WO2015023017A1 - 이차전지용 양극 활물질 - Google Patents
이차전지용 양극 활물질 Download PDFInfo
- Publication number
- WO2015023017A1 WO2015023017A1 PCT/KR2013/007398 KR2013007398W WO2015023017A1 WO 2015023017 A1 WO2015023017 A1 WO 2015023017A1 KR 2013007398 W KR2013007398 W KR 2013007398W WO 2015023017 A1 WO2015023017 A1 WO 2015023017A1
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- WO
- WIPO (PCT)
- Prior art keywords
- active material
- sodium
- secondary battery
- transition metal
- positive electrode
- Prior art date
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
-
- 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
- C01B25/38—Condensed phosphates
- C01B25/42—Pyrophosphates
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
Definitions
- the present invention relates to a positive electrode active material for a secondary battery, and to a positive electrode active material for a secondary battery capable of inserting / removing ions very quickly in detail.
- An phosphate-based material of an olivine structure such as LiFeP0 4 of a lithium ion battery is a material having excellent stability due to strong P-0 bonds.
- the object of the present invention is to provide a secondary battery positive electrode active material having excellent structural stability and reversible insertion and desorption of silver.
- the present invention provides a positive electrode active material for a secondary battery, the secondary battery according to the present invention
- the positive electrode active material contains sodium transition metal pyrophosphate satisfying the following formula (1).
- the sodium transition metal pyrophosphate may be a triclinic phase.
- the sodium transition metal pyrophosphate may be a P-1 space group.
- Ml and M2 of sodium transition metal pyrophosphate are independently of each other, Co, Ni, Fe, Mn, V, Cu, Ti, Al, Cr, It may be one or more selected elements from Mo and Nb.
- a of the sodium transition metal pyrophosphate may be one or more selected elements from Li, Mg, and Ca.
- the sodium transition metal pyrophosphate may contain at least iron (Fe), manganese (Mn), or iron and manganese.
- the positive electrode active material for a secondary battery according to an embodiment of the present invention may have a capacity of 80 mAh / g or more under layer discharge conditions of 1.7 V / 4.0 V and 0.05 C.
- the cathode active material for a secondary battery may be for a sodium secondary battery.
- the cathode active material for a secondary battery may further contain carbon.
- the present invention includes a sodium secondary battery containing the positive electrode active material described above.
- the positive electrode active material for secondary batteries according to the present invention contains sodium transition metal pyrophosphate according to formula I, and has structural advantages due to the strong P-0 bond of the sodium transition metal phosphate having an oligo structure. As a result, the smooth insertion and desorption of Na ions having a large ion radius can be performed, thereby remarkably improving the reversibility and layer discharge speed during layer discharge.
- Fig. 1 is a scanning electron micrograph of the manufactured sodium iron pyrophosphate.
- Fig. 2 is a manufactured sodium iron pyrophosphate, iron-manganese (Fe 1 22 M n
- FIG. 3 is a diagram illustrating a crystal structure of manufactured sodium iron pyrophosphate by Rietveld refinement using the GSAS program.
- FIG. 6 is a diagram showing a reversible capacity according to the number of charge and discharge cycles of a manufactured sodium iron pyrophosphate secondary battery
- FIG. 7 is a diagram showing changes in reversible capacity (speed characteristic) according to an increase in current density of a manufactured sodium iron pyrophosphate secondary battery.
- the cathode active material for a secondary battery according to the present invention contains sodium transition metal pyrophosphate satisfying the following formula (1).
- M 2 may be the same element having different atoms, and may be different elements having different atoms. May be one or more elements with the atoms of a, and M 2 may be one or more elements with the atoms of b.
- A may be selected from one or more of alkali metals and alkaline earth metals except sodium (Na).
- M or M 2 is At least it may contain transition metals.
- a cathode active material for a secondary battery according to an embodiment of the present invention wherein the transition metal is Sc, Ti,
- Groups 12 to 14 may include Zn, Al, Ga, In, Tl, Ge, Sn and Pb groups.
- the alkali metal may include Li, K, Rb, and Cs groups
- the alkaline earth metal may include Be, Mg, Ca, Sr, and Ba groups. have.
- sodium transition metal pyrophosphate of Chemical Formula 1 may be a discharge state composition of the positive electrode active material.
- a layer discharge is performed at 0.05C in the Na / Na + voltage range, it can mean that the discharge is completed at 1.7 V, and may include the discharge state of the first charge-discharge cycle (charge-discharge).
- the sodium secondary battery subjected to the cycle is
- Cathodic active Conductive material: Binder is mixed in a weight ratio of 7: 1.5: 1.5 and N-methyl
- a slurry of the positive electrode active material prepared by injecting pyrrolidone (NMP) solution was applied on an aluminum foil, and dried in a vacuum oven at 120 ° C. for 10 hours to prepare a positive electrode and sodium metal as a counter electrode, 0.8 M NaC10 4
- sodium transition metals such as NaFeP0 4 in the cathode active material for sodium secondary batteries
- the sodium transition metal phosphate has an oligo structure, so that when the ion radius is very large, such as Na ions, structural limitations are unlikely to result in reversible insertion and removal of ions.
- the sodium transition metal phosphate having an oligo structure is used as the positive electrode active material of the secondary battery, not only the reversibility of the reaction but also the layer discharge rate is very low.
- the positive electrode active material for sodium secondary battery according to the present invention contains sodium transition metal pyrophosphate of Formula 1, and has a strong structural stability even when inserting and desorbing ions due to strong P-0 bonds. Smooth insertion and desorption of ions with large ionic radii can be performed to significantly improve reversibility and layer discharge rates during charging and discharging.
- the sodium transition metal pyrophosphate may be a triclinic phase, and may have a crystal structure of ⁇ -1 space group. Transition metal pyrophosphates [100] and [010] Sodium in the direction can have a tunnel structure with a smooth movement of (Na + ).
- a contained in sodium transition metal pyrophosphate may be one or more selected elements from Li, Mg, and Ca.
- Li, Mg, and Ca have an ion radius similar to that of Na, which can be substituted for the site of sodium (sodium ions) in the crystal structure of sodium transition metal pyrophosphate, leading to a substitutional solid solution. .
- M, and M 2 contained in sodium transition metal pyrophosphate according to Formula 1 are independently of each other, Co, Ni, Fe, Mn, V, It may be at least one selected from Cu, Ti, Al, Cr, Mo and Nb.
- the transition metals Ml and M2 contained in the sodium transition metal pyrophosphate according to Formula 1 may be different elements.
- M L and M 2 contained in sodium transition metal pyrophosphate according to Formula 1 are independently of each other, but at least in Co, Ni, Fe, and Mn. Alternatively, more than one may be selected, preferably, different elements from and M 2 fe.
- the cathode active material for a secondary battery may contain sodium transition metal pyrophosphate satisfying the following Formula 1-1.
- ⁇ 3 ⁇ is one or more selected from Co, Ni, Fe, Mn, V, Cu, Ti, Al, Cr, Mo and Nb having a valency of 2 (M 3 )
- Co, Ni, Fe, Mn, V, Cu, Ti, Al, Cr, Mo, and Nb have similar ionic radii, so that the transition metals in the crystal structure of sodium transition metal pyrophosphates (eg, Fe C) can be substituted at the site, leading to a substitutional solid solution.
- transition metal pyrophosphates eg, Fe C
- the cathode active material 3 ⁇ 4 for secondary batteries is represented by the following chemical formula
- It may contain sodium transition metal pyrophosphate that satisfies 1-2.
- ⁇ 5 ⁇ is an element (M 5 ) at least one selected from Co, Mn, Ni, and Fe having a valency of 2.
- the positive electrode active material for secondary batteries may contain particulate sodium transition metal pyrophosphate.
- the positive electrode active material for secondary batteries has a particulate sodium transition having an average primary particle size of 500 nm to ⁇ . It can contain metal pyrophosphate.
- the positive electrode active material for secondary batteries consists of primary particles and may contain sodium transition metal pyrophosphate, a secondary particle having an average size of ⁇ to 500 ⁇ .
- the positive electrode active material for a secondary battery according to one embodiment of the present invention may further contain carbon. Carbon contained in the positive electrode active material is sufficient to satisfy carbon used in a normal secondary battery positive electrode active material, for example, acetylene black, By all means, soft or hard carbon.
- the sodium transition metal pyrophosphate contained in the positive electrode active material is in a particulate form, and a coating layer coated with carbon may be formed on the surface of the particle.
- the positive electrode active material may further contain 1 to 43 parts by weight of carbon based on 100 parts by weight of sodium transition metal pyrophosphate. Carbon may be in a homogeneous mixture with sodium transition metal pyrophosphate and may exist as a coating layer on the surface of the sodium transition metal pyrophosphate particles.
- the positive electrode active material for a secondary battery is 1.7 / 4.0 V and 0.05 to 0.05.
- It can have a capacity of more than 80mAh / g under charge and discharge conditions of 0.2C (current density).
- the cathode active material for a secondary battery may be a cathode active material for a sodium secondary battery.
- the sodium secondary battery may be a sodium secondary battery or an all-solid-state Na secondary battery having molten Na as a cathode.
- the present invention includes a cathode for a sodium secondary battery containing the cathode active material for secondary batteries described above.
- the anode may include the cathode active material and the current collector described above, and a cathode active material layer coated or coated with the cathode active material may be formed on at least one surface of the current collector.
- a slurry of the positive electrode active material may be applied or coated on the current collector, and the positive electrode active material slurry may contain a dispersion medium, a binder, and a conductive agent commonly used in the manufacture of the secondary battery active material together with the positive electrode active material described above.
- the present invention includes the above-described anode secondary sodium battery.
- a sodium secondary battery may include a cathode containing sodium, an anode having the above-described cathode active material, and an electrolyte having an ion conductivity with respect to sodium ions, provided between the anode and the cathode.
- the sodium secondary battery according to one embodiment of the present invention is an all-solid sodium, in which both the negative electrode containing sodium, the positive electrode containing the positive electrode active material described above, and the electrolyte are all solid.
- a secondary battery including a sodium secondary battery with a liquid electrolyte, a sodium secondary battery with a positive electrolyte along with a solid electrolyte (for example, NASICON), and a separator may be further provided if necessary.
- electrolyte or liquid electrolyte
- the anode and / or cathode may be located in the electrolyte so that the sodium ions conducted in the solid electrolyte can be effectively transferred to the active material.
- the cathode is sodium
- the electrolyte may include an organic solvent containing sodium salt.
- the cathode may be a sodium metal
- the sodium salt in the electrolyte may be NaAsF 6 , NaPF 6 , NaC 10 4 , NaB. (C 6 H 5 ), NaAlCl 4 , NaBr, NaBF 4 or a combination thereof.
- the organic solvent may be ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate. (methylethyl carbonate), propylene carbonate or their mixtures, although the present invention cannot be limited by the type of cathode, the type of electrolyte or the structure of the battery.
- the manufacturing method includes the steps of: preparing a precursor raw material by mixing a sodium precursor, a metal precursor and a phosphate precursor; b) heat treating the precursor raw material in an inert gas atmosphere.
- step b) comprises the steps of bl) heat treating the precursor material in an inert gas atmosphere of 200 to 400 ° C. to produce a first precursor material; and b2) pulverizing the first precursor material; b3) 500 to 1 milled precursor material
- the grinding step (b4) of physically crushing to have a size suitable for the positive electrode active material can be further performed.
- the sodium precursor is sodium carbonate (Na 2 CO 3 ), sodium acetate (NaOCH 2 CH 3 ), sodium carbonate (Na 2 CO 3 ) May include one or more selected materials from sodium hydroxide (NaOH) and their hydrates.
- the metal precursor may comprise one or more selected materials from oxalates, acetates, carbonates and their hydrates of the metal.
- the precursor may comprise one or more materials selected from (NH 4 ) 2 HP0 4 , NH 4 H 2 P0 4 , and 3 ⁇ 41> 4 .
- the metal of the metal precursor may be one or more selected elements from transition metal and group 12 to 14, Specifically, the transition metal is Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Mo, Tc, Ru, Th, Pd, Ag, Hf, Ta, W, Re, Os, Ir,
- Group Pt and Au, group 12 to 14 are Zn, Al, Ga, In, Tl, Ge, Sn and
- the metals in the metal precursors are Co, Ni, Fe, Mn, V, Cu,
- the metal of the metal precursor may be at least one element selected from Co, Ni, Fe and Mn.
- each precursor material can be mixed so that the molar ratio of Na: metal: phosphoric acid is 3 to 3.3: 2.2 to 2.5: 1 in the production of precursor raw materials.
- the mixing of the precursors can be carried out by milling, which is typically used for the homogeneous mixing and grinding of powders, such as ball mills, rod mills or attrition mills. It can be done using the method.
- the raw materials produced are heat treated in an inert gas atmosphere comprising argon, helium, neon, nitrogen or their mixtures.
- the manufactured raw material is subjected to low temperature heat treatment at a temperature of 200 to 400 ° C. in an inert gas atmosphere, and then pulverizes the product obtained by the low temperature heat treatment to a temperature of 500 to 700 ° C. in an inert gas atmosphere. It can be hot heat treated.
- low and high temperature two-stage heat treatment of precursor raw materials are carried out, and the product obtained by low temperature heat treatment is again crushed and mixed by milling including ball mill, rod mill or attrition mill.
- milling including ball mill, rod mill or attrition mill.
- Pyrophosphate Conductive material (Carbon black (super P)): Binder (PVdF; Polyvinylidene fluoride) was mixed in a weight ratio of 7: 1.5: 1.5, and a slurry was prepared using N-methylpyrrolidone (NMP) solution. The slurry was then applied over aluminum foil and dried in a vacuum furnace at 120 ° C. for 10 hours to produce an anode. The anode was prepared in a globe box with sodium metal as the counter electrode, containing 0.8 M NaClO 4 . Ethylene carbonate / diethylene carbonate (l / 1 vol. Ratio) was used as an electrolyte to prepare a cell.
- NMP N-methylpyrrolidone
- FIG. 1 is a scanning electron micrograph of the sodium iron pyrophosphate prepared in Preparation Example 1
- Figure 1 (a) is a high magnification scanning electron micrograph
- Figure 1 (b) is a low magnification
- FIG. 1 A view showing an X- ray diffraction analysis results, and FIG.
- Na 3.12 Fe 2 .44 (P 2 0 7) 2 prepared in Preparation Example 2 1 triclinic crystal system of Na ⁇ Fe ⁇ Mn ⁇ X ⁇ O ⁇ and Production Example '3 confirm that ⁇ .12 ⁇ 2.44 ( ⁇ 2 0 7 ) 2 was prepared.
- the prepared sodium transition metal pyrophosphate has a P-1 space group, and as shown in FIG. It can be seen that the ion radius provides a pathway for desorption of large sodium ions.
- FIG. 6 is a view showing the reversible capacity according to the number of charge and discharge cycles of a sodium secondary battery of Preparation Example 4 containing sodium iron pyrophosphate prepared in Preparation Example 1 as a cathode active material, and 1.7 (discharge)- 4.0 (layer war) V vs. Results of layer discharge at 0.05 C (C / 20 in FIG. 6) and 0.2 C (C / 5 in FIG. 6) in the Na / Na + voltage range. As can be seen in FIG. 6, the reversible insertion and desorption of sodium silver It can be seen that it is performed smoothly, and it can be seen that it has stable layer discharge characteristics even up to 60 cycles.
- the reversible capacity is SOmAhg- 1 or higher, and a reversible capacity of 65 ⁇ 1 ⁇ ⁇ or more is maintained even at a current density of 1C (1C in FIG. 6).
- FIG. 8 is a diagram illustrating the crystal structure of the layered sodium iron pyrophosphate using Rietveld refinement using the GSAS program to confirm the structural change.
- FIG. 9 is a rietveld refinement of the positive electrode active material in the charged state of FIG. As can be seen from the crystal structure analysis, it was confirmed that the tetraclinic structure was maintained even when the sodium ion was inserted or removed.
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Abstract
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Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/904,237 US10026520B2 (en) | 2013-08-16 | 2013-08-16 | Positive electrode active material for secondary battery |
PCT/KR2013/007398 WO2015023017A1 (ko) | 2013-08-16 | 2013-08-16 | 이차전지용 양극 활물질 |
JP2016534518A JP2016534509A (ja) | 2013-08-16 | 2013-08-16 | 二次電池用正極活物質 |
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PCT/KR2013/007398 WO2015023017A1 (ko) | 2013-08-16 | 2013-08-16 | 이차전지용 양극 활물질 |
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WO2015023017A1 true WO2015023017A1 (ko) | 2015-02-19 |
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US (1) | US10026520B2 (ko) |
JP (1) | JP2016534509A (ko) |
WO (1) | WO2015023017A1 (ko) |
Cited By (4)
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WO2018069957A1 (ja) * | 2016-10-11 | 2018-04-19 | 富士通株式会社 | 二次電池用正極材料、及びその製造方法、並びにリチウムイオン二次電池 |
RU2718878C1 (ru) * | 2019-03-28 | 2020-04-15 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Соединение для электродного материала металл-ионных аккумуляторов, электродный материал на его основе, электрод и аккумулятор на основе электродного материала |
CN111446429A (zh) * | 2020-03-27 | 2020-07-24 | 珠海冠宇电池股份有限公司 | 一种聚多阴离子正极材料及其制备方法和用途 |
WO2022102961A1 (ko) * | 2020-11-11 | 2022-05-19 | 삼성전자주식회사 | 양극활물질, 이를 포함하는 양극 및 리튬전지, 및 그 제조방법 |
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CN116364914A (zh) * | 2017-04-27 | 2023-06-30 | 日本电气硝子株式会社 | 钠离子二次电池用正极活性物质 |
JP7101005B2 (ja) * | 2018-03-22 | 2022-07-14 | Fdk株式会社 | 正極活物質の製造方法 |
JP7131258B2 (ja) * | 2018-09-27 | 2022-09-06 | 株式会社豊田自動織機 | 複合粒子の製造方法 |
US20240145679A1 (en) * | 2019-10-04 | 2024-05-02 | The Research Foundation For The State University Of New York | Composition and method for rechargeable battery |
CN113921779B (zh) * | 2021-09-08 | 2022-12-13 | 西北大学 | 一种nasicon型钠快离子导体材料、制备方法及应用 |
CN116053470B (zh) * | 2023-04-03 | 2023-06-20 | 中南大学 | 一种铁基复合正极活性材料及其制备方法和应用 |
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- 2013-08-16 US US14/904,237 patent/US10026520B2/en active Active
- 2013-08-16 WO PCT/KR2013/007398 patent/WO2015023017A1/ko active Application Filing
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018069957A1 (ja) * | 2016-10-11 | 2018-04-19 | 富士通株式会社 | 二次電池用正極材料、及びその製造方法、並びにリチウムイオン二次電池 |
JPWO2018069957A1 (ja) * | 2016-10-11 | 2019-06-27 | 富士通株式会社 | 二次電池用正極材料、及びその製造方法、並びにリチウムイオン二次電池 |
RU2718878C1 (ru) * | 2019-03-28 | 2020-04-15 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Соединение для электродного материала металл-ионных аккумуляторов, электродный материал на его основе, электрод и аккумулятор на основе электродного материала |
CN111446429A (zh) * | 2020-03-27 | 2020-07-24 | 珠海冠宇电池股份有限公司 | 一种聚多阴离子正极材料及其制备方法和用途 |
WO2022102961A1 (ko) * | 2020-11-11 | 2022-05-19 | 삼성전자주식회사 | 양극활물질, 이를 포함하는 양극 및 리튬전지, 및 그 제조방법 |
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JP2016534509A (ja) | 2016-11-04 |
US20160164095A1 (en) | 2016-06-09 |
US10026520B2 (en) | 2018-07-17 |
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