JP2013232403A - 蓄電装置用負極、その製造方法及び蓄電装置 - Google Patents
蓄電装置用負極、その製造方法及び蓄電装置 Download PDFInfo
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- JP2013232403A JP2013232403A JP2013048578A JP2013048578A JP2013232403A JP 2013232403 A JP2013232403 A JP 2013232403A JP 2013048578 A JP2013048578 A JP 2013048578A JP 2013048578 A JP2013048578 A JP 2013048578A JP 2013232403 A JP2013232403 A JP 2013232403A
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- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical group O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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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
- 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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- 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
- H01M4/13—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
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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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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Abstract
【解決手段】負極集電体と、負極集電体上の、複数の粒状の負極活物質を有する負極活物質層と、該粒状の負極活物質の一部を被覆する被膜と、を有し、該被膜は、絶縁性とリチウムイオン伝導性とを有する膜である蓄電装置用負極である。
【選択図】図1
Description
本実施の形態では、電解液の分解反応を抑制することができる被膜を有する負極活物質の構造について、図1を用いて説明する。
本実施の形態では、本発明に係る粒状の負極活物質への被膜の作製方法について、図2を用いて説明する。
本実施の形態では、被膜を有する粒状の負極活物質を用いた蓄電装置用負極及びその製造方法について、図3を用いて説明する。
本実施の形態では、蓄電装置としてリチウムイオン電池の構造及び製造方法について説明する。
はじめに、正極及びその製造方法について説明する。
図5(A)は、コイン型(単層偏平型)のリチウムイオン電池の外観図であり、図5(B)は、その断面図である。
次に、ラミネート型のリチウムイオン電池の一例について、図6を参照して説明する。
次に、円筒型のリチウムイオン電池の一例について、図7を参照して説明する。円筒型のリチウムイオン電池500は図7(A)に示すように、上面に正極キャップ(電池蓋)501を有し、側面及び底面に電池缶(外装缶)502を有している。これら正極キャップと電池缶(外装缶)502とは、ガスケット(絶縁パッキン)510によって絶縁されている。
本実施の形態では、蓄電装置としてリチウムイオンキャパシタについて説明する。
本発明の一態様に係る蓄電装置は、電力により駆動する様々な電気機器の電源として用いることができる。
次に、電気機器の一例である携帯情報端末について、図9を用いて説明する。
さらに、電気機器の一例である移動体の例について、図10を用いて説明する。
酸化ニオブについて、X線回折法(XRD:X−Ray Diffraction)により構造評価を行った。ここでは、黒鉛は用いず、ゾル−ゲル法によりゲル状のニオブを形成し、坩堝に入れて、600℃で3時間焼成することで作製した酸化ニオブを測定した。X線回折法による測定結果を図11に示す。
次に、被膜として酸化ニオブ膜を有する負極活物質を作製した。負極活物質には、JFEケミカル株式会社製の黒鉛を用いた。まず、実施の形態2で示したように、Nb(OEt)5と安定化剤として機能するアセト酢酸エチルにトルエンを加え、撹拌してNb(OEt)5トルエン溶液を作製した。この溶液の配合比は、Nb(OEt)5を3.14×10―4mol、アセト酢酸エチルを6.28×10―4mol、トルエンを2mlとした。次に、ドライルーム環境において、Nb(OEt)5トルエン溶液に負極活物質である粒状の黒鉛を添加して撹拌した。この後、湿気環境において、50℃で3時間溶液を保持することで、黒鉛を加えたNb(OEt)5トルエン溶液中のNb(OEt)5を加水分解反応及び縮合反応させた。すなわち、該溶液中のNb(OEt)5を大気中の水分と徐々に加水分解反応させ、引き続いて起こる脱水反応により縮合させた。このようにして、粒状の黒鉛の表面にゲル状のニオブを付着させた。その後、大気下において500℃、3時間の焼成を行い、酸化ニオブからなる被膜に覆われた粒状の黒鉛を作製した。
図12及び13に粒状の黒鉛についてのSEM(Scanning Electron Microscope)観察像を示す。図12(A)、図12(B)は、酸化ニオブ膜を形成していない粒状の黒鉛700を観察したSEM像である。図12(A)は3000倍のSEM像、図12(B)はその一部を拡大した、5000倍のSEM像である。粒径が概略20μmの粒状の黒鉛700が観察されるが、その表面は粗く、さらに小さい粒子が凝集している様子が確認される。
次に、本発明に係る被膜が、リチウムイオンの挿入脱離反応を示すものであるか否かを、サイクリックボルタンメトリ(Cyclic Voltammetry。CV)により確認した。
次に、酸化ニオブ膜の被覆による黒鉛と電解液との反応の抑制を直接確認するため、負極活物質としてHOPG膜を用いてCV測定を行った。
次に、上記のようにゾル−ゲル法を用いて形成した酸化ニオブ膜を被膜として有する粒状の黒鉛を負極活物質とした負極を作製し、フルセルとしてセル組みして二次電池のサイクル特性を測定した。
以上のことから、リチウムイオン電池の初期容量の低下を引き起こす不可逆容量の発生を低減し、負極における電解液などの電気化学的な分解を抑制することができた。また、リチウムイオン電池の充放電の繰り返しにおいて、充放電の副反応として生じる電解液等の分解反応を抑制することで、リチウムイオン電池のサイクル特性を向上させることができた。また、高温下において早まる電解液の分解反応を抑制し、高温充放電における容量の減少を防止することで、リチウムイオン電池の使用温度範囲を拡大することができる。
実施例として、実際に作製した蓄電装置用負極及び該負極を用いた蓄電装置について説明する。
上記ゾル−ゲル法を用いて酸化シリコンを形成した黒鉛粒子を負極活物質とした負極と、LiPO4を用いた正極と、を用いて電池を作製し、サイクル特性を比較した。
また、図28に、電極E4及び電極F4についてのSEM観察像を示す。図28(A)に、電極E4のSEM観察像を示し、図28(B)に、電極F4についてのSEM観察像を示す。なお、図28(A)に示すSEM観察像と、図28(B)に示すSEM観察像は、同じ倍率で観察したものである。
正極活物質として炭素層を表面に設けたリン酸鉄リチウム(LiFePO4)を用いた。まずリン酸鉄リチウムとグルコースとをアセトン中で混練し、この混合物を乾燥させた後に600℃で焼成することにより、正極活物質を得た。
負極活物質として、酸化シリコンからなる被膜に覆われた黒鉛を用いた。まず、黒鉛としては、JFEケミカル株式会社製の平均粒径の9μm黒鉛(MCMB:メソカーボンマイクロビーズ)を用いた。まず、Si(OEt)4と触媒として機能する塩酸に、水とエタノールを加え、撹拌してSi(OEt)4溶液を作製した。この溶液の配合比は、Si(OEt)4を1.8×10−2mol、塩酸を4.44×10−4mol、水1.9ml、エタノール6.3mlとした。次に、ドライルーム環境において、Si(OEt)4溶液に負極活物質である粒状の黒鉛を添加して撹拌した。この後、湿気環境において、70℃で20時間溶液を保持することで、黒鉛を加えたSi(OEt)4水とエタノールとの混合溶液中のSi(OEt)4を加水分解反応及び縮合反応させた。すなわち、該溶液中のSi(OEt)4を大気中の水分と徐々に加水分解反応させ、引き続いて起こる脱水反応により縮合させた。このようにして、粒状の黒鉛の表面にゲル状の酸化シリコンを付着させた。その後、大気下において500℃、3時間の乾燥を行い、酸化シリコンからなる被膜に覆われた粒状の黒鉛を作製した。
まず、上述した正極を50mm×41mmに、負極を53mm×45mmの矩形状にそれぞれ成形した。なお、成形した正極及び負極は、端子部として機能する突出部が形成されるように設け、当該突出部上における活物質層を除去して集電体を露出させた。
まず、上述した負極を減圧雰囲気下で170℃の温度で10時間加熱して、電極を乾燥させた。続いて、上述した正極、負極及びセパレータを、円形にカットした。セルの形状はCR2032タイプ(直径20mm、高さ3.2mm)を用いた。上述した正極、電解液に含浸させたセパレータ、及び負極を積層したものをステンレス(SUS)製の正極缶及び負極缶の間に設け、これらをかしめることによりコイン型リチウムイオン電池を作製した。
まず、ラミネート型のサンプル1とコイン型のサンプル2について放電特性を評価した。充電は0.2CのレートでCCCV充電し、上限電圧を4.0Vとした。放電は、0.2C、1C、2C、5CのレートのそれぞれについてCC放電により行い、下限電圧は2Vとした。また、測定温度は25℃で行った。それぞれのサンプルの正極の担持量、負極の担持量、及び容量比を表1に示す。
続いて、放電時の温度を−25℃、0℃、25℃の3条件として放電特性を評価した結果を示す。充電は上記と同様に行い、放電は0.2Cのレートで行った。評価はラミネート型のサンプル3並びにコイン型のサンプル4及びサンプル5を用いて行った。なお、コイン型のサンプルにおいて、25℃及び0℃の評価はサンプル4を用いて行い、−25℃の評価はサンプル5を用いて行った。それぞれのサンプルの正極の担持量、負極の担持量、及び容量比を表2に示す。
続いて、ラミネート型のサンプルとコイン型のサンプルとで、それぞれ放電容量のサイクル特性を評価した。充放電は1Cのレートで行い、電圧範囲は2V〜4Vとした、環境温度は60℃に設定して測定を行った。評価はラミネート型のサンプル6、サンプル7、コイン型のサンプル8、サンプル9、及びサンプル10を用いた。それぞれのサンプルの正極の担持量、負極の担持量、及び容量比を表3に示す。
102 被膜
200 負極
201 負極集電体
202 負極活物質層
203 負極活物質
204 導電助剤
205 グラフェン
250 正極
251 正極集電体
252 正極活物質層
253 正極活物質
254 グラフェン
300 リチウムイオン電池
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
400 リチウムイオン電池
401 正極集電体
402 正極活物質層
403 正極
404 負極集電体
405 負極活物質層
406 負極
407 セパレータ
408 電解液
409 外装体
500 リチウムイオン電池
501 正極キャップ
502 電池缶
503 正極端子
504 正極
505 セパレータ
506 負極
507 負極端子
508 絶縁板
509 絶縁板
510 ガスケット(絶縁パッキン)
511 PTC素子
512 安全弁機構
600 表示装置
601 筐体
602 表示部
603 スピーカ部
604 蓄電装置
610 照明装置
611 筐体
612 光源
613 蓄電装置
614 天井
615 側壁
616 床
617 窓
620 室内機
621 筐体
622 送風口
623 蓄電装置
624 室外機
630 電気冷凍冷蔵庫
631 筐体
632 冷蔵室用扉
633 冷凍室用扉
634 蓄電装置
650 タブレット型端末
651 筐体
652 表示部
652a 表示部
652b 表示部
653 表示モード切り替えスイッチ
654 電源スイッチ
655 省電力モード切り替えスイッチ
656 操作スイッチ
657a 領域
657b 領域
658 操作キー
659 キーボード表示切り替えボタン
660 太陽電池
670 充放電制御回路
671 バッテリー
672 DCDCコンバータ
673 コンバータ
680 電気自動車
681 バッテリー
682 制御回路
683 駆動装置
684 処理装置
700 粒状の黒鉛
701 粒状の黒鉛
702 酸化ニオブ膜
703 粒状の黒鉛
704 炭素膜
705 酸化ニオブ膜
706 タングステン膜
780 ガラス基板
781 酸化ニオブ膜
782 炭素膜
783 白金膜
Claims (8)
- 負極集電体と、
前記負極集電体上の、複数の粒状の負極活物質を有する負極活物質層と、
前記粒状の負極活物質の一部を被覆する被膜と、を有し、
前記被膜は、絶縁性とリチウムイオン伝導性とを有する膜であることを特徴とする蓄電装置用負極。 - 負極集電体と、
前記負極集電体上の、負極活物質として複数の粒状の黒鉛を有する負極活物質層と、
前記粒状の黒鉛の一部を被覆する被膜と、を有し、
前記被膜は、絶縁性とリチウムイオン伝導性とを有する膜であることを特徴とする蓄電装置用負極。 - 請求項1又は2において、
前記被膜は、ニオブ、チタン、バナジウム、タンタル、タングステン、ジルコニウム、モリブデン、ハフニウム、クロム、アルミニウム若しくはシリコンのいずれか一の酸化膜、又はこれら元素のいずれか一とリチウムとを含む酸化膜であることを特徴とする蓄電装置用負極。 - 請求項1又は2において、
前記被膜は、六方晶系の結晶構造を有するNb2O5であることを特徴とする蓄電装置用負極。 - 請求項1乃至4のいずれか一項において、
前記被膜の膜厚は、5nm以上50nm以下であることを特徴とする蓄電装置用負極。 - 請求項1乃至5のいずれか一項に記載の蓄電装置用負極を用いた蓄電装置。
- 金属アルコキシドと安定化剤と溶媒とを含む溶液に、粒状の黒鉛を分散して分散溶液を作製し、
前記金属アルコキシドを加水分解反応及び縮合反応させてゲル化することで、前記粒状の黒鉛の表面に前記金属アルコキシドの金属を含むゲルを付着させ、
加熱処理により前記ゲルを焼成することで、前記粒状の黒鉛の表面に金属酸化膜を形成し、
前記金属酸化膜が形成された前記粒状の黒鉛と結着剤とを有するスラリーを、負極集電体上に塗布した後に、焼成することを特徴とする蓄電装置用負極の製造方法。 - 請求項7の方法により製造した蓄電装置用負極を用いた蓄電装置。
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TWI575804B (zh) | 2017-03-21 |
JP2021073656A (ja) | 2021-05-13 |
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US20230216019A1 (en) | 2023-07-06 |
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KR102101352B1 (ko) | 2020-04-17 |
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US10263243B2 (en) | 2019-04-16 |
US9899660B2 (en) | 2018-02-20 |
KR102306497B1 (ko) | 2021-09-28 |
KR20200040911A (ko) | 2020-04-20 |
JP2023162271A (ja) | 2023-11-08 |
US20210408516A1 (en) | 2021-12-30 |
US11605804B2 (en) | 2023-03-14 |
TW201407868A (zh) | 2014-02-16 |
WO2013151110A1 (en) | 2013-10-10 |
KR20150007283A (ko) | 2015-01-20 |
US20160315309A1 (en) | 2016-10-27 |
KR20190092613A (ko) | 2019-08-07 |
JP6552543B2 (ja) | 2019-07-31 |
US20190245195A1 (en) | 2019-08-08 |
JP2017157566A (ja) | 2017-09-07 |
JP6137884B2 (ja) | 2017-05-31 |
JP2019175864A (ja) | 2019-10-10 |
US20130266858A1 (en) | 2013-10-10 |
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