JP2007257867A - 負極および電池 - Google Patents
負極および電池 Download PDFInfo
- Publication number
- JP2007257867A JP2007257867A JP2006077073A JP2006077073A JP2007257867A JP 2007257867 A JP2007257867 A JP 2007257867A JP 2006077073 A JP2006077073 A JP 2006077073A JP 2006077073 A JP2006077073 A JP 2006077073A JP 2007257867 A JP2007257867 A JP 2007257867A
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- JP
- Japan
- Prior art keywords
- negative electrode
- active material
- material layer
- fluoride
- electrode active
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000007773 negative electrode material Substances 0.000 claims abstract description 138
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 56
- 239000002245 particle Substances 0.000 claims abstract description 27
- 239000000470 constituent Substances 0.000 claims abstract description 24
- 239000011149 active material Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 10
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 9
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 45
- 239000010703 silicon Substances 0.000 claims description 45
- 229910052710 silicon Inorganic materials 0.000 claims description 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 37
- 229910052760 oxygen Inorganic materials 0.000 claims description 37
- 239000001301 oxygen Substances 0.000 claims description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 31
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 26
- 239000011737 fluorine Substances 0.000 claims description 23
- 229910052731 fluorine Inorganic materials 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims description 19
- 239000003792 electrolyte Substances 0.000 claims description 18
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 13
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims description 11
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000010941 cobalt Substances 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 10
- 230000003746 surface roughness Effects 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 7
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 7
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 7
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 7
- 239000012808 vapor phase Substances 0.000 claims description 7
- 235000003270 potassium fluoride Nutrition 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 claims description 4
- 229910001637 strontium fluoride Inorganic materials 0.000 claims description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 4
- 239000008151 electrolyte solution Substances 0.000 abstract description 16
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- 239000010410 layer Substances 0.000 description 217
- 230000000052 comparative effect Effects 0.000 description 21
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 19
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 18
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- 239000007774 positive electrode material Substances 0.000 description 15
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 9
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- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
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- 229910001882 dioxygen Inorganic materials 0.000 description 6
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
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- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
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- 150000003377 silicon compounds Chemical class 0.000 description 2
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- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
【解決手段】負極活物質層12Bは、気相法により形成されたものであり、構成元素としてSiを含む活物質粒子を有している。活物質粒子は厚み方向に成長されており、内部にアルカリ金属またはアルカリ土類金属のフッ化物を含有している。これにより負極活物質層12Bの膨張が抑制されると共に、膨張により新たな面が露出しても、フッ化物により被膜の形成を促進し、電解液の分解などにより堆積される新たな被膜の形成を抑制することができる。
【選択図】図1
Description
図1は、本発明の第1の実施の形態に係る二次電池の構成を表すものである。この二次電池は、いわゆるコイン型といわれるものであり、外装カップ11に収容された負極12と、外装缶13に収容された正極14とが、セパレータ15を介して積層されている。セパレータ15には液状の電解質である電解液が含浸されており、外装カップ11および外装缶13の周縁部は絶縁性のガスケット16を介してかしめることにより密閉されている。外装カップ11および外装缶13は、例えば、ステンレスあるいはアルミニウム(Al)などの金属によりそれぞれ構成されている。
図4は、本発明の第2の実施の形態に係る二次電池の構成を表すものである。この二次電池は、リード21,22が取り付けられた電極巻回体20をフィルム状の外装部材30の内部に収容したものであり、小型化,軽量化および薄型化が可能となっている。
図4,5に示した構造の二次電池を作製した。まず、厚み12μmの表面を粗化した銅箔よりなる負極集電体23Aに、真空蒸着法によりケイ素とアルカリ金属のフッ化物とを共蒸着させ、厚み約5μmの負極活物質層23Bを成膜した。その際、アルカリ金属のフッ化物には、実施例1−1〜1−5ではフッ化リチウムを用い、実施例1−6〜1−8ではフッ化ナトリウムを用い、実施例1−9〜1−11ではフッ化カリウムを用いた。また、実施例1−1〜1−11でフッ化物の蒸着量を調節し、負極活物質層23Bにおけるフッ化物の含有量を変化させた。次いで、減圧雰囲気において熱処理を行った。
負極活物質層23Bを成膜する際に、アルカリ金属のフッ化物に代えて、アルカリ土類金属のフッ化物を共蒸着させたことを除き、他は実施例1−1〜1−11と同様にして二次電池を組み立てた。アルカリ土類金属のフッ化物には、実施例2−1〜2−4ではフッ化マグネシウムを用い、実施例2−5〜2−7ではフッ化カルシウムを用い、実施例2−8,2−9ではフッ化ストロンチウムを用い、実施例2−10〜2−14ではフッ化バリウムを用いた。また、実施例2−1〜2−14でフッ化物の蒸着量を調節し、負極活物質層23Bにおけるフッ化物の含有量を変化させた。
負極活物質層23Bを成膜する際に、フッ化物を共蒸着せずに、ケイ素の層とフッ化物の層とを交互に積層したことを除き、他は実施例1−1〜1−11と同様にして二次電池を組み立てた。実施例3−1〜3−3ではフッ化物にフッ化リチウムを用い、フッ化物層はスパッタリング法により成膜した。実施例3−4〜3−6ではフッ化物にフッ化バリウムを用い、フッ化物層は真空蒸着法により成膜した。なお、ケイ素の層はいずれも真空蒸着法により成膜した。
負極集電体23Aの表面粗度Ra値を0.1μm〜0.5μmの範囲内で変化させたことを除き、他は実施例1−2または実施例2−6と同様にして二次電池を組み立てた。実施例4−1〜4−5ではフッ化物にフッ化リチウムを用い、実施例4−6〜4−10ではフッ化カルシウムを用いた。作製した実施例4−1〜4−10の負極23についても、実施例1−2,2−6と同様にしてフッ化物の含有量を調べたところ、実施例4−1〜4−5はリチウムとフッ素との合計の存在比率が約6.5原子数%であり、実施例4−6〜4−10はカルシウムとフッ素との合計の存在比率が約15.3原子数%であった。
負極活物質層23Bを成膜する際に、ケイ素とフッ化物とを共蒸着した第1層と、酸化ケイ素の第2層とを交互に積層し、たことを除き、他は実施例1−2または実施例2−6と同様にして二次電池を組み立てた。第2層は、実施例5−1〜5−6では真空蒸着法により成膜し、実施例6−1〜6−6では酸素ガスを導入して第1層の表面を酸化させることにより成膜した。また、実施例5−1〜5−3,6−1〜6−3ではフッ化物にフッ化リチウムを用い、実施例5−4〜5−6,6−4〜6−6ではフッ化物にフッ化カルシウムを用いた。
負極活物質層23Bを成膜する際に酸素ガスを連続して導入し、酸素を添加したことを除き、他は実施例1−2または実施例2−6と同様にして二次電池を組み立てた。その際、酸素ガスの導入量を調節し、酸素の含有量を変化させた。なお、実施例7−1〜7−10ではフッ化物にフッ化リチウムを用い、実施例7−11〜7−20ではフッ化物にフッ化カルシウムを用いた。作製した実施例7−1〜7−20の負極23についても、実施例1−2,2−6と同様にしてフッ化物の含有量および酸素の含有量を調べた。その結果、実施例7−1〜7−10はリチウムとフッ素との合計の存在比率が約6.5原子数%であり、実施例7−11〜7−20はカルシウムとフッ素との合計の存在比率が約15.3原子数%であった。また、酸素の含有量は表8に示した通りであった。
負極活物質層23Bを成膜する際に酸素ガスを導入して酸素を添加すると共に、鉄,ニッケル,チタンまたはコバルトを共蒸着したことを除き、他は実施例1−2と同様にして二次電池を組み立てた。その際、フッ化物にはフッ化リチウムを用い、酸素ガスの導入量は実施例8−1〜8−12で一定とした。また、金属元素は、実施例8−1〜8−9が鉄、実施例8−10がニッケル、実施例8−11がチタン、実施例8−12がコバルトとし、実施例8−1〜8−9で金属元素の蒸着量を変化させた。作製した実施例8−1〜8−12の負極23についても、実施例1−2と同様にしてフッ化物、酸素および金属元素の含有量を調べた。その結果、リチウムとフッ素との合計の存在比率はいずれも約6.5原子数%であり、酸素の含有量はいずれも約5原子数%であった。また、金属元素の含有量は表9に示した通りであった。
Claims (24)
- 負極集電体と、構成元素としてケイ素(Si)を含む負極活物質層とを備えた負極であって、
前記負極活物質層は、内部に、アルカリ金属のフッ化物およびアルカリ土類金属のフッ化物からなる群のうちの少なくとも1種を含有する
ことを特徴とする負極。 - 前記フッ化物は、フッ化リチウム、フッ化ナトリウム、フッ化カリウム、フッ化マグネシウム、フッ化カルシウム、フッ化ストロンチウム、およびフッ化バリウムからなる群のうちの少なくとも1種を含む
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層におけるアルカリ金属のフッ化物の含有量は、アルカリ金属とフッ素との合計の存在比率で、1原子数%以上40原子数%以下の範囲内である
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層におけるアルカリ土類金属のフッ化物の含有量は、アルカリ土類金属とフッ素との合計の存在比率で、0.5原子数%以上30原子数%以下の範囲内である
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層は、構成元素としてケイ素を含む活物質粒子を有し、
この活物質粒子の少なくとも一部は、粒子中に前記フッ化物を含む
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層の少なくとも一部は、気相法により形成されたことを特徴とする請求項1記載の負極。
- 前記負極活物質層は、前記負極集電体と少なくとも一部において合金化している
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層は、更に構成元素として酸素(O)を含有し、その含有量は3原子数%以上40原子数%以下である
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層は、構成元素として酸素を含有し、酸素の含有量が異なる第1層と第2層とを交互に積層して有し、
前記第2層は前記第1層よりも酸素の含有量が多く、かつ、少なくとも前記第1層の間に1層以上存在する
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層は、更に構成元素として鉄(Fe)、コバルト(Co)、ニッケル(Ni)およびチタン(Ti)からなる群のうちの少なくとも1種の金属元素を含有する
ことを特徴とする請求項1記載の負極。 - 前記負極活物質層における前記金属元素の含有量は、0.5原子数%以上30原子数%以下である
ことを特徴とする請求項10記載の負極。 - 前記負極集電体の表面粗度は、Ra値で0.1μm以上であることを特徴とする請求項1記載の負極。
- 正極および負極と共に電解質を備えた電池であって、
前記負極は、負極集電体と、構成元素としてケイ素(Si)を含む負極活物質層とを有し、
前記負極活物質層は、内部に、アルカリ金属のフッ化物およびアルカリ土類金属のフッ化物からなる群のうちの少なくとも1種を含有する
ことを特徴とする電池。 - 前記フッ化物は、フッ化リチウム、フッ化ナトリウム、フッ化カリウム、フッ化マグネシウム、フッ化カルシウム、フッ化ストロンチウム、およびフッ化バリウムからなる群のうちの少なくとも1種を含む
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層におけるアルカリ金属のフッ化物の含有量は、アルカリ金属とフッ素との合計の存在比率で、1原子数%以上40原子数%以下の範囲内である
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層におけるアルカリ土類金属のフッ化物の含有量は、アルカリ土類金属とフッ素との合計の存在比率で、0.5原子数%以上30原子数%以下の範囲内である
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層は、構成元素としてケイ素を含む活物質粒子を有し、
この活物質粒子の少なくとも一部は、粒子中に前記フッ化物を含む
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層の少なくとも一部は、気相法により形成されたことを特徴とする請求項13記載の電池。
- 前記負極活物質層は、前記負極集電体と少なくとも一部において合金化している
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層は、更に構成元素として酸素(O)を含有し、その含有量は3原子数%以上40原子数%以下である
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層は、構成元素として酸素を含有し、酸素の含有量が異なる第1層と第2層とを交互に積層して有し、
前記第2層は前記第1層よりも酸素の含有量が多く、かつ、少なくとも前記第1層の間に1層以上存在する
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層は、更に構成元素として鉄(Fe)、コバルト(Co)、ニッケル(Ni)およびチタン(Ti)からなる群のうちの少なくとも1種の金属元素を含有する
ことを特徴とする請求項13記載の電池。 - 前記負極活物質層における前記金属元素の含有量は、0.5原子数%以上30原子数%以下である
ことを特徴とする請求項22記載の電池。 - 前記負極集電体の表面粗度は、Ra値で0.1μm以上であることを特徴とする請求項13記載の電池。
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KR20070095218A (ko) | 2007-09-28 |
US20150349340A1 (en) | 2015-12-03 |
KR101384429B1 (ko) | 2014-04-10 |
CN102931376A (zh) | 2013-02-13 |
CN102931376B (zh) | 2018-07-10 |
US9806371B2 (en) | 2017-10-31 |
CN101060170B (zh) | 2015-01-14 |
US20080113270A1 (en) | 2008-05-15 |
US9112238B2 (en) | 2015-08-18 |
JP4655976B2 (ja) | 2011-03-23 |
CN101060170A (zh) | 2007-10-24 |
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