JP6793813B2 - 全固体電池用電極及びその製造方法 - Google Patents
全固体電池用電極及びその製造方法 Download PDFInfo
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- JP6793813B2 JP6793813B2 JP2019506730A JP2019506730A JP6793813B2 JP 6793813 B2 JP6793813 B2 JP 6793813B2 JP 2019506730 A JP2019506730 A JP 2019506730A JP 2019506730 A JP2019506730 A JP 2019506730A JP 6793813 B2 JP6793813 B2 JP 6793813B2
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- 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
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 229920003050 poly-cycloolefin Polymers 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003047 styrene-styrene-butadiene-styrene Polymers 0.000 description 1
- ZVTQDOIPKNCMAR-UHFFFAOYSA-N sulfanylidene(sulfanylideneboranylsulfanyl)borane Chemical compound S=BSB=S ZVTQDOIPKNCMAR-UHFFFAOYSA-N 0.000 description 1
- VDNSGQQAZRMTCI-UHFFFAOYSA-N sulfanylidenegermanium Chemical compound [Ge]=S VDNSGQQAZRMTCI-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
-
- 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
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
-
- 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
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Description
[製造例1−1.負極の製造]
天然黒鉛(AGP8)、VGCF、BR(ブタジエンゴム)及びHNBR(水素化ニトリルブタジエンゴム)を重量比で94:2:3.96:0.04の比率でキシレンに投入し、乳鉢ミキシングして均一な負極スラリーを得た。スラリーの混合中に架橋開始剤としてDCP(過酸化ジクミル)を添加した。DCP溶液(キシレン中に40%含量)はBRとHNBRの100重量部に対して5重量部の比率で添加された(固形分基準)。前記スラリーを銅薄膜に250μmの厚さで塗布した後、25℃で乾燥した。溶媒が除去された後、約130℃に昇温し、約10分間静置して架橋反応を開始及び進行させた。その後、ロール間隔0μmでロールプレスを4回行った。
正極活物質としてLiCo2O3を使用した。前記正極活物質、VGCF、BR及びHNBRを重量比で94:2:3.96:0.04の比率でキシレンに投入し撹拌して均一な正極スラリーを得た。スラリーの撹拌中に架橋開始剤としてDCPを添加した。DCP溶液(キシレン中に40%含量)はBR及びHNBRの100重量部に対して5重量部の比率で添加された(固形分基準)。前記スラリーをアルミニウム薄膜に250μmの厚さで塗布した後、25℃で乾燥した。溶媒が除去された後、約130℃に昇温し、約10分間静置して架橋反応を開始及び進行させた。その後、ロール間隔0μmでロールプレスを4回行って正極を収得した。
DCPが添加されないことを除き、製造例1−1と同じ方法で負極を製造した。
DCPが添加されないことを除き、製造例1−2と同じ方法で正極を製造した。
製造例1−1で製造した負極とリチウム金属との間に分離膜(ポリエチレン素材分離膜、厚さ:20μm)を介在させて電極組立体を製造した後、LiPF6 1M濃度の有機溶媒(エチレンカーボネート:ジエチルカーボネート=3:7体積比)を電解液にしてコイン型ハーフセルを製造した。また、同じ電極を用いて2組の電池を製造し、それぞれ実施例1及び実施例2にした。
製造例2−1で製造した負極とリチウム金属との間に分離膜(ポリエチレン素材分離膜、厚さ:20μm)を介在させて電極組立体を製造した後、LiPF6 1M濃度の有機溶媒(エチレンカーボネート:ジエチルカーボネート=3:7体積比)を電解液にしてコイン型ハーフセルを製造した。また、同じ電極を用いて2組の電池を製造し、それぞれ比較例1及び比較例2にした。
それぞれの製造例で収得した電極を用いて電極層と集電体との界面の剥離力を確認し、その結果を下記表1に示した。剥離力の評価は引張試験機を用いた90゜剥離テストで測定した。
それぞれの電池に対し、0.1Cで0.005VまでCC−CVモード(電流が0.05Cになれば、充電を終了)で充電し、0.1Cで1.5Vまで定電流で放電して、負極に対する充放電サイクルを確認した。結果を図7に示した。図面によれば、充電初期の抵抗減少、放電容量のバラツキの減少及び電圧の安定性増加の面から、実施例の電池が比較例の電池に比べて優れることが確認された。図7を参照すれば、実施例の充電初期の電圧減少が比較例に比べてより低いことが分かるが、これは電極抵抗の減少に起因するものであって、実施例の電池が比較例の電池に比べてより低い抵抗を有するためである。また、実施例に該当する2組(実施例1及び2)の放電容量は同一に測定された一方、比較例に該当する2組(比較例1及び2)の放電容量はグラフ上で約20mAh/gの差を見せた。そして、比較例の場合、充電初期の電圧曲線が不安定である一方、実施例の場合は安定的に充電が行われている。このような現象は電極の架橋化により電極の物理的安定性が増加したためである。
2:架橋開始剤
3:固体電解質
4:電極活物質
5:非極性溶媒
10:負極
11:電極活物質層
12:集電体
100:電極組立体
20:正極
50:固体電解質層
30:負極
Claims (6)
- (S10)電極活物質、ゴム系バインダーを含むバインダー樹脂、架橋開始剤、無機固体電解質及び溶媒を含む電極層製造用スラリーを用意する段階;
(S20)前記電極層製造用スラリーを集電体の表面に塗布し乾燥して電極層aを形成する段階であって、前記溶媒を完全に除去して前記電極層aを固化させる、段階;
(S30)前記電極層aを圧延して電極層a’を形成する段階;及び
(S40)前記電極層a’を加温処理して電極層a’’を形成する段階;を含み、
前記(S20)段階は架橋反応が開始されない温度範囲で行われ、(S40)段階は電極層の架橋反応が開始及び進行する温度範囲で行われる、電極の製造方法。 - 前記(S10)段階の溶媒が非極性溶媒である、請求項1に記載の電極の製造方法。
- 前記スラリーが導電材をさらに含む、請求項1に記載の電極の製造方法。
- 前記架橋開始剤が有機過酸化物系架橋開始剤である、請求項1に記載の電極の製造方法。
- 前記有機過酸化物系架橋開始剤が、ジ(2−エチルヘキシル)ペルオキシジカーボネート、ジ(4−t−ブチルシクロヘキシル)ペルオキシジカーボネート、ジ−sec−ブチルペルオキシジカーボネート、t−ブチルペルオキシネオデカノエート、t−ヘキシルペルオキシピバレート、t−ブチルペルオキシピバレート、ジラウロイルペルオキシド、ジ−n−オクタノイルペルオキシド、1,1,3,3−テトラメチルブチルペルオキシ−2−エチルヘキサノエート、ジ(4−メチルベンゾイル)ペルオキシド、ジベンゾイルペルオキシド、t−ブチルペルオキシイソブチレート、1,1−ジ(t−ヘキシルペルオキシ)シクロヘキサンからなる群より選択された1種以上である、請求項4に記載の電極の製造方法。
- 前記(S40)段階が真空条件で行われる、請求項1に記載の電極の製造方法。
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KR20180107755A (ko) | 2018-10-02 |
US20190229328A1 (en) | 2019-07-25 |
CN110100333A (zh) | 2019-08-06 |
CN110100333B (zh) | 2022-07-22 |
WO2018174565A1 (ko) | 2018-09-27 |
EP3490039B1 (en) | 2020-08-19 |
EP3490039A4 (en) | 2019-10-30 |
US11631839B2 (en) | 2023-04-18 |
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