JP2022133456A - 高出力アプリケーション用のナノスケールポア構造のカソードおよび材料合成方法 - Google Patents
高出力アプリケーション用のナノスケールポア構造のカソードおよび材料合成方法 Download PDFInfo
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- 239000011148 porous material Substances 0.000 title description 49
- 239000000463 material Substances 0.000 title description 48
- 238000001308 synthesis method Methods 0.000 title description 5
- 239000002019 doping agent Substances 0.000 claims abstract description 112
- 239000002243 precursor Substances 0.000 claims abstract description 103
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 72
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 58
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 44
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 44
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 31
- 239000010452 phosphate Substances 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 28
- 229910000398 iron phosphate Inorganic materials 0.000 claims abstract description 26
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 24
- 239000011262 electrochemically active material Substances 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 61
- 229910017052 cobalt Inorganic materials 0.000 claims description 30
- 239000010941 cobalt Substances 0.000 claims description 30
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 30
- 239000013078 crystal Substances 0.000 claims description 18
- GLMOMDXKLRBTDY-UHFFFAOYSA-A [V+5].[V+5].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical group [V+5].[V+5].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GLMOMDXKLRBTDY-UHFFFAOYSA-A 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000012002 vanadium phosphate Substances 0.000 claims description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 7
- 238000012983 electrochemical energy storage Methods 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- -1 lithium metals Chemical class 0.000 claims description 4
- 150000001768 cations Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical group [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- ASYZRLCMYUFCHK-UHFFFAOYSA-N azane cobalt phosphoric acid Chemical compound N.[Co].OP(O)(O)=O ASYZRLCMYUFCHK-UHFFFAOYSA-N 0.000 claims 1
- 239000002355 dual-layer Substances 0.000 claims 1
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- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 70
- 239000000203 mixture Substances 0.000 description 38
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- 229910001416 lithium ion Inorganic materials 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 26
- 235000021317 phosphate Nutrition 0.000 description 25
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 23
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- 229910003206 NH4VO3 Inorganic materials 0.000 description 5
- 239000010406 cathode material Substances 0.000 description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 5
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
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- 229910001456 vanadium ion Inorganic materials 0.000 description 2
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
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- 239000004480 active ingredient Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/372—Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- 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
- H01M4/13—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
-
- 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
-
- 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
-
- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/60—Other road transportation technologies with climate change mitigation effect
- Y02T10/70—Energy storage systems for electromobility, e.g. batteries
Abstract
Description
表I 低NH3放出LFP法のドーパント製剤の例
表II 各種バナジウムドーパント前駆体濃度を有するLFPの電気化学的性能および物理的特性
V2O5+2NH4H2PO4+C→2VPO4+2NH3+3H2O+CO2
表III FePO4・qH2Oの特性;ドーパント;コドーパント(任意);リチウム源の例、LFP前駆体粉末;およびLFP最終粉末
表IV スフェニシダイトFePO4-LFPとPP FePO4-LFPとの比較例
表V 高水分及び低水分で構築されたリチウムイオン電池のガス分析
Claims (14)
- 電気化学的エネルギー貯蔵デバイスの電極に使用するためのリン酸鉄リチウム電気化学的活性材料を形成するための方法であって、
(a)スラリーを形成するために、バナジウムドーパント源と、リチウム源と、炭素源と、少なくとも28重量%の鉄含量および1.000~1.040:1のリン酸塩対鉄のモル比を有するリン酸鉄源と、任意のコドーパントと、を溶媒中で混合する工程と、
(b)前記スラリーを粉砕する工程と、
(c)リン酸鉄リチウム前駆体粉末を形成するために、前記粉砕されたスラリーを乾燥する工程と、
(d)前記リン酸鉄リチウム電気化学的活性材料を得るために、前記乾燥され、粉砕されたスラリーを燃焼する工程と、を含み、
前記リン酸鉄リチウム電気化学的活性材料は、バナジウムドーパントおよび/または結晶格子構造中のFeを部分的に置換するコドーパントと、1.000~1.050:1のリン酸塩対鉄のモル比と、1.000~1.040:1のトータル非リチウム金属対リン酸塩のモル比と、を含むことを特徴とするリン酸鉄リチウム電気化学的活性材料を形成するための方法。 - 前記リン酸鉄リチウム電気化学的活性材料は、約25m2/gより大きい表面積と、1.0~1.4g/mLの範囲内のタップ密度と、150mAh/gより大きいFCCと、140mAh/gより大きい10C放電容量と、を有する請求項1に記載の方法。
- 前記バナジウムドーパントは、酸化物、炭酸塩、シュウ酸塩、リン酸塩または前記バナジウムがカチオンとみなされる他の供給源のオキシアニオン前駆体種由来である請求項1に記載の方法。
- 前記バナジウムドーパント源は、リン酸バナジウム(VPO4)、メタバナジン酸アンモニウム(NH4VO3)、またはこれらの組合せである請求項3に記載の方法。
- 前記コドーパントは、コバルトを含む請求項1に記載の方法。
- 前記コバルトの前記コドーパントは、シュウ酸コバルト(CoC2O4)、リン酸コバルトアンモニウム(NH4CoPO4)、またはこれらの組み合わせである請求項5に記載の方法。
- アンモニア放出源は、前記バナジウムドーパント、前記コドーパント、またはそれらの組み合わせに制限される請求項1に記載の方法。
- 前記アンモニア放出源は、実質的に0である請求項7に記載の方法。
- 前記リン酸鉄源は、六方晶系構造を含む請求項1に記載の方法。
- 前記リン酸鉄リチウム前駆体粉末は、75~125℃、75~250℃、および275~425℃の3つの温度範囲内に観察可能なピークを有する示差熱重量分析損失プロファイルを含む請求項1に記載の方法。
- 前記275~425℃の温度範囲は、2つの態様のピークを含み、
前記範囲内の低温度側で記録された前記ピークは、ピーク高さを含み、
前記ピーク高さは、同じ範囲内の高温度側で記録された前記ピークのピーク高さよりも高く、
500℃を超えて実質的なピークは存在しない請求項10に記載の方法。 - 前記リン酸鉄リチウム前駆体粉末からのトータル熱質量損失は、約25℃~600℃に加熱されたとき、40%未満である請求項11に記載の方法。
- 前記バナジウムドーパントは、2~4モル%で存在し、
コバルトの前記コドーパントは、0.0~0.5モル%で存在する請求項11に記載の方法。 - 前記方法は、-20℃で20mAhの二層パウチ電池について測定されとき、9オーム未満のDCRをもたらす請求項11に記載の方法。
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