JPH10294101A - Graphite for lithium secondary battery cathode and manufacture of same - Google Patents

Graphite for lithium secondary battery cathode and manufacture of same

Info

Publication number
JPH10294101A
JPH10294101A JP9116351A JP11635197A JPH10294101A JP H10294101 A JPH10294101 A JP H10294101A JP 9116351 A JP9116351 A JP 9116351A JP 11635197 A JP11635197 A JP 11635197A JP H10294101 A JPH10294101 A JP H10294101A
Authority
JP
Japan
Prior art keywords
graphite
secondary battery
lithium secondary
particle size
negative electrode
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
Application number
JP9116351A
Other languages
Japanese (ja)
Other versions
JP3683379B2 (en
Inventor
Toshihiko Funabashi
敏彦 船橋
Ryoji Uchimura
良治 内村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Mineral Co Ltd
Original Assignee
Kawatetsu Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kawatetsu Mining Co Ltd filed Critical Kawatetsu Mining Co Ltd
Priority to JP11635197A priority Critical patent/JP3683379B2/en
Publication of JPH10294101A publication Critical patent/JPH10294101A/en
Application granted granted Critical
Publication of JP3683379B2 publication Critical patent/JP3683379B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

PROBLEM TO BE SOLVED: To provide graphite for a lithium secondary battery cathode which can be stably manufactured, has a characteristic equal to natural graphite or more, has a short inter-layer distance and a large crystal size, and its manufacture. SOLUTION: Products having a particle size more than 0.044 mm, are gathered from products which mainly contain graphite generated by a cooling process of molten pig iron of hypereutectic composition, then refined, further ground and screened, thus obtained flake graphite which contains C more than 99%, and has average particle size more than 0.005 mm, an inter-layer distance less than 3.37 Å, crystal size more than 1000 Å is used as graphite for lithium secondary battery cathode.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する分野】本発明はリチウム二次電池負極用
黒鉛及びその製造方法に係り、特に放電容量および初期
充放電効率の高い黒鉛及びその製造方法に関する。
The present invention relates to graphite for a negative electrode of a lithium secondary battery and a method for producing the same, and more particularly to graphite having a high discharge capacity and high initial charge / discharge efficiency and a method for producing the same.

【0002】[0002]

【従来の技術】近年の電子機器のポータブル化、コード
レス化が進むにしたがい、これら機器の電源として小型
・軽量かつ高エネルギー密度の高性能二次電池の開発が
急がれ、その要望に応えるものとしてリチウム二次電池
が提供されている。かかる二次電池用の負極材料には炭
素質材料が使用されるが、中でも特公昭62−2343
3号公報に記載されるように、黒鉛の優位性が認められ
てきている。この黒鉛質負極材料の特性としてはその層
間距離(d)が小さいほど、またその結晶子の大きさ
(Lc)が大きいほど二次電池の放電容量が大きく、初
期充放電効率が大きいことが明らかとなっており、優れ
た性質を持った天然黒鉛の探索や、あるいは人造黒鉛の
製造条件の改良などが進められてきている。
2. Description of the Related Art In recent years, as electronic devices have become more portable and cordless, the development of high-performance secondary batteries of small size, light weight and high energy density has been urgently required as power supplies for these devices. Is provided as a lithium secondary battery. A carbonaceous material is used as a negative electrode material for such a secondary battery, and in particular, Japanese Patent Publication No. 62-2343.
As described in Japanese Patent Publication No. 3 (1999), the superiority of graphite has been recognized. As the characteristics of the graphite negative electrode material, it is clear that the smaller the interlayer distance (d) and the larger the crystallite size (Lc), the larger the discharge capacity of the secondary battery and the larger the initial charge / discharge efficiency. The search for natural graphite having excellent properties and the improvement of production conditions for artificial graphite have been promoted.

【0003】[0003]

【発明が解決しようとする課題】しかしながら、天然黒
鉛はたとえ優れた性質のものが発見されたとしても採掘
場所の変化などにより性質が変化し、安定して供給する
のが困難であり、一方、人造黒鉛は黒鉛の結晶性の発達
のために易黒鉛化炭素を2500℃以上の温度で熱処理
する必要があるが、それでもなお、放電容量が天然黒鉛
に及んでいないのが現状である。ちなみに天然黒鉛の放
電容量として370mAh/g、初期充放電効率92%
が報告されているのに対し、人造黒鉛の場合は最も良い
場合でも放電容量が350〜360mAh/g程度であ
る。これは人造黒鉛の黒鉛の結晶性が天然黒鉛より低い
ためであると推察されている。本発明は、従来技術の問
題点を解決することを目的とし、天然黒鉛相当あるいは
それよりすぐれた性質を有するリチウム二次電池負極材
料を工業製品として提供することを目的とし、安定して
放電容量、初期充放電効率の高い黒鉛質負極材料および
その製造方法を提供することを目的とする。
However, even if natural graphite is found to have excellent properties, its properties change due to changes in mining locations and the like, and it is difficult to supply natural graphite stably. For artificial graphite, it is necessary to heat-treat graphitizable carbon at a temperature of 2500 ° C. or more in order to develop the crystallinity of graphite, but at present, the discharge capacity is still lower than that of natural graphite. Incidentally, the discharge capacity of natural graphite is 370 mAh / g, and the initial charge / discharge efficiency is 92%.
Whereas, in the case of artificial graphite, the discharge capacity is about 350 to 360 mAh / g at best. This is presumed to be due to the lower crystallinity of artificial graphite than natural graphite. The present invention aims to solve the problems of the prior art, and aims to provide a lithium secondary battery negative electrode material having properties equivalent to or superior to natural graphite as an industrial product, with a stable discharge capacity. It is another object of the present invention to provide a graphite negative electrode material having a high initial charge / discharge efficiency and a method for producing the same.

【0004】[0004]

【課題を解決するための手段】本発明者等は、リチウム
二次電池負極用黒鉛について種々の材料を検討した結
果、製鉄工程において発生するいわゆるキッシュグラフ
ァイトが上記リチウム二次電池負極用黒鉛として非常に
好ましい性質を有していることに着目し、その利用手段
について研究した結果、本発明を完成したものである。
The inventors of the present invention have studied various materials for graphite for a negative electrode of a lithium secondary battery, and have found that so-called kish graphite generated in the iron making process is very useful as the graphite for the negative electrode of a lithium secondary battery. The present invention has been completed as a result of studying the means of using the same, focusing on the fact that it has favorable properties.

【0005】本発明は、リチウム二次電池負極用黒鉛
を、過共晶組成の溶融銑鉄の冷却過程において生ずる鱗
状黒鉛を主として含む生成物を処理して得た、Cを99
%以上含有し、平均粒度が0.005mm以上であり、
かつ層間距離(d)3.37Å以下、結晶子の大きさ
(La)1000Å以上の鱗状黒鉛とするものであり、
またその製造方法として、過共晶溶融銑鉄の冷却過程で
得られる鱗状黒鉛を主として含有する生成物のうち粒径
が0.044mmのものを回収し、化学処理を行なって
Cを99%以上するように精製し、しかる後粉砕と篩い
分けを行なって平均粒度0.005mm以上、層間距離
(d)3.37Å以下、結晶子の大きさ(La)100
0Å以上の鱗状黒鉛を得るものである。またこの際、過
共晶溶融銑鉄には高炉溶銑を用い、冷却過程で得られる
生成物には製鉄ダスト、いわゆるキッシュグラファイト
を利用するものである。
According to the present invention, a graphite for a negative electrode of a lithium secondary battery is obtained by treating a product mainly containing scaly graphite generated in a cooling process of molten pig iron having a hypereutectic composition, and C is obtained as 99%.
% Or more, the average particle size is 0.005 mm or more,
And a scale-like graphite having an interlayer distance (d) of 3.37 ° or less and a crystallite size (La) of 1000 ° or more;
In addition, as a method for producing the same, a product having a particle size of 0.044 mm is recovered from a product mainly containing scale graphite obtained in a cooling process of hypereutectic molten pig iron, and subjected to a chemical treatment to increase C to 99% or more. And then pulverized and sieved to obtain an average particle size of 0.005 mm or more, an interlayer distance (d) of 3.37 ° or less, and a crystallite size (La) of 100.
This is to obtain a scale graphite of 0 ° or more. At this time, blast furnace hot metal is used as the hypereutectic molten pig iron, and iron making dust, so-called Kish graphite, is used as a product obtained in the cooling process.

【0006】[0006]

【発明の実施の形態】本発明においては、過共晶組成の
溶融銑鉄の冷却過程で生ずる黒鉛を利用する。本発明者
等の調査によれば、かかる黒鉛は、鱗状黒鉛に属し、そ
の性状は、表1に示すとおりである。ここに表1は、高
炉による製鉄過程で得られる溶融銑鉄の冷却時に発生す
る製鉄ダスト、いわゆるキッシュグラファイトを精製し
篩分けた場合の粒径ごとの性状を示したものであるが、
キッシュグラファイトは黒鉛の層間距離(d)は3.3
7Å以下(実質的に3.36Å以下)となっており、ま
た結晶子の大きさ(Lc)はその粒径が0.044mm
以上のものを篩分けると2000Å以上となることが判
明した。かかる性状を有するキッシュグラファイトは、
従来知られている黒鉛の性状とその負極材としての特性
値の相関関係図を基に考察すれば、これが優れた負極材
となりうる可能性が示された。
BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, graphite produced in a cooling process of molten pig iron having a hypereutectic composition is used. According to the investigation by the present inventors, such graphite belongs to scaly graphite, and the properties thereof are as shown in Table 1. Here, Table 1 shows the properties for each particle size in the case of purifying and sieving iron-made dust, so-called quiche graphite, generated during cooling of molten pig iron obtained in the iron-making process by the blast furnace,
Kish graphite has an interlayer distance (d) of graphite of 3.3.
7 ° or less (substantially 3.36 ° or less), and the crystallite size (Lc) is 0.044 mm.
It was found that sieving of the above resulted in 2,000 mm or more. Kish graphite having such properties is
Consideration based on a correlation diagram between conventionally known properties of graphite and its characteristic value as a negative electrode material showed that this could be an excellent negative electrode material.

【0007】[0007]

【表1】 [Table 1]

【0008】キッシュグラファイトがかかる優れた性状
を呈する原因については、高温の溶融金属と一定の整合
性を保ちながら、かつ、溶融鉄の圧力下で黒鉛結晶が成
長することなどが考えられるが、正確な理由はなお不明
である。しかし、粒径が極めて小さいもの、具体的には
0.044mm未満のものは結晶子の大きさが比較的小
さく、リチウム二次電池負極用黒鉛として十分な特性の
向上が望めない上、不純物も多く精製コストもかかるの
で、本発明においてはキッシュグラファイトのうち粒径
が0.044mm以上のもののみを原料として使用す
る。
The reason why Kish graphite exhibits such excellent properties may be that graphite crystals grow under the pressure of the molten iron while maintaining a certain consistency with the high-temperature molten metal. The reason is still unknown. However, those having an extremely small particle size, specifically, those having a particle size of less than 0.044 mm, have relatively small crystallite sizes, and cannot be expected to have sufficiently improved characteristics as graphite for a negative electrode of a lithium secondary battery. In the present invention, only a Kish graphite having a particle size of 0.044 mm or more is used as a raw material because a large purification cost is required.

【0009】表2は上記によって得た粒径0.044m
m以上のキッシュグラファイトを化学処理によってCを
99%以上に精製し、それに対して粉砕と篩い分けを行
なって平均粒度0.005mm以上のリチウム二次電池
負極用黒鉛を得、その特性を調査した結果である。ここ
に示されるように、キッシュグラファイトから得た鱗状
黒鉛は最優秀の天然黒鉛に匹敵する二次電池負極材料特
性を示し、従来の人造黒鉛の性能を凌ぐものであった。
かかる結果は、高炉による製鉄過程で得られるキッシュ
グラファイトについて最初に認められたものであるが、
過共晶銑鉄の冷却過程で得られるキッシュグラファイト
全般に広く認められるものであることが確認されてい
る。従って、黒鉛としては上記製鉄過程で得られるキッ
シュグラファイトのほか、過共晶溶融銑鉄の冷却過程で
得られるキッシュグラファイトが広く利用できる。な
お、高炉による製鉄過程で発生するキッシュグラファイ
トは大量かつ、安価に得られるのでこれを利用するのが
経済的であることはいうまでもない。
Table 2 shows that the particle size obtained above was 0.044 m.
m is refined to 99% or more by chemical treatment, and then crushed and sieved to obtain graphite for an anode of a lithium secondary battery having an average particle size of 0.005 mm or more, and its characteristics were investigated. The result. As shown here, scaly graphite obtained from Kish graphite exhibited secondary battery negative electrode material properties comparable to the best natural graphite and surpassed the performance of conventional artificial graphite.
These results were first recognized for quiche graphite obtained in the steelmaking process with a blast furnace,
It has been confirmed that it is widely recognized in all quiche graphite obtained in the process of cooling hypereutectic pig iron. Therefore, as the graphite, in addition to the kish graphite obtained in the above iron making process, the kish graphite obtained in the cooling process of the hypereutectic molten pig iron can be widely used. In addition, it is needless to say that it is economical to use quiche graphite generated in the iron making process by the blast furnace in a large amount and at a low cost.

【0010】[0010]

【表2】 [Table 2]

【0011】上記生成物(キッシュグラファイト)は、
そのままでは不純物、すなわち鉄およびその酸化物、珪
素(Si)、カルシウム(Ca)その他製鉄過程で精錬
のため使用される副原料の微粉末などを多く含んでいる
ので、その除去を行い、純度を向上させる。一般に負極
材料として使用するには、C含有量を99%(重量比)
とすることが必要であるので、化学的処理を施して精製
する。化学的処理としては、浮選および塩酸、弗酸によ
る処理が含まれる。そのため特開昭63−151609
号公報記載の方法を用いることができる。
The above product (quiche graphite)
As it is, it contains many impurities, that is, iron and its oxides, silicon (Si), calcium (Ca), and other fine powders of secondary materials used for refining in the iron making process. Improve. Generally, for use as a negative electrode material, the C content is 99% (weight ratio)
Therefore, it is subjected to a chemical treatment for purification. The chemical treatment includes flotation and treatment with hydrochloric acid and hydrofluoric acid. Therefore, Japanese Patent Application Laid-Open No. 63-151609
Can be used.

【0012】化学処理されたキッシュグラファイトはさ
らに適当なミル(例えばボールミル)等によって粉砕を
行ない、篩い分けをする。これらの工程は、平均粒度が
0.005mm以上となるように、かつ使用されるリチ
ウム二次電池負極材料の要求特性に応じて行なえばよ
い。なお、平均粒度を0.005mm未満としないよう
にするのは、かかる粒度のものは一般に負極材料として
も特性値が好ましくなく、また取り扱い上不便だからで
ある。
The chemically treated quiche graphite is further pulverized by a suitable mill (for example, a ball mill) or the like, and sieved. These steps may be performed so that the average particle size is 0.005 mm or more, and according to the required characteristics of the lithium secondary battery negative electrode material used. The reason why the average particle size is not less than 0.005 mm is that such a particle size is generally not preferable as a negative electrode material and is inconvenient in handling.

【0013】上記一連の工程によりリチウム二次電池負
極用黒鉛として十分な層間距離と結晶子の大きさを有す
る黒鉛が得られる。特に、本発明によって提供可能な黒
鉛の特性は原料となるキッシュグラファイトの特性を受
けて実質的に層間距離3.36Å以下、結晶子の大きさ
2000Å以上となり、そのため非常に優れた負極特性
を呈することになる。
By the above series of steps, graphite having a sufficient interlayer distance and crystallite size as graphite for a negative electrode of a lithium secondary battery can be obtained. In particular, the characteristics of graphite that can be provided by the present invention are substantially equal to or less than the interlayer distance of 3.36 ° and the size of crystallites are equal to or more than 2000 ° due to the characteristics of the raw material Kish graphite, thereby exhibiting excellent anode characteristics. Will be.

【0014】[0014]

【発明の効果】本発明により、リチウム二次電池負極用
黒鉛の特性が大きく改善され、リチウム二次電池の用途
拡大、軽量化、長寿命化に資するところが大である。ま
た本発明にかかる黒鉛は、天然産ではないので、極めて
安定して供給することができ、リチウム二次電池の安定
製造に寄与するものである。また、従来廃材として処理
されていたキッシュグラファイトの有効活用を図ること
ができる。
According to the present invention, the characteristics of the graphite for a negative electrode of a lithium secondary battery are greatly improved, which greatly contributes to the expansion of the use of the lithium secondary battery, reduction of the weight, and prolongation of the service life. Further, since the graphite according to the present invention is not naturally produced, it can be supplied extremely stably and contributes to the stable production of lithium secondary batteries. Further, it is possible to effectively utilize the quiche graphite which has been conventionally treated as waste material.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 過共晶組成の溶融銑鉄の冷却過程におい
て生ずる鱗状黒鉛を主として含む生成物を処理して得
た、Cを99%以上を含有し、平均粒度が0.005m
m以上であり、かつ層間距離(d)3.37Å以下、結
晶子の大きさ(La)1000Å以上の鱗状黒鉛からな
るリチウム二次電池負極用黒鉛。
1. A method for processing a product mainly containing scale graphite produced in a process of cooling molten iron having a hypereutectic composition, containing 99% or more of C and having an average particle size of 0.005 m
m, the interlayer distance (d) is 3.37 ° or less, and the crystallite size (La) is 1000 ° or more.
【請求項2】 過共晶溶融銑鉄を冷却させて得られる鱗
状黒鉛を主として含有する生成物のうち粒径が0.04
4mm以上のものを回収し、化学処理を行なってCを9
9%以上含有するように精製し、しかる後粉砕と篩い分
けを行なって平均粒度を0.005mm以上に調整し
て、層間距離(d)3.37Å以下、結晶子の大きさ
(La)1000Å以上の鱗状黒鉛からなるリチウム二
次電池負極用黒鉛を製造する方法。
2. A product containing mainly scale-like graphite obtained by cooling hypereutectic molten pig iron and having a particle size of 0.04
4mm or more is collected and subjected to chemical treatment to reduce C to 9
It is refined so as to contain 9% or more, then pulverized and sieved to adjust the average particle size to 0.005 mm or more, the interlayer distance (d) is 3.37 ° or less, and the crystallite size (La) is 1000 °. A method for producing graphite for a negative electrode of a lithium secondary battery comprising the above flake graphite.
【請求項3】 過共晶溶融銑鉄を冷却させて回収される
鱗状黒鉛を主として含有する生成物は、製鉄過程で得ら
れるキッシュグラファイトであることを特徴とする請求
項2記載のリチウム二次電池負極用黒鉛を製造する方
法。
3. The lithium secondary battery according to claim 2, wherein the product mainly containing scale graphite recovered by cooling the hypereutectic molten pig iron is kish graphite obtained in an iron making process. A method for producing graphite for a negative electrode.
JP11635197A 1997-04-18 1997-04-18 Graphite for negative electrode of lithium secondary battery and method for producing the same Expired - Fee Related JP3683379B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11635197A JP3683379B2 (en) 1997-04-18 1997-04-18 Graphite for negative electrode of lithium secondary battery and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11635197A JP3683379B2 (en) 1997-04-18 1997-04-18 Graphite for negative electrode of lithium secondary battery and method for producing the same

Publications (2)

Publication Number Publication Date
JPH10294101A true JPH10294101A (en) 1998-11-04
JP3683379B2 JP3683379B2 (en) 2005-08-17

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Country Link
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* Cited by examiner, † Cited by third party
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US6456484B1 (en) 1999-08-23 2002-09-24 Honda Giken Kogyo Kabushiki Kaisha Electric double layer capacitor
WO2012029505A1 (en) * 2010-08-31 2012-03-08 株式会社Adeka Nonaqueous electrolyte secondary battery
JP2014519684A (en) * 2011-06-03 2014-08-14 カウンスィル オブ サイエンティフィック アンド インダストリアル リサーチ Preparation method of quiche graphite lithium insertion anode material for lithium ion battery
WO2016039268A1 (en) * 2014-09-09 2016-03-17 株式会社東北テクノアーチ Method for producing porous graphite, and porous graphite
CN106450331A (en) * 2016-10-27 2017-02-22 萝北奥星新材料有限公司 Method for preparing graphene conducting agent slurry from graphite tailings

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US6552894B2 (en) 1999-08-23 2003-04-22 Honda Giken Kogyo Kabushiki Kaisha Electric double layer capacitor
US6603653B2 (en) 1999-08-23 2003-08-05 Honda Giken Kogyo Kabushiki Kaisha Electric double layer capacitor
US6456484B1 (en) 1999-08-23 2002-09-24 Honda Giken Kogyo Kabushiki Kaisha Electric double layer capacitor
US9379411B2 (en) 2010-08-31 2016-06-28 Adeka Corporation Non-aqueous electrolyte secondary battery
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JP5881119B2 (en) * 2010-08-31 2016-03-09 株式会社Adeka Non-aqueous electrolyte secondary battery
JP2014519684A (en) * 2011-06-03 2014-08-14 カウンスィル オブ サイエンティフィック アンド インダストリアル リサーチ Preparation method of quiche graphite lithium insertion anode material for lithium ion battery
WO2016039268A1 (en) * 2014-09-09 2016-03-17 株式会社東北テクノアーチ Method for producing porous graphite, and porous graphite
KR20170048254A (en) * 2014-09-09 2017-05-08 가부시키가이샤 토호쿠 테크노 아치 Method for producing porous graphite, and porous graphite
JPWO2016039268A1 (en) * 2014-09-09 2017-06-22 株式会社 東北テクノアーチ Method for producing porous graphite and porous graphite
US10403900B2 (en) 2014-09-09 2019-09-03 Tohoku Techno Arch Co., Ltd. Method for producing porous graphite, and porous graphite
US10763511B2 (en) 2014-09-09 2020-09-01 Tohoku Techno Arch Co., Ltd. Method for producing porous graphite, and porous graphite
CN106450331A (en) * 2016-10-27 2017-02-22 萝北奥星新材料有限公司 Method for preparing graphene conducting agent slurry from graphite tailings

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