JP7451009B2 - 全固体電池用負極の製造方法 - Google Patents
全固体電池用負極の製造方法 Download PDFInfo
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- JP7451009B2 JP7451009B2 JP2021549534A JP2021549534A JP7451009B2 JP 7451009 B2 JP7451009 B2 JP 7451009B2 JP 2021549534 A JP2021549534 A JP 2021549534A JP 2021549534 A JP2021549534 A JP 2021549534A JP 7451009 B2 JP7451009 B2 JP 7451009B2
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- negative electrode
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- electrolyte
- state battery
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- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
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- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical group [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-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
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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
- H01M4/049—Manufacturing of an active layer by chemical means
-
- 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
-
- 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
-
- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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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Description
負極活物質として人造黒鉛、導電材としてカーボンブラック、固体電解質としてポリエチレンオキシド(PEO)を含むパウダー混合物を準備し、前記パウダー混合物を、図1のように内側面にリチウム金属処理されている反応器に投入する。
前記実施例のようにリチウム金属処理されている反応器でSEI膜を形成するための反応を実施しなかった人造黒鉛、カーボンブラック及びポリエチレンオキシドを含むパウダー混合物を用いた点を除き、前記実施例と同様な方法でコインハーフセルを製造した。
前記実施例及び比較例で製造されたコインハーフセルに対して0.05Cで定電流/定電圧(CC/CV)充電を遂行し、カットオフ(cut-off)の際に電圧が0.005V、Cレート(rate)が0.02Cになるまで充電を遂行し、0.05Cで1.5Vになるまで放電する過程を1回遂行した。前記1回充放電の結果を図2に示した。
前記実験例1と同じ条件で充電及び放電を繰り返し実施しながら充放電回数による容量維持率(cycle retention)を測定し、その結果を図3に示した。
Claims (11)
- 全固体電池用負極の製造方法であって、
(a)負極活物質、固体電解質及び導電剤を含むパウダー混合物を準備する段階と、
(b)前記パウダー混合物を反応器に投入する段階と、
(c)前記反応器に電解液を投入する段階と、
(d)前記反応器を回転させて固体電解質界面(Solid Electrolyte Interface;SEI膜)を形成する段階と、
を含み、
前記反応器は内側面がリチウム金属処理されている、全固体電池用負極の製造方法。 - 前記反応器の内側面にあるリチウム金属が電解液と反応してSEI膜を形成する、請求項1に記載の全固体電池用負極の製造方法。
- 前記段階(c)で添加剤をさらに追加し、
前記添加剤は、ビニルカーボネート、ビニルエチレンカーボネート、フルオロカーボネート及びサクシノニトリルからなる群から選択される1種以上である、請求項1または2に記載の全固体電池用負極の製造方法。 - 前記電解液を投入する前に、パウダー混合物が投入された反応器を回転させて負極活物質とリチウム金属の接触面を増加させる、請求項1から3のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記段階(b)と段階(c)を同時に遂行し、前記負極活物質は、表面に形成されたSEI膜が均一な形態に形成される、請求項1から4のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記電解液は環状カーボネート系電解液である、請求項1から5のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記段階(d)は、前記反応器を加熱する過程を含む、請求項1から6のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記段階(d)の後に、前記反応器内の物質を洗浄及び乾燥する過程をさらに含む、請求項1から7のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記乾燥する過程の後に、残余物を篩で濾す過程を含む、請求項8に記載の全固体電池用負極の製造方法。
- 前記固体電解質は、酸化物系、硫化物系又は高分子系の固体電解質である、請求項1から9のいずれか一項に記載の全固体電池用負極の製造方法。
- 前記SEI膜は主生成物及び副生成物を含み、
前記主生成物はリチウムを含む有機物から構成され、負極活物質に対する付着状態が維持され、
前記副生成物はLi2O及び/又はLi2CO3である、請求項1に記載の全固体電池用負極の製造方法。
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