JP6076928B2 - 電池用活物質材料、非水電解質電池、電池パック及び自動車 - Google Patents
電池用活物質材料、非水電解質電池、電池パック及び自動車 Download PDFInfo
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- JP6076928B2 JP6076928B2 JP2014045366A JP2014045366A JP6076928B2 JP 6076928 B2 JP6076928 B2 JP 6076928B2 JP 2014045366 A JP2014045366 A JP 2014045366A JP 2014045366 A JP2014045366 A JP 2014045366A JP 6076928 B2 JP6076928 B2 JP 6076928B2
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 1
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- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
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- 229910000480 nickel oxide Inorganic materials 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
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- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
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- 238000006557 surface reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical class [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
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- 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
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Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
0.80≦IB/IA≦1.12 (1)
IC/IB≦0.80 (2)。
実施形態によれば、自動車が提供される。この自動車は、上記の電池パックを搭載している。
第1の実施形態に係る電池用活物質材料は、一般式:Ti1-xM1xNb2-yM2yO7の化合物を含む活物質粒子を含む。式中、0≦x<1であり、0≦y<1であり、元素M1及び元素M2はNb、V、Ta、Fe、Ti、Bi、Sb、As、P、Cr、Mo、W、B、Na、Mg、Al及びSiからなる群より選ばれる少なくとも1種である。元素M1と元素M2とは、同じであっても良いし、又は互いに異なっていても良い。この活物質粒子は、Cu―Kα線を用いたX線回折法により得られるX線回折図において、2θ=23.74〜24.14°に現れる(110)面に帰属されるピークAと、2θ=25.81〜26.21°に現れる(003)面に帰属されるピークBと、2θ=26.12〜26.54°に現れる(−602)面に帰属されるピークCとを示す。ピークAの強度IA、ピークBの強度IB及びピークCの強度ICが下記関係式(1)及び(2)を満たす:
0.80≦IB/IA≦1.12 (1)
IC/IB≦0.80 (2)。
(1)X線回折装置:マックサイエンス 社製;M18XHF22−SRA
X線源:CuKα線
出力 :40kV,100mA
スリット系:Div. Slit;0.5°
(2)スキャン方式:2θ/θ連続スキャン
(3)測定範囲(2θ):5〜70°
(4)サンプリング幅(2θ):0.01°
(5)スキャン速度:2°/分。
固相法による従来の合成方法でTiNb2O7を合成した場合、焼結中の反応が速度論的に遅いことから、均質組成の結晶を得るためには1000℃以上の温度でのべ48時間以上の焼成をする必要があり得る。この場合、高結晶材料が得られるものの、粗大粒子かつ緻密な結晶構造となり容量と急速充電特性が低下するという課題があり得る。また、ゾル-ゲル法による従来の合成方法において、1350℃以上の高温処理をする方法が開示されているが、焼成温度が1300℃以上になるとTiNb2O7の結晶成長が急激に進行することから同様の課題があり得る。
第2の実施形態によれば、正極と、上記第1の実施形態に係る電池用活物質材料を含む負極と、非水電解質とを具備することを特徴とする非水電解質電池が提供される。
正極は、集電体と、この集電体の片面もしくは両面に形成され、活物質及び結着剤を含む正極材料層(正極活物質含有層)とを含む。
負極は、集電体と、該集電体の片面若しくは両面に形成され、活物質、導電剤及び結着剤を含む負極材料層(負極活物質含有層)とを含む。
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、又は、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であってよい。
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、またはポリフッ化ビニリデン(PVdF)を含む多孔質フィルム、合成樹脂製不織布から形成されてよい。中でも、ポリエチレン又はポリプロピレンから形成された多孔質フィルムは、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、安全性を向上できる。
外装材は、厚さ0.5mm以下のラミネートフィルムまたは厚さ1mm以下の金属製容器が用いることができる。ラミネートフィルムの厚さは0.2mm以下であることがより好ましい。金属製容器は、厚さ0.5mm以下であることがより好ましく、厚さ0.2mm以下であることがさらに好ましい。
第3の実施形態によれば、電池パックが提供される。この電池パックは、第2の実施形態に係る非水電解質電池を備える。
出発原料として、硫酸チタニルの希硫酸溶液と、塩化ニオブのエタノール溶液とを使用した。両者を、Nb/Tiのモル比が7:3となるように混合し、攪拌しながらアンモニア水で混合溶液のpHを8まで調整した。
この例では、実施例1と同様にして、活物質粒子を得た。
この例では、前駆体合成までの工程において活物質粒子の組成を変化させたこと以外は、実施例1と同様の方法で活物質粒子を合成した。
この例では、前駆体合成までの工程において活物質粒子の組成を変化させたこと以外は、実施例1と同様の方法で活物質粒子を合成した。
この例では、焼成を1100℃で1時間にわたって行った以外は、実施例1と同様の方法で活物質粒子を合成した。
この例では、焼成を700℃で1時間にわたって行った以外は、実施例1と同様の方法で活物質粒子を合成した。
この例では、炭素被覆を実施しなかったこと以外は、実施例3と同様の方法で活物質粒子を合成した。
この例では、炭素被覆を実施しなかったこと以外は、実施例4と同様の方法で活物質粒子を合成した。
この例では、炭素被覆を実施しなかったこと以外は、実施例5と同様の方法で活物質粒子を合成した。
この例では、炭素被覆を実施しなかったこと以外は、実施例6と同様の方法で活物質粒子を合成した。
特許文献1に記載の方法に従って、固相法により活物質粒子TiNb2O7を合成した。
焼成温度を1350℃とした以外は、比較例1と同様にして活物質粒子を合成した。
この例では、出発原料として、硝酸鉄のエタノール溶液と、硫酸チタニルの希硫酸溶液と、塩化ニオブのエタノール溶液とを用いて、混合溶液の組成比を変えたこと以外は、実施例5と同様の方法で活物質粒子を合成した。
この例では、出発原料として、塩化タンタルのエタノール溶液と、硫酸チタニルの希硫酸溶液と、塩化ニオブのエタノール溶液とを用いて混合溶液の組成比を変えたこと以外は、実施例5と同様の方法で活物質粒子を合成した。
この例では、出発原料として、塩化モリブデンのエタノール溶液と、硫酸チタニルの希硫酸溶液と、塩化ニオブのエタノール溶液とを用いて、混合溶液の組成比を変えたこと以外は、実施例5と同様の方法で活物質粒子を合成した。
この例では、出発原料として、塩化バナジウムのエタノール溶液と、硫酸チタニルの希硫酸溶液と、塩化ニオブのエタノール溶液とを用いて、混合溶液の組成比を変えたこと以外は、実施例5と同様の方法で活物質粒子を合成した。
実施例11〜14では、実施例5と同様の実験方法及び評価方法で、Ti1-xM1xNb2-yM2yO7でにおける元素M1及び/又はM2の種類及び/又は量を変えた場合の結果を示している。表2の結果から、実施例11〜14では、実施例5と比較し、0.2C/20C放電容量比が改善されていることが分かる。これは、元素Ti及び/又は元素Nbの一部を価数の異なる元素M1及びM2のそれぞれにより置換することで、活物質の電子導電性が向上することによる効果と推察される。さらに、実施例13のMo元素、実施例14のV元素を置換した系においては、Moを含む原料、Vを含む原料がそれぞれ焼結助剤として機能するため、900℃1時間という焼成条件においても同等以上の特性が得られていることが分かる。
実施例1で得た活物質を用いて、先に説明した手順で、もう1つの三電極式ビーカーセルを作製した。このセルに対して、カットオフ電位1.2V〜2.0Vとした、充放電電流1Cのサイクル試験を実施した。サイクル数は500サイクルとし、サイクル試験の評価温度は25℃とした。初回及び500サイクル後の容量を測定した。初回サイクルに対する500サイクル後の容量を、容量維持率(%)とした。実施例1の500サイクル後の容量維持率は76.8%であった。
以下に、本願の出願当初の特許請求の範囲に記載していた発明を付記する。
[1]一般式:Ti 1-x M1 x Nb 2-y M2 y O 7 (式中、0≦x<1であり、0≦y<1であり、元素M1及び元素M2はNb、V、Ta、Fe、Ti、Bi、Sb、As、P、Cr、Mo
、W、B、Na、Mg、Al及びSiからなる群より選ばれる少なくとも一種であり、前記元素M1と前記元素M2とは、同じであっても良いし、又は互いに異なっていても良い)で表される化合物を含み、Cu―Kα線を用いるX線回折法により得られるX線回折図において、2θ=23.74〜24.14°に現れる(110)面に帰属されるピークAと、2θ=25.81〜26.21°に現れる(003)面に帰属されるピークBと、2θ=26.12〜26.54°に現れる(−602)面に帰属されるピークCとを示し、前記ピークAの強度I A 、前記ピークBの強度I B 及び前記ピークCの強度I C が下記関係式(1)及び(2)を満たす活物質粒子を含む電池用活物質材料。
0.80≦I B /I A ≦1.12 (1)
I C /I B ≦0.80 (2)
[2]一般式:Ti 1-x M x Nb 2 O 7 (式中、0≦x<1であり、元素MはNb、V、Ta、Bi、Sb、As、P、Cr、Mo、W、B、Na、Mg、Al及びSiからなる群より選ばれる少なくとも一種である)で表される化合物を含み、Cu―Kα線を用いるX線回折法により得られるX線回折図において、2θ=23.74〜24.14°に現れる(110)面に帰属されるピークAと、2θ=25.81〜26.21°に現れる(003)面に帰属されるピークBと、2θ=26.12〜26.54°に現れる(−602)面に帰属されるピークCとを示し、前記ピークAの強度I A 、前記ピークBの強度I B 及び前記ピークCの強度I C が下記関係式(1)及び(2)を満たす活物質粒子を含む電池用活物質
材料。
0.80≦I B /I A ≦1.12 (1)
I C /I B ≦0.80 (2)
[3]炭素材料を更に含む[1]又は[2]に記載の電池用活物質材料。
[4]前記炭素材料が前記活物質粒子の表面の少なくとも一部を被覆している[3]に記載の電池用活物質材料。
[5]正極と、[1]乃至[4]の何れか1つに記載の電池用活物質材料を含む負極と、非水電解質と、を具備する非水電解質電池。
[6][5]記載の非水電解質電池を備える電池パック。
Claims (9)
- 一般式:Ti1-xM1xNb2-yM2yO7(式中、0≦x<1であり、0≦y<1であり、元素M1及び元素M2はNb、V、Ta、Fe、Ti、Bi、Sb、As、P、Cr、Mo、W、B、Na、Mg、Al及びSiからなる群より選ばれる少なくとも一種であり、前記元素M1と前記元素M2とは、同じであっても良いし、又は互いに異なっていても良い)で表される化合物を含み、Cu―Kα線を用いるX線回折法により得られるX線回折図において、2θ=23.74〜24.14°に現れる(110)面に帰属されるピークAと、2θ=25.81〜26.16°に現れる(003)面に帰属されるピークBと、2θ=26.31〜26.54°に現れる(−602)面に帰属されるピークCとを示し、前記ピークAの強度IA、前記ピークBの強度IB及び前記ピークCの強度ICが下記関係式(1)及び(2)を満たす活物質粒子を含む電池用活物質材料。
0.80≦IB/IA≦1.12 (1)
IC/IB≦0.80 (2) - 一般式:Ti1-xMxNb2O7(式中、0≦x<1であり、元素MはNb、V、Ta、Bi、Sb、As、P、Cr、Mo、W、B、Na、Mg、Al及びSiからなる群より選ばれる少なくとも一種である)で表される化合物を含み、Cu―Kα線を用いるX線回折法により得られるX線回折図において、2θ=23.74〜24.14°に現れる(110)面に帰属されるピークAと、2θ=25.81〜26.16°に現れる(003)面に帰属されるピークBと、2θ=26.31〜26.54°に現れる(−602)面に帰属されるピークCとを示し、前記ピークAの強度IA、前記ピークBの強度IB及び前記ピークCの強度ICが下記関係式(1)及び(2)を満たす活物質粒子を含む電池用活物質材料。
0.80≦IB/IA≦1.12 (1)
IC/IB≦0.80 (2) - 炭素材料を更に含む請求項1又は2に記載の電池用活物質材料。
- 前記炭素材料が前記活物質粒子の表面の少なくとも一部を被覆している請求項3に記載の電池用活物質材料。
- 正極と、
請求項1乃至4の何れか1項記載の電池用活物質材料を含む負極と、
非水電解質と、
を具備する非水電解質電池。 - 請求項5記載の非水電解質電池を備える電池パック。
- 複数の前記非水電解質電池を備え、
前記複数の非水電解質電池は、直列に、並列に、又は直列及び並列の組み合わせにより電気的に接続されている請求項6記載の電池パック。 - 通電用の外部端子と、
保護回路と
を更に含む請求項6又は7に記載の電池パック。 - 請求項6乃至8の何れか1項に記載の電池パックを搭載した自動車。
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CN111137919B (zh) * | 2018-11-06 | 2022-08-12 | 财团法人工业技术研究院 | 掺杂铌酸钛与电池 |
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JP7159133B2 (ja) * | 2019-09-17 | 2022-10-24 | 株式会社東芝 | 電極、二次電池、電池パック及び車両 |
CN111416116B (zh) * | 2020-03-27 | 2021-06-29 | 宁德新能源科技有限公司 | 正极活性材料及包含其的电化学装置 |
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JP7480096B2 (ja) * | 2021-09-08 | 2024-05-09 | 株式会社東芝 | 活物質、電極、二次電池、電池パック、及び車両 |
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US20080261113A1 (en) | 2006-11-15 | 2008-10-23 | Haitao Huang | Secondary electrochemical cell with high rate capability |
JP5706327B2 (ja) | 2008-10-23 | 2015-04-22 | サントル ナスィオナル ド ラ ルシェルシュ スィアンティフィク | 無機化合物の製造方法 |
JP2010287496A (ja) * | 2009-06-12 | 2010-12-24 | Mitsubishi Chemicals Corp | 非水電解質二次電池用負極材、非水電解質二次電池用負極及びそれを用いた非水電解質二次電池 |
KR20130096258A (ko) * | 2010-07-30 | 2013-08-29 | 더 보드 오브 리전츠 오브 더 유니버시티 오브 텍사스 시스템 | 니오븀 옥사이드 조성물 및 이를 사용하는 방법 |
JP5230713B2 (ja) * | 2010-10-29 | 2013-07-10 | 株式会社東芝 | 電池用活物質、非水電解質電池及び電池パック |
CN102479950B (zh) * | 2010-11-23 | 2015-06-24 | 中国科学院物理研究所 | 铌酸钛复合材料、其制备方法及含该复合材料的负极和电池 |
JP5649492B2 (ja) | 2011-03-22 | 2015-01-07 | 株式会社東芝 | 電池用活物質、非水電解質電池及び電池パック |
FR2996838B1 (fr) * | 2012-10-17 | 2014-11-21 | Commissariat Energie Atomique | Procede de preparation d'un oxyde mixte de titane et de niobium par traitement solvothermal ; electrode et accumulateur au lithium comprenant ledit oxyde mixte |
FR3001725B1 (fr) * | 2013-02-06 | 2017-10-20 | Commissariat Energie Atomique | Oxyde mixte de titane et de niobium comprenant un metal trivalent |
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US10608250B2 (en) | 2017-09-20 | 2020-03-31 | Kabushiki Kaisha Toshiba | Active material, active material composite material, electrode, secondary battery, battery pack, and vehicle |
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JP2014209445A (ja) | 2014-11-06 |
KR20170141641A (ko) | 2017-12-26 |
EP2784026B1 (en) | 2016-02-03 |
US20140295231A1 (en) | 2014-10-02 |
KR20140117273A (ko) | 2014-10-07 |
US10361429B2 (en) | 2019-07-23 |
CN104078660A (zh) | 2014-10-01 |
EP2784026A1 (en) | 2014-10-01 |
KR101930572B1 (ko) | 2018-12-18 |
KR101930648B1 (ko) | 2018-12-18 |
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