CN108288701B - Sodium ion battery positive electrode complex phase material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 24
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 23
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- 229910019469 NaV6O15 Inorganic materials 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 239000013077 target material Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Substances OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- 238000002441 X-ray diffraction Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 abstract description 22
- 239000007772 electrode material Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000010405 anode material Substances 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- 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
- H01M4/362—Composites
-
- 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
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- 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
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- 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
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a sodium ion battery anode multiphase material Na1.1V3O7.9/NaV6O15The multiphase material is prepared by adjusting hydrothermal temperature to prepare a precursor material VO2Mixing with NaOH according to a certain proportion, and performing heat treatment to obtain the complex phase target material Na1.1V3O7.9/NaV6O15The complex phase electrode material has excellent electrochemical performance when used as the positive electrode of the sodium ion battery.
Description
Technical Field
The invention relates to a sodium-ion battery positive electrode multiphase material Na with good electrochemical performance1.1V3O7.9/NaV6O15Belonging to the technical field of positive electrode materials of sodium ion batteries.
Background
The sodium element and the lithium element are in the same main group, have similar physical and chemical properties, and have the advantages of rich global reserves, wide distribution, simple extraction and the like. Research conditions in recent years show that sodium ion batteries have electrochemical performance similar to that of lithium ion batteries, and therefore, sodium ion batteries are also considered to be a novel energy storage battery system with great potential, and development of research work on sodium ion batteries is of great significance for maintaining sustainable development of energy. Similar to lithium ion batteries, sodium ion batteries have a major problem that the positive electrode material of the batteries still cannot meet the requirements of high energy and high power. The vanadium compound material with low cost and high specific capacity becomes a hotspot for researching the sodium-ion battery. The vanadate material has the advantages of high capacity, low cost, easy synthesis and the like, and has good application prospect in the fields of sodium ion batteries and the like. But the vanadium anode material has poor cycle stability and rate capabilityThe major problems facing today. Na (Na)1.1V3O7.9A layered compound belonging to a monoclinic, 21/m space group, Na+Occupies octahedral void sites between layers, which have higher activation energy. Na (Na)1.1V3O7.9The lithium/Na ion secondary battery anode material has high specific capacity by carrying out ion embedding and ion releasing through oxidation and reduction reactions with ions, and the current research mainly improves the cycling stability of the lithium/Na ion secondary battery anode material through the nanocrystallization and the structural compounding of the material size. NaV6O15Belongs to A2/m (12) space group a =10.07 Å, b =3.61 Å and c =15.38 Å, and simultaneously has a three-dimensional channel structure capable of providing sodium ion migration, and consists of shared [ VO6]The octahedron forms a zigzag chain, and the zigzag chains are connected through a common point to form a plane. [ VO5]The quadrangular pyramid is arranged in a twisted manner as a plane with [ VO ]6]The octahedral layers together form a channel structure, the interior of which can then be filled with lithium/sodium ions. NaV6O15The valence of the medium vanadium element is +4.83, near its maximum valence (+ 5). V4+/V5+The mixed valence of (A) makes it have very high electronic conductivity and chemical reactivity. The targeted modification and doping of the electrode material morphology is an effective means for improving the specific capacity, the cycle performance and the rate capability. The invention mainly relates to a complex phase electrode material Na1.1V3O7.9/NaV6O15And the lithium ion battery has excellent electrochemical performance when used as a positive electrode of a sodium ion battery.
Disclosure of Invention
Mainly aiming at the problem of poor cycle stability of vanadium anode materials, the invention adjusts hydrothermal temperature to prepare precursor VO2Mixing with NaOH according to a certain proportion, and performing heat treatment to obtain the complex phase target material Na1.1V3O7.9/NaV6O15The material has excellent electrochemical performance when used as a positive electrode of a sodium ion battery.
The specific preparation scheme is as follows:
(1) a certain amount of V2O5(molecular weight 181.88, analytical grade), oxalic acid,Distilled water is mixed according to the mass ratio of 1: 1: 30, stirring the mixture for 2 hours at the temperature of 80 ℃, pouring the mixture into a polytetrafluoroethylene reaction kettle, controlling the filling volume to be 80 percent, adjusting the hydrothermal temperature to be 160-200 ℃, preserving the heat for 24 hours, collecting blue-black precipitates, washing and drying to obtain the required precursor material VO2。
(2) Adding a certain amount of the precursor material VO in the step (1)2NaOH and ethanol according to a mass ratio of 1: 0.16: 100, stirring at 80 deg.C to evaporate ethanol, collecting powder, calcining at 450 deg.C for 8 hr to obtain Na as target material1.1V3O7.9/NaV6O15。
(3) A certain amount of the target material Na prepared in the above (2)1.1V3O7.9/NaV6O15Acetylene black and polyvinylidene fluoride (PVDF) according to the mass ratio of 8: 1: 1, adding N-methyl pyrrolidone solvent, and stirring to obtain colloidal precoating refined slurry.
(4) And (3) coating the precoated refined slurry prepared in the step (3) on an aluminum foil, drying at 130 ℃ for 0.5h and at 110 ℃ for 12h in vacuum, naturally cooling, and cutting into a wafer with the diameter of 12mm by using a punching machine to obtain the positive electrode plate of the sodium-ion battery.
(5) Sequentially assembling the positive electrode shell, the electrode plate, the electrolyte, the diaphragm, the electrolyte, the sodium sheet, the gasket, the elastic sheet and the negative electrode shell, and sealing the battery by using a sealing machine to obtain the CR2032 type button half-battery.
(6) Using a CT-3008W-5V-10mA-S4 type charge-discharge instrument, wherein the charge-discharge voltage is 1.5-4.0V and 300mAg-1And carrying out charge and discharge tests on the battery under the current density.
The invention has the following remarkable advantages:
(1) using V2O5Oxalic acid and NaOH are used as initial raw materials, the materials are cheap and easy to obtain, and the production cost is reduced.
(2) The multiphase electrode material Na1.1V3O7.9/NaV6O15The production process is simple and easy to operate, and large-scale industrial production can be realized.
(3) Multiphase electrode material Na1.1V3O7.9/NaV6O15When used as the positive electrode material of the sodium-ion battery, the capacity performance and the cycle performance of the material are both better than those of single-phase Na1.1V3O7.9With single-phase NaV6O15。
Description of the drawings:
FIG. 1 shows a multiphase electrode material Na of the present invention1.1V3O7.9/NaV6O15In which ♦ represents NaV6O15Peak of (3), ♠ represents Na1.1V3O7.9The peak of (a) is consistent with the standard spectrum of the two.
FIG. 2 shows a multiphase electrode material Na in example 2 of the present invention1.1V3O7.9/NaV6O15300mAg when used as the positive electrode of a sodium ion battery-1The current density of (a), wherein the ordinate is the specific capacity and the abscissa is the cycle number.
The specific implementation method comprises the following steps:
example 1:
(1) a certain amount of V2O5(molecular weight 181.88, analytical purity), oxalic acid, distilled water according to the mass ratio of 1: 1: 30, stirring the mixture for 2 hours at the temperature of 80 ℃, pouring the mixture into a polytetrafluoroethylene reaction kettle, controlling the filling volume to be 80 percent, adjusting the hydrothermal temperature to be 160 ℃, preserving the heat for 24 hours, collecting blue-black precipitates, washing and drying the blue-black precipitates to obtain the required precursor material VO2。
(2) Adding a certain amount of the precursor material VO in the step (1)2Mixing NaOH and ethanol (mass ratio 1: 0.16: 100) to obtain suspension, stirring at 80 deg.C to volatilize ethanol, collecting powder, calcining at 450 deg.C for 8 hr to obtain target material Na1.1V3O7.9/NaV6O15。
The synthetic material has a charging and discharging voltage of 1.5-4.0V and 300mAg-1The first discharge specific capacity is 70mAhg under the current density-1And the specific discharge capacity after 100 cycles is 61mAhg-1And excellent cycle performance is shown.
Example 2:
(1) a certain amount of V2O5(molecular weight 181.88, analytical purity), oxalic acid, distilled water according to the mass ratio of 1: 1: 30, stirring the mixture for 2 hours at the temperature of 80 ℃, pouring the mixture into a polytetrafluoroethylene reaction kettle, controlling the filling volume to be 80 percent, adjusting the hydrothermal temperature to be 180 ℃, preserving the heat for 24 hours, collecting blue-black precipitates, washing and drying the blue-black precipitates to obtain the required precursor material VO2。
(2) Adding a certain amount of the precursor material VO in the step (1)2Mixing NaOH and ethanol (mass ratio 1: 0.16: 100) to obtain suspension, stirring at 80 deg.C to volatilize ethanol, collecting powder, calcining at 450 deg.C for 8 hr to obtain target material Na1.1V3O7.9/NaV6O15。
The synthetic material has a charging and discharging voltage of 1.5-4.0V and 300mAg-1The first discharge specific capacity is 97mAhg at current density-1The specific discharge capacity after 1000 cycles is 107mAhg-1. The electrochemical performance of the material is shown in figure 2.
Example 3:
(1) a certain amount of V2O5(molecular weight 181.88, analytical purity), oxalic acid, distilled water according to the mass ratio of 1: 1: 30, stirring the mixture for 2 hours at the temperature of 80 ℃, pouring the mixture into a polytetrafluoroethylene reaction kettle, controlling the filling volume to be 80 percent, adjusting the hydrothermal temperature to be 200 ℃, preserving the heat for 24 hours, collecting blue-black precipitates, washing and drying the blue-black precipitates to obtain the required precursor material VO2。
(2) Adding a certain amount of the precursor material VO in the step (1)2Mixing NaOH and ethanol (mass ratio 1: 0.16: 100) to obtain suspension, stirring at 80 deg.C to volatilize ethanol, collecting powder, calcining at 450 deg.C for 8 hr to obtain target material Na1.1V3O7.9/NaV6O15。
The synthetic material has a charging and discharging voltage of 1.5-4.0V and 300mAg-1First discharge ratio at current densityCapacity of 163mAhg-1The specific discharge capacity after 100 cycles was 104mAhg-1And the specific capacity is higher.
Claims (1)
1. Sodium-ion battery positive electrode complex-phase material Na1.1V3O7.9/NaV6O15And represents Na in X-ray diffraction pattern thereof1.1V3O7.9And represents NaV6O15The peak of (A) is consistent with the standard spectrogram of the two, and the peak is prepared by the following method:
(1) a certain amount of V2O5Oxalic acid and distilled water according to the mass ratio of 1: 1: 30, stirring the mixture for 2 hours at the temperature of 80 ℃, pouring the mixture into a polytetrafluoroethylene reaction kettle, controlling the filling volume to be 80 percent, adjusting the hydrothermal temperature to be 180 ℃, preserving the heat for 24 hours, collecting blue-black precipitates, washing and drying the blue-black precipitates to obtain the required precursor material VO2；
(2) Adding a certain amount of the precursor material VO in the step (1)2NaOH and ethanol according to a mass ratio of 1: 0.16: 100 preparing into suspension, stirring at 80 deg.C to volatilize ethanol, collecting powder, calcining at 450 deg.C for 8 hr to obtain target material Na1.1V3O7.9/NaV6O15。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109626425B (en) * | 2019-02-25 | 2021-02-02 | 上海海事大学 | Nano linear Na1.1V3O7.9Material, method for the production thereof and use thereof |
| CN110467221A (en) * | 2019-09-17 | 2019-11-19 | 安徽建筑大学 | A kind of NaV6O15The preparation method of film and NaV obtained6O15Film |
| CN110729474B (en) * | 2019-10-24 | 2021-04-06 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing NaV6O15 sodium ion battery electrode material by using spent vanadium battery electrolyte |
| CN111153436A (en) * | 2019-12-31 | 2020-05-15 | 中国地质大学（武汉） | Self-assembly NaV6O15Nanosheet microsphere and preparation method and application thereof |
| CN114956171A (en) * | 2021-02-24 | 2022-08-30 | 陕西则明未来科技有限公司 | Preparation and application of sodium-vanadium-oxygen heterojunction material |
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