JP2018526799A - 接着力が改善されたリチウム二次電池用電極およびその製造方法 - Google Patents
接着力が改善されたリチウム二次電池用電極およびその製造方法 Download PDFInfo
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- JP2018526799A JP2018526799A JP2018512906A JP2018512906A JP2018526799A JP 2018526799 A JP2018526799 A JP 2018526799A JP 2018512906 A JP2018512906 A JP 2018512906A JP 2018512906 A JP2018512906 A JP 2018512906A JP 2018526799 A JP2018526799 A JP 2018526799A
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- BLBBMBKUUHYSMI-UHFFFAOYSA-N furan-2,3,4,5-tetrol Chemical compound OC=1OC(O)=C(O)C=1O BLBBMBKUUHYSMI-UHFFFAOYSA-N 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N germanium monoxide Inorganic materials [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 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
- 229940017219 methyl propionate Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 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
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 235000015041 whisky Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- 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
- H01M4/622—Binders being polymers
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- H01M10/052—Li-accumulators
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- H01M10/052—Li-accumulators
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- H01M4/04—Processes of manufacture in general
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- H01M4/0435—Rolling or calendering
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/04—Processes of manufacture in general
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Abstract
Description
外部導線と電極活物質との間で電子を伝達する集電体と、前記集電体上に塗布された電極合剤層とを含む二次電池用電極であって、
前記電極合剤層は、架橋高分子、電極活物質、およびバインダーを含んでおり、
前記架橋高分子は、第1重合単位体と第2重合単位体との架橋結合によって形成されて相互侵入型ポリマーネットワーク構造(interpenetrating polymer network、IPN)を有することを特徴とする。
(i)第1重合単位体、第2重合単位体、光開始剤、電極活物質、およびバインダーを溶媒に入れて混合して電極スラリーを製造する過程;
(ii)前記電極スラリーを集電体に塗布する過程;
(iii)前記電極スラリーに紫外線(UV)処理して相互侵入型ポリマーネットワーク構造(IPN)を形成する過程;および
(iv)乾燥および圧延する過程;を含むことができる。
(i)第1重合単位体、第2重合単位体、熱開始剤、電極活物質、およびバインダーを溶媒に入れて混合して電極スラリーを製造する過程;
(ii)前記電極スラリーを集電体に塗布する過程;
(iii)前記電極スラリーに熱処理して相互侵入型ポリマーネットワーク構造(IPN)を形成する過程;および
(iv)乾燥および圧延する過程;を含むことができる。
1.負極の製造
ビスフェノールA(Bisphenol A)系アクリルウレタン(重量平均分子量Mw:1000)、ポリジメチルシロキサン系ビニルエーテルウレタン(重量平均分子量Mw:3000)、および光開始剤(benzophenone)を重量基準で94.9:5:0.1で混合し、前記混合物:人造黒鉛:カーボンブラック(Carbon black):SBRの量が重量基準で4:93.5:1:1.5となるように計量した後、水に入れて混合(mixing)して負極合剤層製造用負極混合物スラリーを製造した後、銅箔上に108μmの厚さにコーティングし、波長250〜400nmの紫外線を240秒間照射した後、乾燥および圧延して負極を製造した。
Li(Ni1/3Mn1/3Co1/3)O2、カーボンブラック(Carbon black):PVdFの量が重量基準で96:1.5:2.5となるように計量した後、NMPに入れて混合(mixing)して正極合剤層製造用正極混合物スラリーを製造した後、アルミニウム箔上に80μmの厚さにコーティングし、乾燥および圧延して正極を製造した。
前記実施例1において、負極のスラリーを製造する時、混合物:人造黒鉛:カーボンブラック(Carbon black):SBRの量を2:95:1:2にしたことを除いて、実施例1と同様の方法で負極および正極を製造した。
水に溶解したカルボキシメチルセルロース(重量平均分子量(Mw)=90,000)および水に溶解したポリアクリル酸(重量平均分子量(Mw)=100,000)を均一に混合(カルボキシメチルセルロース:ポリアクリル酸の混合モル比=73.5:26.5)し、前記混合物:人造黒鉛:カーボンブラック(Carbon black):SBRの量が4:93.5:1:1.5となるように計量した後、NMPに入れて混合(mixing)して負極合剤層製造用負極混合物スラリーを製造した後、銅箔上に100μmの厚さにコーティングし、90℃で一次熱処理、真空下、200℃で二次熱処理を進行させた後、圧延して負極を製造し、正極は実施例1と同様に製造した。
前記実施例3において、負極のスラリーを製造する時、混合物:人造黒鉛:カーボンブラック(Carbon black):SBRの量を2:95:1:2にしたことを除いて、実施例3と同様の方法で負極および正極を製造した。
前記実施例1において、人造黒鉛、カーボンブラック(Carbon black):CMC:SBRの量が95:1:1:3となるように計量した後、水に入れて混合(mixing)して負極合剤層製造用負極混合物スラリーを製造した後、銅箔上に100μmの厚さにコーティングし、乾燥および圧延して負極を製造したことを除けば、実施例1と同様に負極を製造し、正極は実施例1と同様に製造した。
本発明による電極の接着力を評価するために、下記のような実験を実施した。
実施例1〜4と比較例1で製造された正極と負極との間に、分離膜としてポリエチレン膜(Celgard、厚さ:20μm)を介在させ、EC、DMC、EMC混合溶液に1MのLiPF6を溶かした電解液を用いて電池セルを製造し、これについて寿命特性を評価した。前記寿命特性評価は、4.2V〜2.5Vの間で1/3C⇔1/3C(1回充放電)の条件で実施した。寿命特性は、放電容量維持率から評価し、前記放電容量維持率は、充放電を200回繰り返し実施した後の容量を、初期容量に対する%比率で表した。その結果を表2に示した。
Claims (27)
- 外部導線と電極活物質との間で電子を伝達する集電体と、前記集電体上に塗布された電極合剤層とを含む二次電池用電極であって、
前記電極合剤層は、架橋高分子、電極活物質、およびバインダーを含んでおり、
前記架橋高分子は、第1重合単位体と第2重合単位体との架橋結合によって形成されて相互侵入型ポリマーネットワーク構造(interpenetrating polymer network、IPN)を有することを特徴とする二次電池用電極。 - 前記第1重合単位体と第2重合単位体は、互いに独立にモノマー、オリゴマー、またはポリマーであることを特徴とする請求項1に記載の二次電池用電極。
- 前記モノマーは、アクリレート系モノマー、ヒドロキシ基含有モノマー、アミン系モノマー、ビニル基を有する線状ニトリル系化合物由来のモノマー、およびカルボン酸系モノマーからなる群より選択される1種以上であることを特徴とする請求項2に記載の二次電池用電極。
- 前記オリゴマーは、ウレタン系オリゴマーであることを特徴とする請求項2に記載の二次電池用電極。
- 前記ポリマーは、ポリビニルアルコールおよびポリウレタンからなる群より選択される1種以上であることを特徴とする請求項2に記載の二次電池用電極。
- 前記第1重合単位体と第2重合単位体は、互いに異なるウレタン系オリゴマーまたはポリマーであることを特徴とする請求項2に記載の二次電池用電極。
- 前記第1重合単位体は、アクリルウレタン系オリゴマーまたはポリマーであり、第2重合単位体は、ビニルエーテルウレタン系オリゴマーまたはポリマーであることを特徴とする請求項6に記載の二次電池用電極。
- 前記アクリルウレタン系オリゴマーまたはポリマーは、ビスフェノールA(Bisphenol A)系アクリルウレタン、または6FビスフェノールA(Bisphenol A)系アクリルウレタンであることを特徴とする請求項7に記載の二次電池用電極。
- 前記アクリルウレタン系オリゴマーまたはポリマーは、重量平均分子量が100〜500,000であることを特徴とする請求項7に記載の二次電池用電極。
- 前記ビニルエーテルウレタン系オリゴマーまたはポリマーは、シロキサン系ビニルエーテルウレタンであることを特徴とする請求項7に記載の二次電池用電極。
- 前記シロキサン系ビニルエーテルウレタンは、ポリジメチルシロキサン系ビニルエーテルウレタンであることを特徴とする請求項10に記載の二次電池用電極。
- 前記ビニルエーテルウレタン系オリゴマーまたはポリマーは、重量平均分子量が100〜500,000であることを特徴とする請求項7に記載の二次電池用電極。
- 前記第1重合単位体および第2重合単位体は、5:95〜95:5の重量比で架橋反応してIPN構造を形成することを特徴とする請求項7に記載の二次電池用電極。
- 前記架橋高分子は、イオン伝導が可能な特性を有することを特徴とする請求項1に記載の二次電池用電極。
- 前記架橋高分子のイオン伝導度は、10−6S/cm〜10−2S/cmであることを特徴とする請求項14に記載の二次電池用電極。
- 前記架橋高分子は、水または非水系電解液に対して5%以下の耐溶剤性を示すことを特徴とする請求項1に記載の二次電池用電極。
- 前記架橋高分子は、電極合剤層の全体重量を基準として0.1重量%〜30重量%含まれていることを特徴とする請求項1に記載の二次電池用電極。
- 二次電池用電極を製造する方法であって、
(i)第1重合単位体、第2重合単位体、光開始剤、電極活物質、およびバインダーを溶媒に入れて混合して電極スラリーを製造する過程;
(ii)前記電極スラリーを集電体に塗布する過程;
(iii)前記電極スラリーに紫外線(UV)処理して相互侵入型ポリマーネットワーク構造(IPN)を形成する過程;および
(iv)乾燥および圧延する過程;を含むことを特徴とする二次電池用電極の製造方法。 - 前記光開始剤は、ベンゾインエーテル系、ベンゾフェノン系、アセトフェノン系、およびチオキサントン系光開始剤からなる群より選択される1種以上であることを特徴とする請求項18に記載の二次電池用電極の製造方法。
- 前記紫外線処理は、50秒〜300秒間紫外線照射によって行われることを特徴とする請求項18に記載の二次電池用電極の製造方法。
- 二次電池用電極を製造する方法であって、
(i)第1重合単位体、第2重合単位体、熱開始剤、電極活物質、およびバインダーを溶媒に入れて混合して電極スラリーを製造する過程;
(ii)前記電極スラリーを集電体に塗布する過程;
(iii)前記電極スラリーに熱処理して相互侵入型ポリマーネットワーク構造(IPN)を形成する過程;および
(iv)乾燥および圧延する過程;を含むことを特徴とする二次電池用電極の製造方法。 - 前記熱開始剤は、アゾ系化合物、およびパーオキサイド系化合物からなる群より選択される1種以上であることを特徴とする請求項21に記載の二次電池用電極の製造方法。
- 前記相互侵入型ポリマーネットワーク構造(IPN)を形成する熱処理と乾燥は、同じ過程で一緒に行われることを特徴とする請求項21に記載の二次電池用電極の製造方法。
- 請求項1〜17のいずれか1項に記載の二次電池用電極を含むことを特徴とするリチウム二次電池。
- 請求項24に記載のリチウム二次電池を単位電池として含むことを特徴とする電池モジュール。
- 請求項25に記載の電池モジュールを含むことを特徴とする電池パック。
- 請求項26に記載の電池パックを電源として用いることを特徴とするデバイス。
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