CN105680029A - Sodion positive electrode material and preparing method - Google Patents

Sodion positive electrode material and preparing method Download PDF

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Publication number
CN105680029A
CN105680029A CN201610244680.0A CN201610244680A CN105680029A CN 105680029 A CN105680029 A CN 105680029A CN 201610244680 A CN201610244680 A CN 201610244680A CN 105680029 A CN105680029 A CN 105680029A
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nacl
deionized water
surfactant
positive electrode
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王银娣
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/621—Binders
    • 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
    • H01M4/624—Electric conductive fillers
    • 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

Abstract

The invention discloses a sodion positive electrode material and a preparing method. The preparing method includes the steps that NaV6O15, acetylene black and a binding agent are mixed by the mass ratio of 75:15:10, an appropriate amount of N-methyl-2-pyrrolidone is added dropwise, the mixture is continuously ground and stirred to be uniform paste, a metal bar is coated with the paste and dried in vacuum to obtain the sodion positive electrode material. The NaV6O15 crystal structure is a nano rodlike structure uniform in size and is prepared from NH4VO3, NaCl, a surfactant and deionized water by the mass ratio of 1:(1.5-2.5):(0.1-0.3):100 on the highly acidic hydrothermal condition. The appropriate content of the surfactant in the prepared NaV6O15 electrode material is determined, the prepared NaV6O15 crystal structure is a nano rodlike structure uniform in size, the electrode material prepared from NaV6O15 is excellent in electrochemical performance, then a prepared battery is excellent in electrochemical performance, and the sodion positive electrode material is low in cost and has huge application and development prospects.

Description

Sodium ion positive electrode and preparation method
Technical field
The present invention relates to a kind of positive electrode, especially relate to a kind of sodium ion positive electrode and preparation method.
Background technology
Along with prevailing of the new-energy automobile being representative with tesla, lithium ion battery obtains express delivery at full speed. But lithium ion battery is limited to exploitation and the processing of lithium ore resources, constantly rising suddenly and sharply from the second half year in 2014 of lithium carbonate price so far is exactly best proof. For this reason, it is necessary to exploitation sodium-ion battery as an alternative product similar to lithium ion battery operation principle, sodium ion electronics has that cost is low and the feature of excellent electrochemical performance, it is believed that in the development prospect that future is also huge.
Summary of the invention
The present invention proposes that a kind of preparation technology is simple, realize sodium ion positive electrode that is less costly and that have good electric chemical property and preparation method.
A kind of sodium ion positive electrode, by NaV6O15, after acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on metal bar to homogeneous paste, vacuum drying is made; Wherein, NaV6O15Crystal structure be size uniform nano bar-shape structure, by mass ratio NH4VO3: NaCl: surfactant: deionized water=1:(1.5～2.5): (0.1～0.3): the NH of 1004VO3, NaCl, surfactant and deionized water be prepared under highly acid hydrothermal condition.
Wherein, NH4VO3: NaCl: surfactant: deionized water=1:2:0.2:100.
A kind of preparation method of sodium ion positive electrode, comprising:
Step one, in mass ratio NH4VO3: NaCl: surfactant: deionized water=1:(1.5～2.5): (0.1～0.3): 100 take NH4VO3, NaCl and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, be stirred continuously to being completely dissolved at 60 DEG C, add appropriate hydrochloric acid and regulate mixing and be easy to pH value to less than 2;
Step 2, pour gained mixed solution into stainless steel autoclave, 200 DEG C of-300 DEG C of Water Unders thermal response 12-24 hour, NH4VO3In VO3-Can with the H of hydrochloric acid+In conjunction with generating HVO3, HVO3Hydrolysis generates the V with layer structure further2O5, along with the carrying out of hydro-thermal reaction, system temperature elevated pressure increases, and the Na ion in NaCl can progressively embed V2O5Layer structure in, ultimately generate NaV6O15, then naturally cool to room temperature and carry out vacuum filtration, respectively washing twice with deionized water and ethanol, after vacuum drying, placing in high temperature furnace 400 DEG C-600 DEG C and calcine 6-12 hour, prepare the NaV into brown ceramic powder6O15;
Step 3, the NaV that will prepare6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on metal bar to homogeneous paste, namely vacuum drying is fabricated to positive pole.
Wherein, NH4VO3: NaCl: surfactant: deionized water=1:2:0.2:100.
Wherein, metal bar is aluminium bar or copper rod.
Compared with prior art, there is advantages that
Present invention determine that preparation NaV6O15In electrode material, the appropriate content of surfactant, prepares NaV6O15Crystal structure be size uniform nano bar-shape structure, by NaV6O15The electrode material of preparation has preferably chemical property, and then the chemical property of the battery prepared is also preferably, therefore the present invention realizes less costly, and has huge application development prospect.
Detailed description of the invention
Step one, in mass ratio NH4VO3: NaCl: surfactant: deionized water=1:(1.5～2.5): (0.1～0.3): 100 take NH4VO3, NaCl, surfactant and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, be stirred continuously to being completely dissolved at 60 DEG C, add appropriate strong acid solution (than example hydrochloric acid, sulphuric acid etc.) and regulate mixing and be easy to pH value to less than 2.
Step 2, pour gained mixed solution into teflon lined stainless steel autoclave, 200 DEG C of-300 DEG C of Water Unders thermal response 12-24 hour, then room temperature is naturally cooled to, by react product carries out vacuum filtration, respectively wash twice with deionized water and ethanol, after vacuum drying, place in high temperature furnace 400 DEG C-600 DEG C and calcine 6-12 hour, prepare the NaV into brown ceramic powder6O15。
For strong acid for hydrochloric acid. In hydrothermal reaction process, in acid condition, NH4VO3In VO3-Can with the H of hydrochloric acid+In conjunction with generating HVO3, HVO3Hydrolysis generates the V with layer structure further2O5Even if along with the carrying out of hydro-thermal reaction, system temperature elevated pressure increases, and the Na ion in NaCl can progressively embed V2O5Layer structure in, ultimately generate NaV6O15。
In above-mentioned steps one, if adding excessive or a small amount of surfactant, all it is unfavorable for the generation NaV ultimately generated6O15Crystal structure. It is demonstrated experimentally that when adding excessive or a small amount of surfactant, the NaV ultimately produced6O15Crystal structure be that length difference is big and the unordered laminated structure piled up, the NaV of this crystal structure6O15When being used for preparing positive pole, charge and discharge process there will be the more serious polarization phenomena of ratio, its chemical property produced very adverse influence. And present invention determine that the adding proportion of surfactant, surfactant can effectively reduce original interfacial tension, it is also possible to material difference crystal face is produced different selective absorptions simultaneously, utilize space steric effect to reduce product reunite and change pattern, realize the controlledly synthesis to product morphology, therefore the present invention has been determined by the adding proportion of surfactant, make the NaV prepared6O15Crystal structure be size uniform nano bar-shape structure.
Step 3, the NaV that will prepare6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat to homogeneous paste on metal bar (such as aluminum, copper etc.), namely vacuum drying is fabricated to positive pole.
Embodiment 1
NH in mass ratio4VO3: NaCl: surfactant: deionized water=1:1.5:0.1:100 takes NH4VO3, NaCl and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, add appropriate hydrochloric acid and regulate mixing and be easy to pH value to 2.Pour gained mixed solution into teflon lined stainless steel autoclave, 200 DEG C of Water Under thermal responses 24 hours, then room temperature is naturally cooled to, by react product carries out vacuum filtration, respectively wash twice with deionized water and ethanol, after vacuum drying, place in high temperature furnace 400 DEG C and calcine 12 hours, prepare the NaV into brown ceramic powder6O15. This NaV prepared is found through the detection of Flied emission transmission electron microscope6O15The nano bar-shape structure of crystal structure length all about 1.35um and even particle size.
NaV by preparation6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on aluminium bar to homogeneous paste, namely vacuum drying is fabricated to positive pole. Making electrode with metallic sodium, barrier film made by glass fibre, adds electrolyte and namely constitutes battery. After tested, when voltage 3.5V, when electric current density respectively 20,50,100 and 150mAg-1Time, this battery discharge capacity first respectively 147,128,118 and 107mAhg-1, the capacity retention after 30 charge and discharge cycles is 64.3%, 68.7%, 71.9% and 74.1%.
Embodiment 2
Mass ratio NH4VO3: NaCl: surfactant: deionized water=1:2:0.2:100 takes NH4VO3, NaCl and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, be stirred continuously to being completely dissolved at 60 DEG C, add appropriate strong acid solution (than example hydrochloric acid, sulphuric acid etc.) and regulate mixing and be easy to pH value most 1. Pour gained mixed solution into teflon lined stainless steel autoclave, 300 DEG C of Water Under thermal responses 12 hours, then room temperature is naturally cooled to, by react product carries out vacuum filtration, respectively wash twice with deionized water and ethanol, after vacuum drying, place in high temperature furnace 600 DEG C and calcine 6 hours, prepare the NaV into brown ceramic powder6O15. This NaV prepared is found through the detection of Flied emission transmission electron microscope6O15The nano bar-shape structure that crystal structure is length all about 1.5um and even particle size.
NaV by preparation6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on aluminium bar to homogeneous paste, namely vacuum drying is fabricated to positive pole. Making electrode with metallic sodium, barrier film made by glass fibre, adds electrolyte and namely constitutes battery. After tested, when voltage 3.5V, when electric current density respectively 20,50,100 and 150mAg-1Time, this battery discharge capacity first respectively 167,158,142 and 124mAhg-1, the capacity retention after 30 charge and discharge cycles is 66.1%, 69.5%, 73.2% and 76.4%.
Embodiment 3
Mass ratio NH4VO3: NaCl: surfactant: deionized water=1:2.5:0.3:100 takes NH4VO3, NaCl and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, be stirred continuously to being completely dissolved at 60 DEG C, add appropriate strong acid solution (than example hydrochloric acid, sulphuric acid etc.) and regulate mixing and be easy to pH value most 1. Pour gained mixed solution into teflon lined stainless steel autoclave, 300 DEG C of Water Under thermal responses 12 hours, then room temperature is naturally cooled to, by react product carries out vacuum filtration, respectively wash twice with deionized water and ethanol, after vacuum drying, place in high temperature furnace 600 DEG C and calcine 6 hours, prepare the NaV into brown ceramic powder6O15.This NaV prepared is found through the detection of Flied emission transmission electron microscope6O15The nano bar-shape structure that crystal structure is length all about 1.4um and even particle size.
NaV by preparation6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on aluminium bar to homogeneous paste, namely vacuum drying is fabricated to positive pole. Making electrode with metallic sodium, barrier film made by glass fibre, adds electrolyte and namely constitutes battery. After tested, when voltage 3.5V, when electric current density respectively 20,50,100 and 150mAg-1Time, this battery discharge capacity first respectively 159,151,134 and 114mAhg-1, the capacity retention after 30 charge and discharge cycles is 63.4%, 65.7%, 71.9% and 75.8%.
Being proved by the above-mentioned test to battery, the number of the addition of surfactant can be effectively improved NaV6O15The chemical property of electrode material, this with synthesis NaV6O15Pattern for the nano bar-shape of size uniform is relevant, it is possible not only to reduce the distance of sodium ion diffusion and electric transmission in charge and discharge process, and increase the contact area between electrode material and electrolyte, be conducive to the infiltration of electrolyte, thus improving chemical property. But, excessive surfactant can make on the contrary as NaV6O15Pattern be irregular shape, reduce the chemical property of electrode material on the contrary, therefore present invention determine that preparation NaV6O15The appropriate content of surfactant in electrode material, it can be ensured that electrode material has the chemical property of the best, and the performance of the battery prepared is also best.
It addition, the surfactant that the present invention mentions is prepare any surfactant used in sodium-ion battery in prior art, it is not described in detail one by one at this.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention.

Claims (5)

1. a sodium ion positive electrode, it is characterised in that by NaV6O15, after acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on metal bar to homogeneous paste, vacuum drying is made;
Wherein, NaV6O15Crystal structure be size uniform nano bar-shape structure, by mass ratio NH4VO3: NaCl: surfactant: deionized water=1:(1.5～2.5): (0.1～0.3): the NH of 1004VO3, NaCl, surfactant and deionized water be prepared under highly acid hydrothermal condition.
2. sodium ion positive electrode according to claim 1, it is characterised in that NH4VO3: NaCl: surfactant: deionized water=1:2:0.2:100.
3. the preparation method of a sodium ion positive electrode, it is characterised in that including:
Step one, in mass ratio NH4VO3: NaCl: surfactant: deionized water=1:(1.5～2.5): (0.1～0.3): 100 take NH4VO3, NaCl and deionized water, by NH4VO3, NaCl and surfactant be dissolved in deionized water, be stirred continuously to being completely dissolved at 60 DEG C, add appropriate hydrochloric acid and regulate mixing and be easy to pH value to less than 2;
Step 2, pour gained mixed solution into stainless steel autoclave, 200 DEG C of-300 DEG C of Water Unders thermal response 12-24 hour, NH4VO3In VO3-Can with the H of hydrochloric acid+In conjunction with generating HVO3, HVO3Hydrolysis generates the V with layer structure further2O5, along with the carrying out of hydro-thermal reaction, system temperature elevated pressure increases, and the Na ion in NaCl can progressively embed V2O5Layer structure in, ultimately generate NaV6O15, then naturally cool to room temperature and carry out vacuum filtration, respectively washing twice with deionized water and ethanol, after vacuum drying, placing in high temperature furnace 400 DEG C-600 DEG C and calcine 6-12 hour, prepare the NaV into brown ceramic powder6O15;
Step 3, the NaV that will prepare6O15, acetylene black and binding agent 75:15:10 in mass ratio mixing, drip appropriate METHYLPYRROLIDONE, constantly grind stirring and coat on metal bar to homogeneous paste, namely vacuum drying is fabricated to positive pole.
4. the preparation method of sodium ion positive electrode according to claim 3, it is characterised in that NH4VO3: NaCl: surfactant: deionized water=1:2:0.2:100.
5. the preparation method of sodium ion positive electrode according to claim 3, metal bar is aluminium bar or copper rod.
CN201610244680.0A 2016-04-18 2016-04-18 Sodion positive electrode material and preparing method Pending CN105680029A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110729474A (en) * 2019-10-24 2020-01-24 成都先进金属材料产业技术研究院有限公司 NaV preparation by using failure vanadium battery electrolyte6O15Method for preparing sodium ion battery electrode material

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110729474A (en) * 2019-10-24 2020-01-24 成都先进金属材料产业技术研究院有限公司 NaV preparation by using failure vanadium battery electrolyte6O15Method for preparing sodium ion battery electrode material

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Application publication date: 20160615