JPWO2016076387A1 - 蓄電デバイス用負極組成物、その組成物を含む負極および蓄電デバイスならびに蓄電デバイス用負極の製造方法 - Google Patents
蓄電デバイス用負極組成物、その組成物を含む負極および蓄電デバイスならびに蓄電デバイス用負極の製造方法 Download PDFInfo
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- JPWO2016076387A1 JPWO2016076387A1 JP2016559102A JP2016559102A JPWO2016076387A1 JP WO2016076387 A1 JPWO2016076387 A1 JP WO2016076387A1 JP 2016559102 A JP2016559102 A JP 2016559102A JP 2016559102 A JP2016559102 A JP 2016559102A JP WO2016076387 A1 JPWO2016076387 A1 JP WO2016076387A1
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- negative electrode
- sodium
- active material
- storage device
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Images
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- H—ELECTRICITY
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Abstract
Description
最初に、本発明の実施形態の内容を列記して説明する。
次に、本発明の実施形態を、図面を参照しながら説明する。なお、本発明は以下の例示に限定されるものではなく、添付の特許請求の範囲によって示され、特許請求の範囲と均等の意味および範囲内での全ての変更が含まれることが意図される。
まず、負極活物質層の前駆体である負極組成物について説明する。
負極組成物は、ナトリウムイオンを可逆的に担持する負極活物質と、金属ナトリウムとを含む。負極組成物は、更に、任意成分として、結着剤、導電助剤、液状分散媒(第一分散媒)などを含んでもよい。
負極組成物を負極集電体の表面に固定化することにより、負極前駆体を得ることができる。負極前駆体は、例えば、負極組成物である負極スラリーを負極集電体の表面に塗布し、乾燥し、必要に応じて圧延することなどにより形成できる。
正極は、正極活物質を含む。正極活物質は、電気化学的にナトリウムイオンを吸蔵および放出することが好ましい。正極は、正極集電体および正極集電体の表面に固定化された正極活物質を含み、任意成分として、結着剤、導電助剤などを含んでもよい。
セパレータは、正極と負極とを物理的に隔絶して、内部短絡を防止する役割を果たす。セパレータは、多孔質材料からなり、当該多孔質材料の空隙には電解質が含浸され、電池反応を確保するために、ナトリウムイオン透過性を有する。セパレータとしては、例えば、樹脂製の微多孔膜の他、不織布などが使用できる。セパレータの厚さは、特に限定されないが、例えば、10〜300μm程度の範囲から選択できる。
ナトリウムイオン伝導性を有する電解質は、少なくともナトリウム塩を含む。電解質には、ナトリウム塩を含むイオン液体を用いてもよく、ナトリウム塩を溶解させた有機溶媒(有機電解質)を用いてもよい。有機電解質に含まれるナトリウム塩の濃度は、例えば0.3〜3mol/リットルであればよい。
次に、蓄電デバイスの一例としてナトリウムイオン電池の構造について説明する。
(1)正極の作製
NaCrO2(正極活物質)とアセチレンブラック(導電助剤)とポリフッ化ビニリデン(PVDF)(結着剤)とを、正極活物質/導電助剤/結着剤(質量比)が85/10/5となるようにN−メチル−2−ピロリドン(NMP)に混合して、正極スラリーを調製した。得られた正極スラリーを、正極集電体としてのアルミニウム箔の片面に塗布し、乾燥後に圧縮し、150℃で真空乾燥後、円形に打ち抜くことで、円盤状の正極(直径12mm、正極活物質層の厚み85μm)を作製した。得られた正極の単位面積当たりの正極活物質の質量は、13.3mg/cm2であった。
(第一工程)
溶融金属ナトリウムを鋳型中で固化させた後、取り出した。得られた固体の金属ナトリウムを、露点が−10℃以下、酸素濃度0.01%以下の4Nグレードの窒素雰囲気(グローブボックス中)に移した。グローブボックス中で、固体の金属ナトリウム10.2gと、ノルマルパラフィン90gとを、四つ口フラスコに投入した。その後、金属ナトリウムの融点以上に加熱しながら撹拌し、ナトリウムを分散させ、金属ナトリウム粒子を10質量%含むディスパージョンを得た。
得られた負極組成物を、負極集電体としてのアルミニウム箔に塗布した。
負極集電体に塗布された負極組成物を130℃で乾燥させ、第一分散媒および第二分散媒を蒸発させた。乾燥後の負極組成物には、第一分散媒および第二分散媒を合計で負極活物質100質量部あたり0.01質量部残存させた。その後、負極組成物を圧延し、円形に打ち抜くことで、円盤状の負極前駆体(直径12mm、負極活物質層の前駆体の厚み70μm)を得た。負極前駆体の単位面積当たりの負極活物質の質量は、5.4mg/cm2であった。
得られた正極と負極前駆体とを用いてコイン型電池を作製した。ここでは、コイン型電池の容器の内底部に負極前駆体を配置し、負極前駆体上にセパレータを配置した。次に、正極を負極と対向するように、セパレータを介在させた状態で配置した。その後、容器内に電解質を注液し、周縁に絶縁性ガスケットを備えた蓋体を、電池容器の開口部に嵌め込むことで、コイン型のナトリウムイオン電池(電池A1)を作製した。セパレータとしては、耐熱性ポリオレフィン製の微多孔膜(厚さ50μm)を用いた。なお、正極の可逆容量に対する負極の可逆容量の比Cn/Cpは1とした。
以下の点以外は、実施例1と同様にして、電池B1を作製した。
(第一工程)
金属ナトリウムのディスパージョンを用いないこと以外、実施例1と同様に、負極組成物(負極スラリー)を調製した。
得られた負極組成物を、負極集電体としてのアルミニウム箔に塗布した。
負極集電体に塗布された負極組成物を130℃で乾燥させ、第一分散媒および第二分散媒を蒸発させた。乾燥条件を整合させる観点から、乾燥後の負極組成物には、第一分散媒および第二分散媒を合計で負極活物質100質量部あたり0.01質量部残存させた。その後、負極組成物を圧延し、円形に打ち抜くことで、円盤状の負極(直径12mm、負極活物質層の厚み70μm)を得た。負極の単位面積当たりの負極活物質の質量は、5.4mg/cm2であった。
得られた正極と負極前駆体とを用いてコイン型電池を作製した。ここでは、コイン型電池の容器の内底部に、厚さ50μmの金属ナトリウム箔を貼り付けた。その後、金属ナトリウム箔の上に負極を配置し、負極上にセパレータを配置した。次に、正極を負極と対向するように、セパレータを介在させた状態で配置した。その後、容器内に電解質を注液し、周縁に絶縁性ガスケットを備えた蓋体を、電池容器の開口部に嵌め込むことで、コイン型のナトリウムイオン電池(電池B1)を作製した。
ナトリウムイオン電池を、60℃になるまで加熱し、時間率1Cレートの電流値で3.3Vになるまで定電流充電し、3.3Vで定電圧充電(初回充電)を行った。次いで、時間率1Cレートの電流値で、1.8Vになるまで放電(初回放電)を行い、初回放電時の電池の放電容量(1サイクル目の放電容量)を測定した。
Claims (11)
- ナトリウムイオンを可逆的に担持する負極活物質と、金属ナトリウムとを含む、蓄電デバイス用負極組成物。
- 前記金属ナトリウムが、金属ナトリウム粒子である、請求項1に記載の蓄電デバイス用負極組成物。
- 前記負極活物質が有する不可逆容量の10〜200%に相当する量の前記金属ナトリウムを含む、請求項1または2に記載の蓄電デバイス用負極組成物。
- 前記負極活物質の少なくとも一部と、前記金属ナトリウムの少なくとも一部とが、混在している、請求項1〜3のいずれか1項に記載の蓄電デバイス用負極組成物。
- 前記金属ナトリウムが、10〜60μmの平均粒径Dを有する、請求項1〜4のいずれか1項に記載の蓄電デバイス用負極組成物。
- 前記金属ナトリウムの一部が、イオン化して前記負極活物質に吸蔵されている、請求項1〜5のいずれか1項に記載の蓄電デバイス用負極組成物。
- 請求項6に記載の負極組成物と、前記負極組成物を保持する負極集電体とを備える、蓄電デバイス用負極。
- 請求項7に記載の負極と、正極活物質を含む正極と、前記負極と前記正極との間に介在するセパレータと、ナトリウムイオン伝導性を有する電解質とを含む、蓄電デバイス。
- 前記電解質が、アニオンとカチオンとで構成されるイオン液体を含む、請求項8に記載の蓄電デバイス。
- 前記アニオンの90モル%以上が、フッ素含有ビススルホニルアミドアニオンである、請求項9に記載の蓄電デバイス。
- ナトリウムイオンを可逆的に担持する負極活物質と、金属ナトリウムと、前記負極活物質および前記金属ナトリウムを分散させる液状分散媒とを含む、負極組成物を調製する工程と、
前記負極組成物を、負極集電体に保持させる工程と、
前記負極集電体に保持させた負極組成物から、前記液状分散媒の少なくとも一部を蒸発させることにより、前記負極活物質と、前記金属ナトリウムと、前記負極集電体とを備える負極前駆体を得る工程と、
前記負極前駆体を、ナトリウムイオン伝導性を有する電解質と接触させ、前記金属ナトリウムをイオン化させて前記負極活物質にドープする工程と
を含む、蓄電デバイス用負極の製造方法。
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JP2013175311A (ja) * | 2012-02-23 | 2013-09-05 | National Institute Of Advanced Industrial & Technology | ナトリウム二次電池正極材料、該ナトリウム二次電池用正極材料の製造方法、該ナトリウム二次電池用正極材料を用いるナトリウム二次電池用電極、該ナトリウム二次電池用電極を備える非水系ナトリウム二次電池、及び該非水系ナトリウム二次電池を用いる電気機器 |
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JP6666259B2 (ja) | 2020-03-13 |
US20180151877A2 (en) | 2018-05-31 |
CN107078286B (zh) | 2021-04-16 |
TWI597887B (zh) | 2017-09-01 |
US20170324086A1 (en) | 2017-11-09 |
WO2016076387A1 (ja) | 2016-05-19 |
KR102376834B1 (ko) | 2022-03-21 |
CN107078286A (zh) | 2017-08-18 |
US10886531B2 (en) | 2021-01-05 |
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