JP6865355B2 - 電気化学デバイスおよびこれに用いる負極とその製造方法 - Google Patents
電気化学デバイスおよびこれに用いる負極とその製造方法 Download PDFInfo
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- JP6865355B2 JP6865355B2 JP2018503052A JP2018503052A JP6865355B2 JP 6865355 B2 JP6865355 B2 JP 6865355B2 JP 2018503052 A JP2018503052 A JP 2018503052A JP 2018503052 A JP2018503052 A JP 2018503052A JP 6865355 B2 JP6865355 B2 JP 6865355B2
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Images
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
- H01M4/0438—Processes of manufacture in general by electrochemical processing
- H01M4/0459—Electrochemical doping, intercalation, occlusion or alloying
-
- 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
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- 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
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- 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
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- 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
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- 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
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Description
(負極)
負極は、負極集電体と、負極集電体の一方の面に担持された第1負極活物質層と、負極集電体の他方の面に担持された第2負極活物質層と、を具備する。第1負極活物質層および第2負極活物質層は、単位質量当たりの容量が異なる点以外、同様に形成される。
負極活物質としては、炭素材料、金属化合物、合金、セラミックス材料などが挙げられる。炭素材料としては、難黒鉛化炭素(ハードカーボン)、易黒鉛化炭素(ソフトカーボン)、黒鉛などが好ましく、高出力を得る観点からは、ハードカーボンが特に好ましい。金属化合物としては、ケイ素酸化物、錫酸化物などが挙げられる。合金としては、ケイ素合金、錫合金などが挙げられる。セラミックス材料としては、チタン酸リチウム、マンガン酸リチウムなどが挙げられる。これらは単独で用いてもよく、2種以上を組み合わせて用いてもよい。
(正極)
正極は、例えば、正極集電体と、正極集電体の表面に担持された正極活物質層とを具備する。
(リチウムイオン伝導性の非水電解液)
リチウムイオン伝導性を有する非水電解液は、リチウム塩と、リチウム塩を溶解させる非水溶媒とを含む。リチウム塩に由来するアニオンは、電気化学デバイスの充放電に伴って正極へのドープと脱ドープとを可逆的に繰り返す。一方、リチウム塩に由来するリチウムイオンは、電気化学デバイスの充放電に伴って負極に吸蔵または負極から放出される。
組み合わせて用いてもよい。非水電解液中のリチウム塩の濃度は、例えば0.2〜4mol/Lであればよく、特に限定されない。
(セパレータ)
セパレータとしては、セルロース繊維製の不織布、ガラス繊維製の不織布、ポリオレフィン製の微多孔膜、織布、不織布などが好ましく用いられる。セパレータの厚みは、例えば10〜300μmであり、10〜40μmが好ましい。
(i)負極を準備する工程
まず、負極活物質、結着剤および導電剤を含む負極合剤を液状成分(分散媒)に分散させて、組成の異なる第1スラリーと第2スラリーを調製する。分散媒には、水、N−メチル−2−ピロリドン(NMP)などが好ましく用いられる。
(ii)正極を準備する工程
正極は、例えば、正極集電体に導電性高分子を付着させることにより製造される。例えば、正極集電体を、導電性高分子の原料である重合性化合物(モノマーもしくはオリゴマ
ー)を含む溶液(重合液)に浸漬し、正極集電体の存在下で重合性化合物を重合することにより、正極集電体の表面を覆う導電性高分子の被膜が形成される。導電性高分子の被膜は、正極活物質層として機能する。
(iii)電極群を形成する工程
負極へのリチウムイオンのプレドープは、電極群にリチウム箔を組み込み、非水電解液とともに電極群を電気化学デバイスのケースに収容してから進行させることが効率的である。その際、電極群を形成する前に、負極の表面にリチウム箔が貼り付けられる。このとき、第1負極活物質層にはリチウム箔を貼り付けず、第2負極活物質層にリチウム箔を貼り付けることで、リチウム箔の貼り付け工程が簡略化されるとともに、厚さ10μm以上、更には15μm以上のリチウム箔を用いることが可能となり、製造コストを大きく削減することが可能になる。その後、正極とリチウム箔が貼り付けられた負極とを、セパレータを介して捲回または積層して、電極群が形成される。
(iv)負極にリチウムイオンをプレドープする工程
電極群は、非水電解液とともに、例えば、開口を有する有底ケースに収容される。その後、開口は封口体により塞がれ、電気化学デバイスが完成する。図1は、電気化学デバイスの一例の断面模式図であり、図2は、同電気化学デバイスの一部を展開した概略図である。すなわち、電極群は、ケース内で非水電解液と接触する。電極群に非水電解液が含浸され、リチウム箔と非水電解液とが接触すると、リチウムイオンが非水電解液に溶出し、電極群の内部を移動して、第1負極活物質層および第2負極活物質層に含まれる負極活物質にドープされる。このとき、正極集電体および負極集電体の少なくとも一方が、リチウムイオン透過性を有することで、リチウムイオンのプレドープが迅速に進行する。また、
リチウムイオンの移動の自由度が大きいため、リチウムイオンは負極の全体に均一にプレドープされ易くなる。
[実験例]
本発明の効果を確認するために、以下の実験を行った。
《実験例1》
(1)正極の作製
約2cm角の平面形状を有し、厚さ30μm、開口率10%のアルミニウム箔を原料とするパンチングメタルを正極集電体として準備した。パンチングメタルの両面に、厚さ1.5μmの導電性カーボン層を形成した。導電性カーボン層は、カーボンブラック100質量部と結着剤30質量部との混合層である。
(2)負極の作製
(第1負極)
約2cm角の平面形状を有し、厚さ20μmの銅箔を第1負極集電体として準備した。次に、ハードカーボン97質量部と、カルボキシメチルセルロース(CMC)1.5質量部と、スチレンブタジエンゴム(SBR)2質量部とを混合した第1負極合剤を水に分散させ、固形分40質量%の第1スラリーを調製した。第1スラリーを第1負極集電体の一方の表面に塗布し、乾燥させた。乾燥後、圧延を行い、第1負極集電体の一方の表面に厚さ(T1)58μmの第1負極活物質層を有する第1負極を得た。
(第2負極)
第1負極集電体と同様の銅箔を第2負極集電体として準備した。次に、ハードカーボン93.5質量部と、カルボキシメチルセルロース(CMC)1.5質量部と、スチレンブタジエンゴム(SBR)5質量部とを混合した第2負極合剤を水に分散させ、固形分40質量%の第2スラリーを調製した。第2スラリーを第2負極集電体の一方の表面に塗布し、乾燥させた。乾燥後、圧延を行い、第2負極集電体の一方の表面に厚さ(T2)60μmの第2負極活物質層を有する第2負極を得た。
(3)電極群の形成
第2負極活物質層の表面に、厚さ15μmのリチウム箔を貼り付けた。その後、正極、第1負極、第2負極にそれぞれリードタブを接続した。次に、セルロース製不織布のセパレータ(厚さ35μm)を介在させて、第1負極の第1負極活物質層と、正極の一方の表面に形成された正極活物質層とを対向させた。また、同様のセパレータを介在させて、正極の他方の面に形成された正極活物質層と、第2負極の第2負極活物質層(リチウム箔が貼り付けられた面)とを対向させた。このように、第1負極、セパレータ、正極、セパレータおよび第2負極を、この順で重ねて積層体を作製して電極群を得た。
(4)非水電解液
プロピレンカーボネートとジメチルカーボネートとの体積比1:1の混合物に、ビニレンカーボネートを0.2質量%添加して、非水溶媒を調製した。得られた非水溶媒にLiPF6を2mol/Lの濃度で溶解させて、正極にドープおよび脱ドープされるアニオン
としてヘキサフルオロ燐酸イオン(PF6 −)を有する非水電解液を調製した。
(5)電気化学デバイスの作製
電極群と非水電解液とをAlラミネートシートからなる袋状の外装体の中に収容し、封止することにより、電気化学デバイスを組み立てた。その後、25℃で24時間放置(エージング)して、リチウムイオンの負極へのプレドープを進行させることにより、電気化学デバイス(A1)を完成させた。
《実験例2》
第1スラリーを用いて第2負極集電体の表面に厚さ58μmの第2負極活物質層を形成したこと以外、実験例1と同様に、電気化学デバイス(B1)を作製した。設計容量は実験例1と同じとした。
《実験例3》
第2スラリーを用いて第1負極集電体の表面に厚さ60μmの第2負極活物質層を形成したこと以外、実験例1と同様に、電気化学デバイス(B2)を作製した。設計容量は実験例1と同じとした。
[評価]
電気化学デバイスの初期の放電容量(C0)と内部抵抗(R0)を25℃と−10℃において、放電電流25mA、電圧範囲3.8V〜3.0Vで測定した。
Claims (8)
- 負極集電体と、
前記負極集電体の一方の面に担持された第1負極活物質層と、
前記負極集電体の他方の面に担持された第2負極活物質層と、を具備し、
前記第1負極活物質層の単位質量当たりの容量C1が、前記第2負極活物質層の単位質量当たりの容量C2よりも大きく、
前記第1負極活物質層の厚さT1が、前記第2負極活物質層の厚さT2よりも薄い、電気化学デバイス用負極。 - 負極集電体と、
前記負極集電体の一方の面に担持された第1負極活物質層と、
前記負極集電体の他方の面に担持された第2負極活物質層と、を具備し、
前記第1負極活物質層の単位質量当たりの容量C1が、前記第2負極活物質層の単位質量当たりの容量C2よりも大きく、
前記第1負極活物質層の単位面積当たりの容量Cs1と、前記第2負極活物質層の単位面積当たりの容量Cs2とが、0.99≦Cs1/Cs2≦1.01を満たす、電気化学デバイス用負極。 - 前記第1負極活物質層および前記第2負極活物質層が、それぞれリチウムイオンのドープおよび脱ドープが可能な負極活物質と、結着剤とを含み、前記第1負極活物質層の単位質量当たりに含まれる前記結着剤の含有量X1が、前記第2負極活物質層の単位質量当たりに含まれる前記結着剤の含有量X2よりも少ない、請求項1または2に記載の電気化学デバイス用負極。
- 正極、請求項1〜3のいずれか1項に記載の負極、前記正極と前記負極との間に介在するセパレータおよびリチウムイオン伝導性の非水電解液を具備する、電気化学デバイス。
- 前記正極は、正極集電体と、前記正極集電体の表面に担持された正極活物質層とを具備し、
前記正極集電体および前記負極集電体の少なくとも一方が、リチウムイオン透過性を有する、請求項4に記載の電気化学デバイス。 - 負極集電体と、前記負極集電体の一方の面に担持された第1負極活物質層と、前記負極集電体の他方の面に担持された第2負極活物質層と、を具備する負極を準備する工程と、
正極集電体と、前記正極集電体の表面に担持された正極活物質層とを具備する正極を準備する工程と、
前記第2負極活物質層の表面にリチウム箔を貼り付ける工程と、
前記正極と前記リチウム箔が貼り付けられた前記負極とを、セパレータを介して捲回または積層して電極群を形成する工程と、
前記電極群を非水電解液と接触させて、前記リチウム箔からリチウムを前記第1負極活物質層および前記第2負極活物質層にドープする工程と、を有し、
前記第1負極活物質層の単位質量当たりの容量C1が、前記第2負極活物質層の単位質量当たりの容量C2よりも大きい、電気化学デバイスの製造方法。 - 前記正極集電体および前記負極集電体の少なくとも一方が、リチウムイオン透過性を有する、請求項6に記載の電気化学デバイスの製造方法。
- 前記リチウム箔の厚さが、10μm以上である、請求項6または7に記載の電気化学デバイスの製造方法。
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