JP5017493B2 - 非水電解質電池用活物質、非水電解質電池および電池パック - Google Patents
非水電解質電池用活物質、非水電解質電池および電池パック Download PDFInfo
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- JP5017493B2 JP5017493B2 JP2011523510A JP2011523510A JP5017493B2 JP 5017493 B2 JP5017493 B2 JP 5017493B2 JP 2011523510 A JP2011523510 A JP 2011523510A JP 2011523510 A JP2011523510 A JP 2011523510A JP 5017493 B2 JP5017493 B2 JP 5017493B2
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Images
Classifications
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Description
試料を直径25mmの標準ガラスホルダに詰め、広角X線回折法で測定を行った。以下に測定装置および条件を示す。測定環境は室温大気中(18〜25℃)で行なう。
X線源:CuKα線(Niフィルター使用)
出力 :40kV,40mA
スリット系:Div. Slit;0.3°
検出器:LynxEye(高速検出器)
(2)スキャン方式:2θ/θ連続スキャン
(3)測定範囲(2θ):5〜100°
(4)ステップ幅(2θ):0.01712°
(5)計数時間:1秒間/ステップ。
このような単斜晶系β型チタン複合酸化物の広角X線回折法で得られるX線回折パターンから2θが48〜49°に存在するピークおよび2θが24〜26°に存在するピークの半値幅に以下に示すシェラーの式を用いて結晶子径(結晶子サイズ)を算出することができる。
結晶子径X,Yの関係が式(1)を満たすTiO2(B)を活物質として含む非水電解質電池は、大電流特性をさらに向上できる。さらに好ましい結晶子径X,Yの関係は次式(2)を満たす。
X/Yが50を超えると、TiO2(B)粉末の粒径が大きくなって粉末の比表面積が低下し、活物質と電解液との接触面積、即ちリチウムイオンを吸蔵できる面積が減少する虞がある。
以下、非水電解質電池の構成部材である外装材、負極、正極、セパレータおよび非水電解質について詳細に説明する。
外装材は、厚さ0.5mm以下のラミネートフィルムから形成される。また、外装材は厚さ1.0mm以下の金属製容器が用いられる。金属製容器は、厚さ0.5mm以下であることがより好ましい。
負極は、集電体と、この集電体の片面または両面に形成され、活物質、導電剤および結着剤を含む負極層とを備える。
正極は、集電体と、この集電体の片面または両面に形成され、活物質、導電剤および結着剤を含む正極層とを備える。
非水電解質は、例えば電解質を有機溶媒に溶解することにより調製される液状非水電解質、または液状電解質と高分子材料を複合化したゲル状非水電解質が挙げられる。
セパレータは、例えばポリエチレン、ポリプロピレン、セルロース、もしくはポリフッ化ビニリデン(PVdF)を含む多孔質フィルム、または合成樹脂製不織布が挙げられる。好ましい多孔質フィルムは、ポリエチレンまたはポリプロピレンから作られ、一定温度において溶融し、電流を遮断することが可能であるために安全性を向上できる。
<正極の作製>
まず、正極活物質としてリチウムニッケル複合酸化物(LiNi0.82Co0.15Al0.03O2)粉末90重量%、導電剤として、アセチレンブラック5重量%と、ポリフッ化ビニリデン(PVdF)5重量%をN−メチルピロリドン(NMP)に加えて混合してスラリーとし、このスラリーを厚さ15μmのアルミニウム箔からなる集電体の両面に塗布し後、乾燥し、プレスすることにより正極層密度が3.15g/cm3の正極を作製した。
まず、炭酸カリウム(K2CO3)、とアナターゼ型酸化チタン(TiO2)を混合し、1000℃で24時間焼成してK2Ti4O9を合成した。得られたK2Ti4O9をジルコニアビーズで約3時間乾式粉砕して粒度調整した後、純水で洗浄してプロトン交換前駆体とした。得られたプロトン交換前駆体を1M濃度の塩酸溶液中に投入し、25℃の環境で120時間の超音波分散を施して、プロトン交換体を得た。
得られたチタン複合酸化物粉末80重量%、導電剤として、アセチレンブラック10重量%と、ポリフッ化ビニリデン(PVdF)10重量%をN−メチルピロリドン(NMP)加えて混合してスラリーを調製した。このスラリーを厚さ15μmのアルミニウム箔からなる集電体の両面に塗布し、乾燥した後、プレスすることにより負極層密度が1.6g/cm3の負極を作製した。
エチレンカーボネート(EC)、ジエチルカーボネート(DEC)の混合溶媒(体積比率1:2)に、電解質としてのLiPF6を1mol/L溶解することにより液状非水電解質を調製した。
正極、厚さ25μmのポリエチレン製の多孔質フィルムからなるセパレータ、負極、セパレータの順番に積層した後、渦巻き状に捲回した。これを90℃で加熱プレスすることにより、幅が30mmで、厚さが1.8mmの偏平状電極群を作製した。得られた電極群を厚さ25μmの延伸ナイロンフィルムと厚さ40μmのアルミニウムシートと厚さ30μmの直鎖状低密度ポリエチレンフィルムとをこの順序でウレタン系接着剤を介して積層・接着した厚さ0.1mmのラミネートフィルムからなるパックに収納し、80℃で24時間真空乾燥を施した。
粉砕時間、プロトン交換時間、第1加熱処理の温度・時間、昇温速度、および第2加熱処理の温度・時間、昇温速度をそれぞれ下記表1に記載の条件でチタン複合酸化物を合成し、得られたチタン複合酸化物を負極の活物質として用いた以外、実施例1と同様な方法で非水電解質二次電池を組立てた。
第1加熱処理を行う際の昇温速度を300℃/時とし、粉砕時間、プロトン交換時間、および加熱処理(第1加熱処理)の時間・温度をそれぞれ下記表1に記載の条件でチタン複合酸化物を合成し、得られたチタン複合酸化物を負極の活物質として用いた以外、実施例1と同様な方法で非水電解質二次電池を組立てた。
粉砕時間、プロトン交換時間、および加熱処理(第1加熱処理)の時間・温度および昇温速度をそれぞれ下記表3に記載の条件でチタン複合酸化物を合成し、得られたチタン複合酸化物を負極の活物質として用いた以外、実施例1と同様な方法で非水電解質二次電池を組立てた。
Claims (10)
- 単斜晶系β型チタン酸化物または単斜晶系β型チタン複合酸化物を含有する非水電解質電池用活物質であって、前記単斜晶系β型チタン酸化物または単斜晶系β型チタン複合酸化物はX線源CuKα線を用いた広角X線回折法により算出される結晶子径において、2θが48〜49°に存在するピークから算出される結晶子径をX、2θが24〜26°に存在するピークから算出される結晶子径をYとすると、前記Xは前記Yより大きい非水電解質電池用活物質。
- 前記結晶子径XおよびYが次式(1)の関係を満たす請求項1記載の非水電解質電池用活物質。
X/Y≧1.27 …(1) - 前記結晶子径Xは、20nm以上である請求項1記載の非水電解質電池用活物質。
- 前記結晶子径Xは、1μm以下である請求項1記載の非水電解質電池用活物質。
- 外装材;
前記外装材内に収納された正極;
前記外装材内に収納され、前記正極と空間的に離間し、単斜晶系β型チタン酸化物または単斜晶系β型チタン複合酸化物を含有する活物質を含む負極;および
前記外装材内に充填された非水電解質;
を具備し、
前記単斜晶系β型チタン酸化物または単斜晶系β型チタン複合酸化物はX線源CuKα線を用いた広角X線回折法により算出される結晶子径において、2θが48〜49°に存在するピークから算出される結晶子径をX、2θが24〜26°に存在するピークから算出される結晶子径をYとすると、前記Xは前記Yより大きい非水電解質電池。 - 前記結晶子径XおよびYが次式(1)の関係を満たす請求項5記載の非水電解質電池。
X/Y≧1.27 …(1) - 前記結晶子径Xは、20nm以上である請求項5記載の非水電解質電池。
- 前記結晶子径Xは、1μm以下である請求項5記載の非水電解質電池。
- 前記正極は、リチウムニッケル複合酸化物またはリチウムマンガン複合酸化物を含む請求項5記載の非水電解質電池。
- 請求項5記載の非水電解質電池を複数備え、各々の電池が直列、並列または直列および並列に電気的に接続される電池パック。
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Cited By (3)
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US8673500B2 (en) | 2009-07-22 | 2014-03-18 | Kabushiki Kaisha Toshiba | Active material for batteries, non-aqueous electrolyte battery, and battery pack |
US10559820B2 (en) | 2016-03-15 | 2020-02-11 | Kabushiki Kaisha Toshiba | Nonaqueous electrolyte battery, battery pack and vehicle |
US10978691B2 (en) | 2017-09-21 | 2021-04-13 | Kabushiki Kaisha Toshiba | Electrode group, secondary battery, battery pack, and vehicle |
Families Citing this family (9)
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KR101621094B1 (ko) * | 2009-08-20 | 2016-05-16 | 삼성에스디아이 주식회사 | 이차 전지 |
JP4966347B2 (ja) * | 2009-08-25 | 2012-07-04 | 株式会社東芝 | 負極活物質、非水電解質電池及び電池パック |
JP5535160B2 (ja) * | 2011-09-20 | 2014-07-02 | 株式会社東芝 | 非水電解質電池及び電池パック |
JP5567056B2 (ja) * | 2012-03-30 | 2014-08-06 | 株式会社東芝 | 非水電解質電池及び電池パック |
JP6206308B2 (ja) * | 2014-04-11 | 2017-10-04 | 株式会社豊田自動織機 | 電池パック |
JP6538500B2 (ja) | 2015-09-16 | 2019-07-03 | 株式会社東芝 | 非水電解質電池、電池パック、及び車 |
JP7000223B2 (ja) * | 2018-03-26 | 2022-01-19 | 株式会社東芝 | 活物質、活物質複合材料、電極、二次電池、電池パック及び車両 |
JP7027363B2 (ja) * | 2018-09-19 | 2022-03-01 | 株式会社東芝 | リチウム亜鉛二次電池、電池パック、車両及び定置用電源 |
WO2020059185A1 (en) | 2018-09-19 | 2020-03-26 | Kabushiki Kaisha Toshiba | Lithium zinc secondary battery, battery pack, vehicle, and stationary power supply |
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US10978691B2 (en) | 2017-09-21 | 2021-04-13 | Kabushiki Kaisha Toshiba | Electrode group, secondary battery, battery pack, and vehicle |
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WO2011010371A1 (ja) | 2011-01-27 |
US20120171550A1 (en) | 2012-07-05 |
JPWO2011010371A1 (ja) | 2012-12-27 |
CN102414881A (zh) | 2012-04-11 |
CN102414881B (zh) | 2014-06-04 |
US8673500B2 (en) | 2014-03-18 |
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