JP4488523B2 - 非水電解液二次電池、それに用いる炭素材料および該炭素材料の前駆体 - Google Patents
非水電解液二次電池、それに用いる炭素材料および該炭素材料の前駆体 Download PDFInfo
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
- Secondary Cells (AREA)
Description
本発明者らは、さらに正極にコバルト酸リチウムを用いた2極式コインセルを用いて、45℃におけるサイクル特性を検討した結果、酸化処理がサイクル特性に大きく影響すること、特に酸化性気体を用いた酸化処理品は未処理品に比べてサイクル特性が優れることを見出した。
さらに、本発明は、常圧蒸留残渣油および/または流動接触分解残渣油を主成分として含む原料油を、圧力2.0MPa以下、温度400〜600℃で3時間以上保持して得た、二次電池用に用いる炭素材料の前駆体である。
また、本発明の酸化処理された炭素材料は、高温サイクル特性に優れるリチウム二次電池用負極活物質として最適であり、移動体用または電力貯蔵用のリチウム二次電池の高性能化に寄与する。
以上の比率で混合した原料油の性状としては、芳香族炭化水素成分40〜95wt%、レジン分0.2〜25wt%、残炭0.1〜10wt%であることが望ましい。さらに好ましくは、芳香族炭化水素成分45〜95wt%、レジン分0.5〜20wt%、残炭0.2〜8wt%であることが望ましい。さらにより好ましくは、芳香族炭化水素成分50〜90wt%、レジン分1.0〜15wt%、残炭0.5〜5wt%であることが望ましい。
なお、コーキングプロセスの原料として、減圧残渣油も石油精製の分野で一般的であるが、本発明において、減圧残渣油あるいはその水素化脱硫油では、所望の二次電池用の炭素材料あるいは該炭素材料の前駆体を得ることができない。
チューブボムは、実験室レベルでニードルコークスを製造するために用いられる一般的な装置で、例えばMochida et al.,Chemistry and Physics of Carbon,24,111(1994)に記載されている重質油の熱分解装置であり、重質油から分解ガス、分解油と比較的良質なコークス(ここでいう炭素材料の前駆体)を製造する。鉄製の缶に原料油を充填し、頭頂にガス排出ラインをつなげ、缶を熱したサンドバスに挿入して保持することによりコークスを製造する実験装置である。このチューブボムでは、ガス排出ラインの圧力計と制御弁により反応圧力を任意に設定でき、かつ反応圧力を一定に保つことができる。また、反応温度はサンドバスの設定温度、反応時間はサンドバスに挿入してから引き出すまでの時間であり、両者とも任意に設定できる。
反応時間(保持時間)が異なると、得られたコークスの特性も微妙に異なる。そこで本発明における炭素材料前駆体は3時間以上の熱履歴を受けたものを炭素材料前駆体として用いる。
このようにチューブボム、あるいはディレードコーカーなどを用いて得られたコークス(炭素材料前駆体)の性状としては、揮発分2〜20wt%、乾燥ベースでの水素含有率1〜6wt%であることが望ましい。
酸化性気体雰囲気は、窒素、アルゴンなどの不活性ガスに、酸素、オゾン、二酸化炭素などの酸化性気体を所望の酸化性気体濃度になるように加えてつくることができる。コストや環境面での配慮から、大気(空気)を窒素ガスなどの不活性ガスまたは酸素ガスなどの酸化性気体の代わりに、あるいは、酸化性気体雰囲気そのものとして用いることも可能である。
酸化処理における温度条件は、200〜1000℃であることが好ましい。処理温度が200℃未満であると、炭素材料粉末表面の酸化反応が十分進行せず、一方、1000℃を超えると炭素材料粉末の比表面積が過大となり、電池特性に悪影響を与えるので好ましくない。
また、負極は、公知の方法によって作製すればよい。例えば、上記炭素材料を粉砕して得られる粉体を結着剤と混合し、溶剤を加えてスラリー状ないしペースト状にしたものを、銅箔等の集電体の表面に塗布乾燥し、必要に応じて電極密度を高めるべく圧縮形成して負極を作製することができる。
比較例2
比較例3
比較例4
該前駆体の粉末をシャトル炉にて毎分0.6℃の昇温速度で16時間昇温し、さらに毎分1.0℃の昇温速度で昇温して炉内温度を1100℃とし、1時間保持して熱処理したのち、自然放冷で室温まで冷却することにより炭素材料粉末を作製した。
得られた炭素材料粉末を酸素と窒素の混合気体の気流下(酸素20容量%、流量3L/min)、昇温速度200℃/hrで800℃に昇温し、800℃で1時間酸化処理した。酸化処理後の収率は約90%であった。
コインセルを25℃で、充電:約0.3mA 4.2V 10時間、放電:約0.3mA 2.5Vの条件で1サイクルさせた。その後、45℃で、充電:約2mA 4.2V 2時間、放電:約2mA 2.5Vの条件で50サイクルさせた。45℃での1サイクル目の放電容量と50サイクル目の放電容量との比(45℃サイクル特性)を求めた。その結果を表2に示す。
酸化処理品を実施例6と同様に45℃サイクル特性を評価した。結果を表2に示す。
比較例5
Claims (5)
- 常圧蒸留残渣油および/または流動接触分解残渣油を主成分として含む原料油を、圧力2.0MPa以下、温度400〜600℃で3時間以上保持して炭素材料の前駆体を得、該前駆体を800〜1500℃で熱処理して得られた非水電解液二次電池の負極活物質用炭素材料。
- 炭素材料をさらに酸化処理することを特徴とする、請求項1に記載の非水電解液二次電池の負極活物質用炭素材料。
- 酸化処理が、酸化性気体を含む窒素、アルゴンまたはこれらの混合気体中で或いは大気中で、200〜1000℃で熱処理するものである請求項2に記載の非水電解液二次電池の負極活物質用炭素材料。
- 請求項1〜3のいずれか1項に記載の炭素材料を負極活物質として用いた非水電解液二次電池。
- 常圧蒸留残渣油および/または流動接触分解残渣油を主成分として含む原料油を、圧力2.0MPa以下、温度400〜600℃で3時間以上保持して得た、非水電解液二次電池の負極活物質に用いる炭素材料の前駆体。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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JP2003316751 | 2003-09-09 | ||
JP2003316751 | 2003-09-09 | ||
JP2004065411 | 2004-03-09 | ||
JP2004065411 | 2004-03-09 | ||
PCT/JP2004/011251 WO2005027242A1 (ja) | 2003-09-09 | 2004-08-05 | 非水電解液二次電池、それに用いる炭素材料および該炭素材料の前駆体 |
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JPWO2005027242A1 JPWO2005027242A1 (ja) | 2007-10-04 |
JP4488523B2 true JP4488523B2 (ja) | 2010-06-23 |
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JP2005513822A Expired - Fee Related JP4488523B2 (ja) | 2003-09-09 | 2004-08-05 | 非水電解液二次電池、それに用いる炭素材料および該炭素材料の前駆体 |
Country Status (6)
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US (1) | US20070009418A1 (ja) |
EP (1) | EP1667259A4 (ja) |
JP (1) | JP4488523B2 (ja) |
KR (1) | KR20060041315A (ja) |
CA (1) | CA2535853A1 (ja) |
WO (1) | WO2005027242A1 (ja) |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
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JP4694288B2 (ja) * | 2005-07-07 | 2011-06-08 | Jx日鉱日石エネルギー株式会社 | 電極材料用低温焼成炭素 |
KR100836524B1 (ko) | 2006-02-23 | 2008-06-12 | 한국전기연구원 | 고용량 전극 활물질, 그 제조방법, 이를 구비한 전극 및에너지 저장 장치 |
JP5270906B2 (ja) | 2007-11-08 | 2013-08-21 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極材料用原料炭組成物及びその製造方法 |
KR101117624B1 (ko) | 2010-05-07 | 2012-02-29 | 삼성에스디아이 주식회사 | 리튬 이차 전지용 음극 활물질, 이의 제조 방법 및 이를 포함하는 리튬 이차 전지 |
JP5490636B2 (ja) * | 2010-06-30 | 2014-05-14 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極炭素材料用の原料油組成物 |
JP5498279B2 (ja) * | 2010-06-30 | 2014-05-21 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極炭素材料用の原料油組成物 |
CN105366666A (zh) * | 2011-06-24 | 2016-03-02 | 株式会社半导体能源研究所 | 多层石墨烯及蓄电装置 |
EP2892096B1 (en) | 2012-08-30 | 2019-03-27 | Kuraray Co., Ltd. | Method for manufacturing a carbon material for nonaqueous electrolyte secondary battery |
JP6102231B2 (ja) * | 2012-12-07 | 2017-03-29 | 日立化成株式会社 | リチウムイオン二次電池用負極材、リチウムイオン二次電池用負極、及びリチウムイオン二次電池、並びにリチウムイオン二次電池用負極材の製造方法 |
KR101725213B1 (ko) * | 2013-02-19 | 2017-04-12 | 주식회사 쿠라레 | 비수전해질 이차전지 음극용 탄소질 재료 |
JP6444106B2 (ja) * | 2014-09-19 | 2018-12-26 | コスモ石油株式会社 | 顔料、顔料を含む組成物及び顔料の製造方法 |
JP6566113B2 (ja) * | 2015-03-27 | 2019-08-28 | 日本電気株式会社 | ボロンドープ活性化炭素材料 |
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JPH05307956A (ja) * | 1992-04-28 | 1993-11-19 | Sanyo Electric Co Ltd | 非水系二次電池 |
JPH08102324A (ja) * | 1994-09-30 | 1996-04-16 | Mitsubishi Chem Corp | 非水系二次電池 |
JPH08287911A (ja) * | 1995-04-18 | 1996-11-01 | Mitsubishi Chem Corp | 非水系二次電池 |
JP2000233123A (ja) * | 1999-02-10 | 2000-08-29 | Japan Yunikkusu:Kk | ミキサー |
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EP0627777B1 (en) * | 1993-06-03 | 2000-02-02 | Sony Corporation | Non-aqueous liquid electrolyte secondary battery |
US6150055A (en) * | 1997-08-05 | 2000-11-21 | Mitsubishi Chemical Corporation | Carbonaceous negative electrode material for nonaqueous secondary battery, process for producing the same, and nonaqueous secondary battery |
JP2000223123A (ja) * | 1999-02-03 | 2000-08-11 | Mitsubishi Chemicals Corp | 非水系二次電池用炭素質負極材料、その製造方法並びに非水系二次電池 |
-
2004
- 2004-08-05 JP JP2005513822A patent/JP4488523B2/ja not_active Expired - Fee Related
- 2004-08-05 US US10/569,503 patent/US20070009418A1/en not_active Abandoned
- 2004-08-05 CA CA002535853A patent/CA2535853A1/en not_active Abandoned
- 2004-08-05 EP EP04771278A patent/EP1667259A4/en not_active Withdrawn
- 2004-08-05 KR KR1020067004703A patent/KR20060041315A/ko not_active Application Discontinuation
- 2004-08-05 WO PCT/JP2004/011251 patent/WO2005027242A1/ja active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH05307956A (ja) * | 1992-04-28 | 1993-11-19 | Sanyo Electric Co Ltd | 非水系二次電池 |
JPH08102324A (ja) * | 1994-09-30 | 1996-04-16 | Mitsubishi Chem Corp | 非水系二次電池 |
JPH08287911A (ja) * | 1995-04-18 | 1996-11-01 | Mitsubishi Chem Corp | 非水系二次電池 |
JP2000233123A (ja) * | 1999-02-10 | 2000-08-29 | Japan Yunikkusu:Kk | ミキサー |
Also Published As
Publication number | Publication date |
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US20070009418A1 (en) | 2007-01-11 |
EP1667259A4 (en) | 2009-07-22 |
EP1667259A1 (en) | 2006-06-07 |
JPWO2005027242A1 (ja) | 2007-10-04 |
CA2535853A1 (en) | 2005-03-24 |
KR20060041315A (ko) | 2006-05-11 |
WO2005027242A1 (ja) | 2005-03-24 |
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