配
合物にコールタールピッチ49部を添加した。以−ト実
施例1表同様にして製品を得た。かくして得らねた製品
の物性及び特性値は[−記の表に示す通りである。Example 2 49 parts of coal tar pitch was added to a blend of 80 parts of raw pitch coke with an average particle size of 1 micron and 20 parts of calcined pinch coke with an average particle size of 48 microns. A product was obtained in the same manner.The physical properties and characteristic values of the product thus obtained are as shown in the table marked with [-].
実施例3
〕ド・均粒径5ミクロンの化ヒツチコークス20部と平
均粒径44−、クロン80部との配合物にコールタ−ル
ビノナ47部を添加した。以下実施例1と同様にして製
品を得た。かくし2て得しれた製品の物性及び特性値は
l′記の表に示す通りである。Example 3 47 parts of coal tar rubinona was added to a blend of 20 parts of converted hitch coke with an average particle size of 5 microns and 80 parts of coke with an average particle size of 44 microns. A product was obtained in the same manner as in Example 1. The physical properties and characteristic values of the product thus obtained are as shown in the table 1'.
(比較例)
平均粒径5ミクY1ンの生石油コークス80部と平均粒
径44ミクロンの石油コークス20部との配合物にコー
ルタールヒツチ58部を添加1〜た。以下実施例1と同
様にして製品を得た。かくして得られた製品の物性及び
特性イnK rJ、ト記の表に示す通りである。(Comparative Example) 58 parts of coal tar hit was added to a blend of 80 parts of raw petroleum coke with an average particle diameter of 5 microns and 20 parts of petroleum coke with an average particle diameter of 44 microns. A product was obtained in the same manner as in Example 1. The physical properties and characteristics of the product thus obtained are as shown in the table below.
製品の物性及び特性値表
以上の結果から明らかなように、本発明の特殊炭素材の
製造方法によれば、見掛比り、(密度)が大きく、それ
ゆえ抗折力が大きく、バナジウム(灰分)などの不和1
物の含有fkが少なく、かつ酸化消耗が少ない品質特性
の優れた炭素相(黒鉛累月)を得ることかできる。Table of Physical Properties and Characteristic Values of the Product As is clear from the above results, according to the manufacturing method of the special carbon material of the present invention, the apparent ratio (density) is large, the transverse rupture strength is large, and vanadium ( Discord 1 such as ash content
It is possible to obtain a carbon phase (graphite crystal) with excellent quality characteristics, which contains less fk and less oxidative consumption.
特許出願人の名称 揖斐川電気工業株式会社 代表者多賀潤一部Patent applicant name Ibigawa Electric Industry Co., Ltd. Representative Jun Taga
Claims (1)
均粒径が44ミクロン以下のか焼ピッチコークスとを主
体とした配合物に粘結剤を添加して混練し、常法により
粉砕し成型し焼成を行ない黒鉛化することを特徴とする
特殊炭素材の製造方法。A blend consisting mainly of raw pitch coke with an average particle size of 15 microns or less and calcined pitch coke with an average particle size of 44 microns or less is kneaded with a binder added, and then crushed, molded, and fired using a conventional method. A method for producing a special carbon material, which is characterized by graphitizing the material.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57190056A JPS5978914A (en) | 1982-10-28 | 1982-10-28 | Manufacture of special carbonaceous material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57190056A JPS5978914A (en) | 1982-10-28 | 1982-10-28 | Manufacture of special carbonaceous material |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3137878A Division JPH0764635B2 (en) | 1991-06-10 | 1991-06-10 | Special carbon material composition |
JP3137877A Division JPH04228411A (en) | 1991-06-10 | 1991-06-10 | Composition for specific carbon material |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5978914A true JPS5978914A (en) | 1984-05-08 |
JPS6323124B2 JPS6323124B2 (en) | 1988-05-14 |
Family
ID=16251603
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP57190056A Granted JPS5978914A (en) | 1982-10-28 | 1982-10-28 | Manufacture of special carbonaceous material |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5978914A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6325273A (en) * | 1986-07-17 | 1988-02-02 | イ−グル工業株式会社 | Manufacture of silicon carbide-carbonaceous composite formed body |
JPH07187878A (en) * | 1992-03-24 | 1995-07-25 | Tokai Carbon Co Ltd | Graphite crucible for production of silicon single crystal |
EP2432052A1 (en) * | 2009-05-15 | 2012-03-21 | Nippon Steel Chemical Co., Ltd. | Anode active material for lithium secondary batteries, anode electrode for lithium secondary batteries, in-vehicle lithium secondary battery using said anode active material and anode electrode, and method for manufacturing an anode active material for lithium secondary batteries |
CN102428594A (en) * | 2009-05-15 | 2012-04-25 | 新日铁化学株式会社 | Anode active material for lithium secondary batteries, anode electrode for lithium secondary batteries, in-vehicle lithium secondary battery using said anode active material and anode electrode, and method for manufacturing an anode active material for lithium secondary batteries |
CN102468484A (en) * | 2010-11-12 | 2012-05-23 | 新日铁化学株式会社 | Negative electrode active material of lithium secondary battery, secondary battery using the same, method for manufacturing the same |
CN102640330A (en) * | 2009-12-02 | 2012-08-15 | 新日铁化学株式会社 | Negative electrode for secondary battery, and secondary battery using same |
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JPS5358496A (en) * | 1976-11-05 | 1978-05-26 | Agency Of Ind Science & Technol | Production of graphite substrate for oxidation resistant coating |
JPS6013962A (en) * | 1983-07-05 | 1985-01-24 | Teikei Kikaki Kk | Carburettor |
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1982
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JPS50118986A (en) * | 1974-03-02 | 1975-09-18 | ||
JPS52133098A (en) * | 1976-04-30 | 1977-11-08 | Ibiden Co Ltd | Production of special carbon material |
JPS5358496A (en) * | 1976-11-05 | 1978-05-26 | Agency Of Ind Science & Technol | Production of graphite substrate for oxidation resistant coating |
JPS6013962A (en) * | 1983-07-05 | 1985-01-24 | Teikei Kikaki Kk | Carburettor |
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JPS6325273A (en) * | 1986-07-17 | 1988-02-02 | イ−グル工業株式会社 | Manufacture of silicon carbide-carbonaceous composite formed body |
JPH07187878A (en) * | 1992-03-24 | 1995-07-25 | Tokai Carbon Co Ltd | Graphite crucible for production of silicon single crystal |
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CN102428594A (en) * | 2009-05-15 | 2012-04-25 | 新日铁化学株式会社 | Anode active material for lithium secondary batteries, anode electrode for lithium secondary batteries, in-vehicle lithium secondary battery using said anode active material and anode electrode, and method for manufacturing an anode active material for lithium secondary batteries |
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EP2432052A4 (en) * | 2009-05-15 | 2014-01-22 | Nippon Steel & Sumikin Chem Co | Anode active material for lithium secondary batteries, anode electrode for lithium secondary batteries, in-vehicle lithium secondary battery using said anode active material and anode electrode, and method for manufacturing an anode active material for lithium secondary batteries |
US9806342B2 (en) * | 2009-05-15 | 2017-10-31 | Nippon Steel & Sumikin Chemical Co., Ltd. | Negative electrode active material of lithium secondary battery, negative electrode of lithium secondary battery, lithium secondary battery for vehicle installation using the negative electrode active material and negative electrode, and method for manufacturing the negative electrode active material |
CN102640330A (en) * | 2009-12-02 | 2012-08-15 | 新日铁化学株式会社 | Negative electrode for secondary battery, and secondary battery using same |
CN102468484A (en) * | 2010-11-12 | 2012-05-23 | 新日铁化学株式会社 | Negative electrode active material of lithium secondary battery, secondary battery using the same, method for manufacturing the same |
US9070933B2 (en) | 2010-11-12 | 2015-06-30 | Nippon Steel Chemical Co., Ltd. | Negative electrode active material of lithium secondary battery, secondary battery using the same, method for manufacturing the same |
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