JP2016048684A - 蓄電池用電極、及びその製造方法、蓄電池、電子機器、並びにグラフェン - Google Patents
蓄電池用電極、及びその製造方法、蓄電池、電子機器、並びにグラフェン Download PDFInfo
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- JP2016048684A JP2016048684A JP2015167051A JP2015167051A JP2016048684A JP 2016048684 A JP2016048684 A JP 2016048684A JP 2015167051 A JP2015167051 A JP 2015167051A JP 2015167051 A JP2015167051 A JP 2015167051A JP 2016048684 A JP2016048684 A JP 2016048684A
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Classifications
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- 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
- H01M4/139—Processes of manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- H—ELECTRICITY
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/04—Processes of manufacture in general
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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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
【解決手段】酸化グラフェンをアルコール又は酸を含む溶液に分散する工程と、溶液に分散させた酸化グラフェンを加熱する工程と、酸化グラフェンを還元する工程と、を有する蓄電池用電極の製造方法を提供する。
【選択図】図1
Description
本実施の形態では、本発明の一態様に係る蓄電池用電極について、図1、図2及び図3を参照して説明する。図1に電極の作製に用いる酸化グラフェンの調製方法を説明するフローチャートを、図2に電極の構成を説明する図を、図3に酸化グラフェンの反応および構造を表す図を示す。
本実施の形態では、本発明の一態様の蓄電池用電極の作製方法について、図4を参照して説明する。具体的には、活物質、酸化グラフェン、結着剤、及び溶媒を用いて、混合物を作製し、該混合物を集電体101上に塗布した後、酸化グラフェンを還元させることで、図2に示した活物質層102を含む蓄電池用電極100を製造する方法について、説明する。
本実施の形態では、本発明の一態様の蓄電池用電極の作製方法について、図5を参照して説明する。具体的には、活物質の表面に酸化グラフェンを被覆し、還元したのちに、グラフェンを有する活物質と、導電助剤、結着剤、及び溶媒を用いて、活物質層102の形成に使用する溶剤を含む組成物(電極合剤組成物ともいう。)を作製する。次に、該電極合剤組成物を集電体101上に塗布することで、図2に示した活物質層102を含む蓄電池用電極100を製造する方法について、説明する。
本実施の形態では、実施の形態1で示した製造方法により製造した蓄電池用電極を用いた蓄電池の構造について、図11乃至図13を参照して説明する。
図11(A)は、コイン型(単層偏平型)の蓄電池の外観図であり、図11(B)は、その断面図である。
図12はラミネート型の蓄電池500の外観図を示す。また、図13(A)および図13(B)は、図12に一点鎖線で示すA1−A2断面およびB1−B2断面を示す。ラミネート型の蓄電池500は、正極集電体501および正極活物質層502を有する正極503と、負極集電体504および負極活物質層505を有する負極506と、セパレータ507と、電解液508と、外装体509と、を有する。正極503と負極506との間にセパレータ507が設置されている。また、外装体509で囲まれた領域内には電解液508が注入されている。
次に、円筒型の蓄電池の一例について、図14を参照して説明する。円筒型の蓄電池600は図14(A)に示すように、上面に正極キャップ(電池蓋)601を有し、側面及び底面に電池缶(外装缶)602を有している。これら正極キャップ601と電池缶(外装缶)602とは、ガスケット(絶縁パッキン)610によって絶縁されている。
本発明の一態様に係る蓄電池用電極を用いた蓄電池は、電力により駆動する様々な電子機器の電源として用いることができる。
次に、電子機器の一例である携帯情報端末について、図16を用いて説明する。
さらに、電子機器の一例である移動体の例について、図17を用いて説明する。
異なる工程により3種類の酸化グラフェンを作製し、それぞれ酸化グラフェンA〜Cとして、電極の作製に用いることとした。また、ステップS12の工程を行わないで作製した酸化グラフェンを比較例1として、同様に電極の作製に用いることとした。
酸化グラフェンA〜C、及び比較例1を用いて正極を作製した。まず、正極活物質(LiFePO4)粒子、結着剤(PVdF、呉羽化学社製)、及び導電助剤の原料として酸化グラフェンA〜C及び比較例1のいずれか1つを混合して、混合物(正極ペーストともいう。)を作製した。正極ペーストの配合比(LiFePO4:酸化グラフェン:PVdF)は、93:2:5(単位wt%)とした。該正極ペーストを集電体(アルミニウム)に塗布し、減圧下、加熱及び還元することで正極を作製した。集電体に対する正極ペーストの担持量は、6mg/cm2とした。酸化グラフェンの還元方法には、熱還元又は化学還元を用いた。
作製した正極をハーフセルに組み込み、それぞれのセルの充放電特性をそれぞれ測定した。負極にはリチウム金属を用い、電解液はエチレンカーボネート(EC)とジエチルカーボネート(DEC)とを体積比で1:1の割合で混合した混合溶液中へ六フッ化リン酸リチウム(LiPF6)を1モル/リットルの濃度で溶解したものを用いた。
CC充電について説明する。CC充電は、充電期間のすべてで一定の電流を二次電池に流し、所定の電圧になったときに充電を停止する充電方法である。二次電池を、図7(A)に示すように内部抵抗Rと二次電池容量Cの等価回路と仮定する。この場合、二次電池電圧VBは、内部抵抗Rにかかる電圧VRと二次電池容量Cにかかる電圧VCの和である。
次に、CCCV充電について説明する。CCCV充電は、まずCC充電にて所定の電圧まで充電を行い、その後CV(定電圧)充電にて流れる電流が少なくなるまで、具体的には終止電流値になるまで充電を行う充電方法である。
次に、CC放電について説明する。CC放電は、放電期間のすべてで一定の電流を二次電池から流し、二次電池電圧VBが所定の電圧、例えば2.5Vになったときに放電を停止する放電方法である。
酸化グラフェンA〜Cを、減圧下で1時間保持した後に170℃まで昇温し、10時間保持する加熱処理により還元した。得られたRGOを5mm径のペレットダイスに詰め、油圧式ポンプで10分加圧を行い、解放後、再度10分加圧を行うことでペレットを作製した。この時、粉体に加わる単位面積当たりの圧力は約7.5Mgf/cm2である。得られたペレットを試料A〜Cとした。試料A、B、Cはそれぞれ、酸化グラフェンA、B、Cを用いて作製したRGOである。また、比較例1に対して同様に還元を行い、ペレット化することにより比較例4を作製した。
次に、温和な条件における酸化グラフェンの還元速度を比較するために、酸化グラフェンA、酸化グラフェンC及び比較例1を、およそ1年と6か月保管した。試料の保管は、ドライルームにて、25℃の条件で行った。
101 集電体
102 活物質層
103 活物質
104 グラフェン
106 酸化グラフェン
107 酸化グラフェン
108 酸化グラフェン
300 コイン型の蓄電池
301 正極缶
302 負極缶
303 ガスケット
304 正極
305 正極集電体
306 正極活物質層
307 負極
308 負極集電体
309 負極活物質層
310 セパレータ
500 蓄電池
501 正極集電体
502 正極活物質層
503 正極
504 負極集電体
505 負極活物質層
506 負極
507 セパレータ
508 電解液
509 外装体
600 蓄電池
601 正極キャップ
602 電池缶
603 正極端子
604 正極
605 セパレータ
606 負極
607 負極端子
608 絶縁板
609 絶縁板
610 ガスケット(絶縁パッキン)
611 PTC素子
612 安全弁機構
700 表示装置
701 筐体
702 表示部
703 スピーカ部
704 蓄電池
710 照明装置
711 筐体
712 光源
713 蓄電池
714 天井
715 側壁
716 床
717 窓
720 室内機
721 筐体
722 送風口
723 蓄電池
724 室外機
730 電気冷凍冷蔵庫
731 筐体
732 冷蔵室用扉
733 冷凍室用扉
734 蓄電池
800 タブレット型端末
801 筐体
802 表示部
802a 表示部
802b 表示部
803 表示モード切り替えスイッチ
804 電源スイッチ
805 省電力モード切り替えスイッチ
807 操作スイッチ
808a タッチパネルの領域
808b タッチパネルの領域
809 操作キー
810 キーボード表示切り替えボタン
811 太陽電池
850 充放電制御回路
851 バッテリー
852 DCDCコンバータ
853 コンバータ
860 電気自動車
861 バッテリー
862 制御回路
863 駆動装置
864 処理装置
Claims (12)
- グラフェンを含む活物質層を集電体上に形成する蓄電池用電極の製造方法であって、
酸化グラフェンをアルコール又は酸を含む溶液に分散する工程と、
前記溶液に分散させた酸化グラフェンを加熱する工程と、
前記酸化グラフェンを還元する工程と、を有することを特徴とする蓄電池用電極の製造方法。 - 酸化グラフェンをアルコール又は酸を含む溶液に分散させ、
前記溶液に分散させた酸化グラフェンを加熱し、
前記酸化グラフェンと、活物質と、結着剤と、溶媒と、を有する混合物を形成し、
前記混合物を集電体上に塗布し、
前記塗布した混合物に含まれる前記溶媒を除去し、
前記塗布した混合物に含まれる前記酸化グラフェンを還元して、グラフェンを含む活物質層を前記集電体上に形成することを特徴とする蓄電池用電極の製造方法。 - 酸化グラフェンをアルコール又は酸を含む溶液に分散させ、
前記溶液に分散させた酸化グラフェンを加熱し、
前記酸化グラフェンと活物質を混合することで、第1の混合物を形成し、
前記第1の混合物に含まれる前記酸化グラフェンを還元することで、第2の混合物を形成し、
前記第2の混合物と、結着剤と、導電助剤と、溶媒と、を含む第3の混合物を集電体上に塗布し、
前記第3の混合物に含まれる前記溶媒を除去することで、グラフェンを含む活物質層を前記集電体上に形成することを特徴とする蓄電池用電極の製造方法。 - 請求項1乃至3のいずれか一項において、
前記酸化グラフェンを、加熱により還元することを特徴とする蓄電池用電極の製造方法。 - 請求項4において、
前記酸化グラフェンを、60℃以上150℃以下に加熱して還元することを特徴とする蓄電池用電極の製造方法。 - 請求項1乃至3のいずれか一項において、
前記酸化グラフェンを、還元剤を含む極性溶媒に浸して還元することを特徴とする蓄電池用電極の製造方法。 - 請求項1乃至6のいずれか一項に記載の蓄電池用電極の製造方法で作製された蓄電池用電極。
- 活物質層と集電体を有し、
前記活物質層は、活物質と、グラフェンと、結着剤とを有し、
前記グラフェンは、エーテル結合もしくはエステル結合で連結されたアルキル基を有し、
前記活物質層は、前記集電体上に位置することを特徴とする蓄電池用電極。 - 第1の電極と、第2の電極と、を有し、
前記第1の電極は、請求項7又は8に記載の蓄電池用電極であり、
前記第1の電極は、正極又は負極の一方として動作させることができる機能を有し、
前記第2の電極は、正極又は負極の他方として動作させることができる機能を有する蓄電池。 - 請求項9に記載の蓄電池と、表示パネル、操作キー、スピーカ、またはマイクと、を搭載することを特徴とする電子機器。
- エーテル結合もしくはエステル結合で連結されたアルキル基を有することを特徴とするグラフェン。
- 請求項11において、
前記アルキル基は炭素数1以上4以下であることを特徴とするグラフェン。
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WO2017209039A1 (ja) * | 2016-05-31 | 2017-12-07 | 地方独立行政法人東京都立産業技術研究センター | 多層グラフェン分散液、熱物性測定用黒化剤および粉末焼結用離型剤・潤滑剤 |
JP2018092934A (ja) * | 2016-12-02 | 2018-06-14 | 株式会社半導体エネルギー研究所 | 電極、電極の製造方法および蓄電装置 |
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US10529977B2 (en) | 2020-01-07 |
US20200144598A1 (en) | 2020-05-07 |
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JP6978484B2 (ja) | 2021-12-08 |
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US11961994B2 (en) | 2024-04-16 |
KR102573541B1 (ko) | 2023-09-01 |
US20160064726A1 (en) | 2016-03-03 |
KR20170044662A (ko) | 2017-04-25 |
US11251415B2 (en) | 2022-02-15 |
JP2020061373A (ja) | 2020-04-16 |
JP7292356B2 (ja) | 2023-06-16 |
JP6634242B2 (ja) | 2020-01-22 |
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