JP5694162B2 - ゲルポリマー電解質二次電池の製造方法 - Google Patents
ゲルポリマー電解質二次電池の製造方法 Download PDFInfo
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- JP5694162B2 JP5694162B2 JP2011522009A JP2011522009A JP5694162B2 JP 5694162 B2 JP5694162 B2 JP 5694162B2 JP 2011522009 A JP2011522009 A JP 2011522009A JP 2011522009 A JP2011522009 A JP 2011522009A JP 5694162 B2 JP5694162 B2 JP 5694162B2
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- polymer electrolyte
- gel polymer
- secondary battery
- monomer
- battery
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- 238000004519 manufacturing process Methods 0.000 title claims description 37
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- 239000002904 solvent Substances 0.000 claims description 30
- 239000003792 electrolyte Substances 0.000 claims description 26
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- 150000003839 salts Chemical class 0.000 claims description 21
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- 238000000034 method Methods 0.000 claims description 14
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- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
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- 230000000379 polymerizing effect Effects 0.000 claims 1
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- 210000001787 dendrite Anatomy 0.000 description 1
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- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 229940093499 ethyl acetate Drugs 0.000 description 1
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- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical compound C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical group 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical class [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 229920005735 poly(methyl vinyl ketone) Polymers 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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Description
<重合開始剤がコートされたセパレータの製造>
重合開始剤としてt‐ブチルペルオキシ‐2‐エチルヘキサノエート0.00825gをアセトンに溶かした後、この溶液をポリオレフィン系の不織布セパレータに均一にコートした後乾燥させることで、重合開始剤がコートされたセパレータを製造した。
エチレンカーボネート(EC):エチルメチルカーボネート(EMC)=1:2(v:v)の組成を有する非水電解液溶媒にLiPF6を1M濃度になるように溶解した後、前記電解液溶液100重量部に対してポリマー電解質モノマーとしてトリメチロールプロパントリアクリレート5重量部を添加してゲルポリマー電解質用組成物3.30gを製造した。
カソード活物質としてLiCoO294重量%、導電材としてカーボンブラック(carbon black)3重量%、バインダーとしてPVdF3重量%を溶媒であるN‐メチル‐2‐ピロリドン(NMP)に添加してカソード混合物スラリーを製造した。前記カソード混合物スラリーを厚さが20μm程度のカソード集電体であるアルミニウム(Al)薄膜に塗布し乾燥した後、ロールプレス(roll press)してカソードを製造した。
ポリマー電解質モノマーとしてトリメチロールプロパントリアクリレートの代わりにジペンタエリスリトールペンタアクリレートを用いたことを除いては、実施例1と同一の方法で二次電池を製造した。
重合開始剤としてt‐ブチルペルオキシ‐2‐エチルヘキサノエートを0.00825gの代わりに0.0165g使用し、ポリマー電解質モノマーとしてトリメチロールプロパントリアクリレートを5重量部の代わりに8重量部使用し、ゲルポリマー電解質用組成物を注入して3時間経過した後、窒素雰囲気の下で80℃で4時間重合させたことを除いては、実施例1と同一の方法で二次電池を製造した。
アノード活物質として炭素粉末、バインダーとしてPVdF、導電材としてカーボンブラック、重合開始剤としてt‐アミル-(2‐エチルヘキシル)モノペルオキシカーボネートをそれぞれ95重量%、3重量%、1重量%、及び1重量%にして溶媒であるNMPに添加してアノード混合物スラリーを製造した。前記アノード混合物スラリーを厚さが10μmのアノード集電体である銅薄膜に塗布し乾燥した後、ロールプレスしてアノードを製造した。乾燥工程においては、可能な限り低い温度と高い圧力を使用して行うことが望ましい。
エチレンカーボネート(EC):ジメチルカーボネート(DMC):ジエチルカーボネート(DEC)=4:3:3の組成を有する非水電解液溶媒にLiPF6を1M濃度になるように溶解した後、前記溶液100重量部に対してビニレンカーボネート1.5重量部及び1,3‐プロパンスルトン(1,3‐propane sultone)0.5重量部を添加して電解液3.30gを製造した。
エチレンカーボネート(EC):プロピレンカーボネート(PC):ジエチルカーボネート(DEC)=3:2:5 の組成を有する非水電解液溶媒にLiPF6を1M濃度になるように溶解して電解液溶液3.30gを製造した。
エチレンカーボネート(EC):エチルメチルカーボネート(EMC)=1:2(v:v)の組成を有する非水電解液溶媒にLiPF6を1M濃度になるように溶解した後、前記電解液溶液100重量部に対してポリマー電解質モノマーとしてトリメチロールプロパントリアクリレート5重量部、及び重合開始剤としてt‐ブチルペルオキシ‐2‐エチルヘキサノエート0.25重量部を添加してゲルポリマー電解質用組成物3.30gを製造した。
エチレンカーボネート(EC):エチルメチルカーボネート(EMC)=1:2(v:v)の組成を有する非水電解液溶媒にLiPF6を1M濃度になるように溶解した後、前記電解液溶液100重量部に対してポリマー電解質モノマーとしてトリメチロールプロパントリアクリレート5重量部、及び重合開始剤としてt‐ブチルペルオキシ‐2‐エチルヘキサノエート0.25重量部を添加してゲルポリマー電解質用組成物3.30gを製造した。
ポリマー電解質モノマーとしてトリメチロールプロパントリアクリレート0.165gをアセトンに溶かした後、この溶液をポリオレフィン系不織布セパレータに均一にコートした後乾燥させることでセパレータを製造した。
1.ゲル化テスト
実施例1で製造されたセパレータ及びゲルポリマー電解質用組成物を使用してゲル化テストをした。具体的には、前記ゲルポリマー電解質用組成物に前記セパレータを入れ、時間によるゲル化程度を下記数学式1に従って算出し、その結果を下記表1に記載した。
実施例1ないし実施例3及び比較例1ないし比較例5で製造された二次電池をそれぞれ常温で0.2Cで充放電した。放電容量と容量保持率とを下記表2に示した。下記表2において、容量は50サイクル後の放電容量を示し、容量保持率は50サイクル後に測定した容量の初期放電容量に対する%値を示す。
Claims (9)
- ゲルポリマー電解質二次電池の製造方法であって、
前記二次電池が、カソードと、アノードと、セパレータと、及びゲルポリマー電解質とを電池ケース内に包含してなるものであり、
(S1)ゲルポリマー電解質と接触する必要がある、前記カソード、アノード、及び電池ケースからなる群より選択される何れか一つ以上の一面に重合開始剤をコートする段階と、
(S2)前記カソード、アノード、及び不織布で形成されたセパレータを備えた電極アッセンブリーを電池ケースに入れる段階と、及び
(S3)電解液溶媒、電解質塩、及びポリマー電解質モノマーを含むゲルポリマー電解質用組成物を前記電池ケースに注入し、前記モノマーを重合させてゲルポリマー電解質を形成する段階を含んでなる、ゲルポリマー電解質二次電池の製造方法。 - 前記不織布で形成されたセパレータが、ポリエチレンまたはポリプロピレンから製造される、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記重合開始剤が、ベンゾイルペルオキシド、アセチルペルオキシド、ジラウリルペルオキシド、ジ‐tert‐ブチルペルオキシド、t‐ブチルペルオキシ‐2‐エチルヘキサノエート、クミルヒドロペルオキシド、t‐アミル‐(2‐エチルヘキシル)モノペルオキシカーボネート、過酸化水素、2,2´‐アゾビス(2‐シアノブタン)、2,2´‐アゾビス(メチルブチロニトリル)、AIBN、及びAMVNからなる群より選択された何れか一種または二種以上の混合物である、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記ポリマー電解質モノマーが、ビニル基、エポキシ基、アリル基、及び(メタ)アクリル基からなる群より選択される重合性官能基を有するモノマーである、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記電解液溶媒が、環状カーボネート、線状カーボネート、ラクトン、エーテル、エステル、スルホキシド、アセトニトリル、ラクタム、ケトン、及びこれらのハロゲン誘導体からなる群より選択される何れか一種または二種以上の混合物である、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記電解質塩が、
(i)Li+、Na+、及びK+からなる群より選択された陽イオンと、及び
(ii)PF6 -、BF4 -、Cl-、Br-、I-、ClO4 -、AsF6 -、CH3CO2 -、CF3SO3 -、N(CF3SO2)2 -、及びC(CF2SO2)3 -からなる群より選択された陰イオンとの組み合わせたものである、請求項1に記載のゲルポリマー電解質二次電池の製造方法。 - 前記モノマーの含量が、前記電解液溶媒と電解質塩との混合物100重量部に対して0.01〜10重量部である、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記重合開始剤の含量が、前記電解液溶媒と電解質塩との混合物100重量部に対して0.01〜5重量部である、請求項1に記載のゲルポリマー電解質二次電池の製造方法。
- 前記重合段階において、熱処理または光照射工程をさらに行うものである、請求項1〜8の何れか一項に記載のゲルポリマー電解質二次電池の製造方法。
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