JP5474991B2 - 電極の効率及びエネルギー密度を改良するカソード活性材料 - Google Patents
電極の効率及びエネルギー密度を改良するカソード活性材料 Download PDFInfo
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- JP5474991B2 JP5474991B2 JP2011533110A JP2011533110A JP5474991B2 JP 5474991 B2 JP5474991 B2 JP 5474991B2 JP 2011533110 A JP2011533110 A JP 2011533110A JP 2011533110 A JP2011533110 A JP 2011533110A JP 5474991 B2 JP5474991 B2 JP 5474991B2
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- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 239000006232 furnace black Substances 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
- 229910021469 graphitizable carbon Inorganic materials 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
- 239000011261 inert gas Substances 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate 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
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000131 polyvinylidene 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
- 238000001556 precipitation Methods 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
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000000346 sugar 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
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 238000012360 testing method Methods 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
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
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
- H01M4/36—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
-
- 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
- H01M4/36—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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
-
- 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
- H01M4/62—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
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/50—Methods or arrangements for servicing or maintenance, e.g. for maintaining operating temperature
- H01M2006/5094—Aspects relating to capacity ratio of electrolyte/electrodes or anode/cathode
-
- 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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
Description
LiFe(P(1−x)O4) (I)
により表され、リン(P)のモル画分(1−x)が0.910〜0.999の範囲内にある組成のもの(組成物)を有するカソード活性材料を提供することにより、達成される。
(a)第一に、原料をアルカリ性付与剤(alkalinizing agent)と混合し、遷移金属水酸化物を調製すること、
(b)第二に、超臨界または臨界未満水を、工程(a)で得た混合物と混合し、リチウム金属複合酸化物を合成し、これを乾燥させること、及び
(c) リチウム金属複合酸化物をか焼すること
により行う。
LiFePO4の製造方法として良く知られている水熱製法により、リン(P)の含有量が0.94(製造例1)、0.96(製造例2)、0.97(製造例3)及び0.985(製造例4)であるカソード活性材料(LiFeP1−xO4)を下記の方法に従って製造した。より詳細な説明を以下に記載する。
カソード活性材料として、製造例1で調製したLiFeP0.94O490重量%、導電性材料としてSuper-P 5重量%及び結合剤としてPVdF 5重量%を、N-メチル-2-ピロリドン(NMP)に加え、カソード混合物スラリーを調製した。このカソード混合物スラリーをアルミニウムホイルの一表面に塗布し、続いて乾燥させ、プレス加工してカソードを製造した。
カソード活性材料として、製造例2で調製したLiFeP0.96O4を使用した以外は、例1と同じ様式でバッテリーを製造した。
カソード活性材料として、製造例3で調製したLiFeP0.97O4を使用した以外は、例1と同じ様式でバッテリーを製造した。
カソード活性材料として、製造例4で調製したLiFeP0.985O4を使用した以外は、例1と同じ様式でバッテリーを製造した。
カソード活性材料として、LiFePO4を使用した以外は、例1と同じ様式でバッテリーを製造した。
例1及び比較例1で製造したバッテリーに対して操作効率を測定し、得られた結果を下記の表1に示す。
製造例4で得たカソード活性材料をXRDにかけ、例4及び比較例1で製造したバッテリーをND(中性子)精製検定、HRTEM構造的分析、及びMossbauer効果を使用するFe原子価分析にかけた。得られた結果を図1〜3に示す。
一次粒子を製造例1で調製し、スクロースと共に水に加え、続いて攪拌して混合物を調製し、この混合物を凝集させ、回転噴霧乾燥により乾燥させ、気孔率28%の二次粒子を調製した。この二次粒子を、噴霧乾燥機を使用して120℃で乾燥させ、窒素雰囲気下、700℃で10時間か焼した。
製造例で調製したカソード活性材料10gを蒸留水100ml中で5分間攪拌し、続いて濾過した。次いで、得られた濾液に0.1M HCl溶液を加え、混合物を攪拌しながらpH滴定にかけ、pHを時間の関数として記録した。この実験は、pHが3以下に達するまで行い、滴定が約20〜30分間で行われるように、流量を適切に決定した。水溶性塩基の含有量は、pHが5以下に達するまで、使用した酸の量に基づいて計算し、水溶性塩基は、pHプロファイルにより試験した。
Claims (22)
- 下記の式(I)により表される組成のものを有するカソード活性材料。
LiFe(P(1−x)O4) (I)
[上記式中、リン(P)のモル画分(1−x)が0.910〜0.999の範囲内にある。] - 前記リン(P)のモル画分(1−x)が0.955〜0.995の範囲内にある、請求項1に記載のカソード活性材料。
- 式(I)中のFeが、Al、Mg、Ni、Co、Mn、Ti、Ga、Cu、V、Nb、Zr、Ce、In、Zn及びYからなる群から選択された少なくとも一種で部分的に置き換えられてなる、請求項1に記載のカソード活性材料。
- 前記カソード活性材料が、二次粒子から構成されてなり、
前記二次粒子が、平均粒子径(D50)5〜100μmであり、かつ、平均粒子径(D50)50〜550nmである一次粒子の凝集により形成されてなるものであり、
前記一次粒子及び二次粒子が、式(I)により表される組成のものをそれぞれ有し、前記二次粒子の気孔率が10%以上である、請求項1に記載のカソード活性材料。 - 前記気孔率が15〜40%である、請求項4に記載のカソード活性材料。
- 前記一次粒子が物理的結合により凝集し、前記二次粒子を形成してなる、請求項4に記載のカソード活性材料。
- 前記二次粒子中に存在する細孔のサイズが10〜1,000nmである、請求項4に記載のカソード活性材料。
- 前記一次粒子の平均粒子径(D50)が100〜300nmであり、
前記二次粒子の平均粒子径(D50)が5〜40μmである、請求項4に記載のカソード活性材料。 - 前記二次粒子が球形状を有する、請求項4に記載のカソード活性材料。
- 前記二次粒子の比表面積(BET)が5〜15m2/gである、請求項4に記載のカソード活性材料。
- 前記カソード活性材料の嵩密度が0.5〜1.5g/mLである、請求項4に記載のカソード活性材料。
- 前記カソード活性材料の嵩密度が0.8〜1.3g/mLである、請求項11に記載のカソード活性材料。
- 前記カソード活性材料が、0.02〜5重量%のLi3PO4を含んでなり、
Li2CO3を含まず、又は0.25%未満の量でLi2CO3を含んでなる、請求項1に記載のカソード活性材料。 - 前記Li3PO4が、0.1〜5重量%の量で存在する、請求項13に記載のカソード活性材料。
- 前記Li2CO3が、0.1重量%以下の量で存在する、請求項13に記載のカソード活性材料。
- 前記カソード活性材料のpHが8.5〜11.5である、請求項13に記載のカソード活性材料。
- 前記カソード活性材料のpHが10.0〜11.5である、請求項13に記載のカソード活性材料。
- 前記Li2CO3及びLi3PO4の大部分が、前記粒子の表面上に存在する、請求項13に記載のカソード活性材料。
- 前記カソード活性材料が超臨界水熱方法により製造されてなる、請求項1に記載のカソード活性材料。
- 請求項1〜19のいずれか一項に記載のカソード活性材料を含んでなる、カソード混合物。
- 請求項20に記載のカソード混合物が集電体上に塗布されている、二次バッテリー用カソード。
- 請求項21に記載のカソードを備えてなる、リチウム二次バッテリー。
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