CN110277555A - A kind of O3 type sodium-ion battery positive material, preparation method and application - Google Patents
A kind of O3 type sodium-ion battery positive material, preparation method and application Download PDFInfo
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- CN110277555A CN110277555A CN201910532644.8A CN201910532644A CN110277555A CN 110277555 A CN110277555 A CN 110277555A CN 201910532644 A CN201910532644 A CN 201910532644A CN 110277555 A CN110277555 A CN 110277555A
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
- H01M4/623—Binders being polymers fluorinated polymers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
Abstract
The invention discloses a kind of O3 type sodium-ion battery positive materials, preparation method and application.By being complexed using sodium salt labile under high temperature, nickel salt, manganese salt and molysite and citric acid, sufficiently making solution be evaporated to obtain wet gel under conditions of being stirred continuously using heating water bath after reaction.Wet gel first carries out pre-burning after being dried and sufficiently removes organic matter and most of impurity, is finally sintered to obtain NaNi at high temperature0.4Mn0.4Fe0.2O2Black powder.Substantially the not loss of element in the preparation process of O3 type sodium-ion battery positive material of the present invention, the element chemistry metering of material is than accurate, O3 type sodium-ion battery positive material particle obtained is thinner, it is used to prepare sodium-ion battery, with preferable coulombic efficiency and cyclical stability, higher charging and discharging capacity is shown when carrying out electro-chemical test.
Description
Technical field
The invention belongs to electrochemistry and new energy materials fields, and in particular to a kind of O3 type sodium-ion battery positive material,
Preparation method and application.
Background technique
Bring energy crisis and environmental problem, renewable energy and clean energy resource are largely used in order to alleviate fossil fuel
Development and utilization become a kind of inexorable trend.Currently, people increasingly pay attention to the development and utilization of clean reproducible energy, respectively
The development of clean reproducible energy is included in national Major Strategic planning by state one after another, is put into a large amount of manpower and material resources and is studied simultaneously
Obtain more achievement.Nearly ten years, intermittent renewable energy and clean energy resource such as wind energy, tide energy and solar energy exist
Specific gravity in human society energy resource structure rises year by year.Since these intermittent energy are by time, place and climatic effect
Larger, these energy cannot be used directly, need that it is stored and is converted using large-scale energy storage system, this is just to energy storage
Technology and device have higher requirement.
Important means of the secondary cell technology as energy storage and conversion, in people's daily life, industrial production, military affairs
National defence and aerospace etc. all have very extensive application, therefore, secondary cell in new energy field in occupation of
Vital status.Currently, the most mature lithium ion battery of with fastest developing speed, technology is closed extensively in secondary cell system
Note.Come using the power that lithium ion battery becomes various mancarried electronic aids and pure electric automobile as the secondary cell system of representative
Source has greatly pushed the development of electronic product and electric car industry.However, the lithium resource in the earth's crust be it is extremely limited,
People be for the consumption of lithium resource it is increased year by year, this not only have stimulated lithium price and persistently increases, and also cause people couple
In the worry of lithium reserves.According to statistics, the reserves of global lithium carbonate are about 13,000,000 tons at present, and the amount of the lithium carbonate consumed every year
Increased with annual 16.5% growth rate, it is contemplated that global lithium resource is only capable of using 28 years for us.This will seriously restrict lithium ion
The further development of battery and energy storage technology.
Sodium and lithium have similar physicochemical property, but the radius ratio lithium ion of sodium ion is big, this has resulted in sodium ion
The performance of battery is not so good as lithium ion battery.However, in the earth's crust sodium element reserves be much larger than lithium, this make sodium-ion battery at
Originally and for there is inherent advantage in amount.In the long run, in addition to extensive energy storage, sodium-ion battery is also in low-speed electronic vehicle, electricity
The dynamic fermentation such as ship and family's energy storage play a role.In recent years, the development of sodium-ion battery is concerned by people, about sodium from
Sub- battery plus-negative plate material, diaphragm, electrolyte research achievement increase year by year.
Sodium-ion battery positive material is the important component of sodium-ion battery, is responsible for providing active sodium ion, need
Oxidation-reduction potential with higher, the activity of positive electrode will have a direct impact on the capacity and operating voltage of battery.It grinds in recent years
The sodium-ion battery positive material with practical value studied carefully mainly has transition metal oxide, polyanionic compound and general
Shandong scholar's indigo plant compound etc..For stratiform transition metal oxide, according to the number and sodium element of sodium element content in material
The difference that material crystal structure plants oneself, studying more stratified material at present can be divided mainly into O3 type and P2 type.Compared to P2
Type stratified material, the main advantage of O3 type stratified material are that this material has material under preferable cyclical stability and high current
Stability is preferable.O3-NaNi0.4Mn0.4Fe0.2O2Material is a kind of stratiform transition metal oxide positive electrode of rich sodium form, system
The standby O3-NaNi that particle is small out, chemical property is good0.4Mn0.4Fe0.2O2Development of the material for sodium-ion battery positive material
It is of great significance.
Summary of the invention
For the deficiency of sodium-ion battery chemical property in the prior art, the present invention provides a kind of O3 type sodium-ion battery
Positive electrode, preparation method and application, the O3 type sodium-ion battery positive material (O3-NaNi being prepared0.4Mn0.4Fe0.2O2)
Powder particle is small, and stoichiometric ratio is accurate, and material repetitive rate is good, and electro-chemical test shows material charge and discharge ratio with higher
Capacity.
The technical solution of the present invention is as follows:
A kind of O3 type sodium-ion battery positive material, the material are nickel manganese sodium ferrite black powder, and chemical formula is
NaNi0.4Mn0.4Fe0.2O2, it is a kind of stratiform transition metal oxide of rich sodium, Na+It occupies in MO2The octahedral site of interlayer
(M Ni, Mn, Fe), it is a kind of layered cathode material of O3 type, which is 200-1000nm.
A kind of preparation method of O3 type sodium-ion battery positive material, by will easily be divided under high temperature using sol-gel method
Sodium salt, nickel salt, manganese salt and the molysite and citric acid of solution are handled to obtain gel, the techniques such as are then dried and are heat-treated
The stratiform nickel manganese sodium ferrite powder of black can be obtained.Specific preparation method the following steps are included:
(1) according to NaNi0.4Mn0.4Fe0.2O2The stoichiometric ratio of middle each element prepares sodium salt, nickel salt, manganese salt and molysite
Mixed solution, metal cation concentration is 0.1-4mol/L in mixed solution, and above-mentioned mixed solution is solution A；Prepare lemon
The aqueous solution of acid is solution B；
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir after no longer changing colour
Mix 1-2h；Wherein, the ratio between amount of substance of citric acid and metal cation is 1-2:1；
(3) pH for the mixed liquor that step (2) obtains is adjusted to 2-4 using ammonium hydroxide, is then stirred in a water bath until solution
It is evaporated, obtains wet gel；
(4) above-mentioned wet gel is dried to obtain xerogel, xerogel is then worn into powdery with mortar；
(5) the powdery xerogel that step (4) obtains is pre-sintered in air atmosphere, pre-sintering temperature 400-
600 DEG C, the pre-sintering time is 6-12h；Again that it is fully calcined in air, calcination temperature is 800-950 DEG C, and calcination time is
9-15h finally obtains nickel manganese sodium ferrite black powder.
Further, sodium salt described in step (1) is at least one of sodium nitrate, sodium acetate and sodium citrate；It is described
Nickel salt is at least one of nickel nitrate, nickel acetate and citric acid nickel；The manganese salt is manganese nitrate, in manganese acetate, manganese citrate
At least one；The molysite is ferric nitrate.
Further, the ratio between amount of substance in step (2) between citric acid and metal cation is preferably 1.3-1.5:
1。
Further, the pH for the mixed liquor that step (2) obtains is adjusted to 2.5-3 using ammonium hydroxide in step (3)；The water
The temperature of bath is 70-90 DEG C.
Further, wet gel is done in 120-150 DEG C of air dry oven or 80-100 DEG C of vacuum oven in step (4)
Dry 6-24h.
Further, it is pre-sintered 9-10h at 450-500 DEG C using Muffle furnace in step (5), using tube furnace in 880-
12-13h is calcined at 920 DEG C.
A kind of application of O3 type sodium-ion battery positive material, using O3 type sodium-ion battery positive material as positive-active
Material, acetylene black are conductive agent, and Kynoar is binder, are 7:2:1 mixing according to its mass ratio, and collector is aluminium foil,
Composition anode；Electrolyte is the organic solution (NC-008) containing sodium perchlorate, and glass fibre is negative as diaphragm, metallic sodium piece
Pole, the assembled battery in argon atmosphere of the partial pressure of oxygen less than 0.1ppm.
Beneficial effects of the present invention: the O3 type sodium-ion battery positive material that the present invention is prepared by sol-gel method
Grain is small, there is no element loss in entire reaction process, so its stoichiometric ratio is accurate.Electro-chemical test shows
Under the conditions of 0.1C charge-discharge magnification, the specific capacity of test voltage 2-4V, the material reach 168.1mAh/g.In addition, of the invention
The O3 type sodium-ion battery positive material of preparation also has preferable coulombic efficiency and cyclical stability, is before one kind has research
The sodium-ion battery positive material of scape.
Detailed description of the invention
Fig. 1 is the XRD diagram of the nickel manganese sodium ferrite of the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the nickel manganese sodium ferrite of the embodiment of the present invention 1；
Fig. 3 is charging and discharging curve figure under the different multiplying of the nickel manganese sodium ferrite of the embodiment of the present invention 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of the nickel manganese sodium ferrite of the embodiment of the present invention 2；
Fig. 5 is cycle performance figure under the 1C of the nickel manganese sodium ferrite of the embodiment of the present invention 2；
Fig. 6 is the XRD diagram of the nickel manganese sodium ferrite of the embodiment of the present invention 3；
Fig. 7 is the high rate performance figure of the nickel manganese sodium ferrite of the embodiment of the present invention 3；
Fig. 8 is the scanning electron microscope (SEM) photograph of the nickel manganese sodium ferrite of the embodiment of the present invention 4.
Specific embodiment
A specific embodiment of the invention, but specific reality described herein are described in detail below in conjunction with technical solution and attached drawing
The mode of applying is only used for the explanation and illustration present invention, is not intended to restrict the invention.
The present invention provides a kind of preparation methods of O3 type sodium-ion battery positive material, by utilizing sol-gel method
Handled sodium salt labile under high temperature, nickel salt, manganese salt and molysite and citric acid to obtain gel, then into excessively dry and
Heat treatment, obtains the stratiform nickel manganese sodium ferrite powder of black.
Embodiment 1
The preparation method of O3 type sodium-ion battery positive material the following steps are included:
(1) mixing for preparing sodium acetate (excessive 3%), nickel acetate, manganese acetate and ferric nitrate according to stoichiometric ratio is molten
Liquid, this GOLD FROM PLATING SOLUTION category cation concn are 0.1mol/L, and above-mentioned solution is solution A；It weighs a certain amount of citric acid and is dissolved in water,
It is configured to solution B；The ratio between amount of substance in citric acid and solution A in solution B between metal cation is 1.5:1.
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir after no longer changing colour
Mix 2h.
(3) pH of the mixed liquor obtained using ammonium hydroxide regulating step (2) is 2.5, then in 80 DEG C of stirred in water bath until
Solution is evaporated, and obtains wet gel.
(4) by above-mentioned wet gel, dry 9h obtains xerogel in 150 DEG C of air dry ovens, then with mortar by xerogel
Wear into powdery.
(5) the powdery xerogel that step (4) obtains is pre-sintered in air atmosphere using Muffle furnace, pre-burning junction temperature
Degree is 500 DEG C, and the pre-sintering time is 9h；Finally using tube furnace that it is fully calcined in air, calcination temperature is 900 DEG C,
Calcination time is 12h, finally obtains the nickel manganese sodium ferrite powder of black.
Using O3 type sodium-ion battery positive material prepared by 1 step of embodiment (1)-(5) as positive electrode active materials, acetylene
Black is conductive agent, and Kynoar is binder, is 7:2:1 mixing according to its mass ratio, and collector is aluminium foil, composition anode；
Electrolyte is the organic solution (NC-008) containing sodium perchlorate, and glass fibre is as diaphragm, and metallic sodium piece is cathode, in partial pressure of oxygen
Assembled battery in argon atmosphere less than 0.1ppm.
Embodiment 2
The preparation method of O3 type sodium-ion battery positive material, comprising the following steps:
(1) mixing of sodium citrate (excessive 3%), nickel acetate, manganese nitrate and ferric nitrate is prepared according to stoichiometric ratio
Solution, this GOLD FROM PLATING SOLUTION category cation concn are 2mol/L, and above-mentioned solution is solution A；It weighs a certain amount of citric acid and is dissolved in water,
It is configured to solution B；The ratio between amount of substance in citric acid and solution A in solution B between metal cation is 1.3:1.
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir after no longer changing colour
Mix 1h.
(3) pH of the mixed liquor obtained using ammonium hydroxide regulating step (2) is 3, then in 70 DEG C of stirred in water bath until molten
Liquid is evaporated, and obtains wet gel.
(4) by above-mentioned wet gel, drying obtains xerogel afterwards for 24 hours in 120 DEG C of air dry ovens, then will be done with mortar
Gel wears into powdery.
(5) the powdery xerogel that step (4) obtains is pre-sintered in air atmosphere using Muffle furnace, pre-burning junction temperature
Degree is 450 DEG C, and the pre-sintering time is 12h；Finally using tube furnace that it is fully calcined in air, calcination temperature is 850 DEG C,
Calcination time is 13h, finally obtains the nickel manganese sodium ferrite powder of black.
With O3 type sodium-ion battery positive electrode active materials prepared by 2 step of embodiment (1)-(5), acetylene black is conductive agent,
Kynoar is binder, is 7:2:1 mixing according to its mass ratio, and collector is aluminium foil, composition anode；Electrolyte is containing height
The organic solution (NC-008) of sodium chlorate, for glass fibre as diaphragm, metallic sodium piece is cathode, in partial pressure of oxygen less than 0.1ppm's
Assembled battery in argon atmosphere.
Embodiment 3
The preparation method of O3 type sodium-ion battery positive material, comprising the following steps:
(1) mixing of sodium nitrate (excessive 3%), citric acid nickel, manganese acetate and ferric nitrate is prepared according to stoichiometric ratio
Solution, this GOLD FROM PLATING SOLUTION category cation concn are 4mol/L, and above-mentioned solution is solution A；It weighs a certain amount of citric acid and is dissolved in water,
It is configured to solution B；The ratio between amount of substance in citric acid and solution A in solution B between metal cation is 1.9:1.
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir after no longer changing colour
Mix 2h.
(3) pH of the mixed liquor obtained using ammonium hydroxide regulating step (2) is 4, then in 90 DEG C of stirred in water bath until molten
Liquid is evaporated, and obtains wet gel.
(4) above-mentioned wet gel is obtained into xerogel after dry 9h in 100 DEG C of vacuum ovens, it then will be dry solidifying with mortar
Glue wears into powdery.
(5) xerogel is pre-sintered in air atmosphere using Muffle furnace, pre-sintering temperature is 600 DEG C, is pre-sintered
Time is 10h；Finally using tube furnace that it is fully calcined in air, calcination temperature is 950 DEG C, calcination time 9h, most
The nickel manganese sodium ferrite powder of black is obtained eventually.
Using O3 type sodium-ion battery positive material prepared by 3 step of embodiment (1)-(5) as positive electrode active materials, acetylene
Black is conductive agent, and Kynoar is binder, is 7:2:1 mixing according to its mass ratio, and collector is aluminium foil, composition anode；
Electrolyte is the organic solution (NC-008) containing sodium perchlorate, and glass fibre is as diaphragm, and metallic sodium piece is cathode, in partial pressure of oxygen
Assembled battery in argon atmosphere less than 0.1ppm.
Embodiment 4
The preparation method of O3 type sodium-ion battery positive material, comprising the following steps:
(1) mixing of sodium acetate (excessive 3%), nickel nitrate, manganese citrate and ferric nitrate is prepared according to stoichiometric ratio
Solution, this GOLD FROM PLATING SOLUTION category cation concn are 0.5mol/L, and above-mentioned solution is solution A；A certain amount of citric acid is weighed to be dissolved in
Water is configured to solution B；The ratio between amount of substance in citric acid and solution A in solution B between metal cation is 1.3:1.
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir after no longer changing colour
Mix 1h.
(3) pH of the mixed liquor obtained using ammonium hydroxide regulating step (2) is 2.5, then in 70 DEG C of stirred in water bath until
Solution is evaporated, and obtains wet gel.
(4) above-mentioned wet gel is obtained into xerogel after dry 9h in 80 DEG C of vacuum ovens, it then will be dry solidifying with mortar
Glue wears into powdery.
(5) xerogel is pre-sintered in air atmosphere using Muffle furnace, pre-sintering temperature is 400 DEG C, is pre-sintered
Time is 12h；Finally using tube furnace that it is fully calcined in air, calcination temperature is 800 DEG C, calcination time 15h, most
The nickel manganese sodium ferrite powder of black is obtained eventually.
Using O3 type sodium-ion battery positive material prepared by 4 step of embodiment (1)-(5) as positive electrode active materials, acetylene
Black is conductive agent, and Kynoar is binder, is 7:2:1 mixing according to its mass ratio, and collector is aluminium foil, composition anode；
Electrolyte is the organic solution (NC-008) containing sodium perchlorate, and glass fibre is as diaphragm, and metallic sodium piece is cathode, in partial pressure of oxygen
Assembled battery in argon atmosphere less than 0.1ppm.
Claims (10)
1. a kind of O3 type sodium-ion battery positive material, which is characterized in that the O3 type sodium-ion battery positive material is nickel manganese
Sodium ferrite black powder, chemical formula NaNi0.4Mn0.4Fe0.2O2；The material is a kind of stratiform transition metal oxide of rich sodium,
Na+It occupies in MO2The octahedral site of interlayer, M Ni, Mn or Fe；The material is a kind of layered cathode material of O3 type, powder
Particle diameter is 200-1000nm.
2. a kind of preparation method of O3 type sodium-ion battery positive material as described in claim 1, which is characterized in that the system
Sodium salt labile under high temperature, nickel salt, manganese salt, molysite and citric acid are handled to obtain by Preparation Method using sol-gel method
Then gel is dried and is heat-treated, obtain the stratiform nickel manganese sodium ferrite powder of black；Specifically includes the following steps:
(1) according to NaNi0.4Mn0.4Fe0.2O2The stoichiometric ratio of middle each element prepares the mixed of sodium salt, nickel salt, manganese salt and molysite
Solution is closed, metal cation concentration is 0.1-4mol/L in mixed solution, and above-mentioned mixed solution is solution A；Prepare citric acid
Aqueous solution is solution B；
(2) solution A and solution B are mixed, obtains mixed liquor, be sufficiently stirred until solution continues to stir 1- after no longer changing colour
2h；Wherein, the ratio between amount of substance of citric acid and metal cation is 1-2:1；
(3) pH for the mixed liquor that step (2) obtains is adjusted to 2-4 using ammonium hydroxide, then in a water bath stirring until solution is evaporated,
Obtain wet gel；
(4) above-mentioned wet gel is dried to obtain xerogel, xerogel is then worn into powdery with mortar；
(5) the powdery xerogel that step (4) obtains being pre-sintered in air atmosphere, pre-sintering temperature is 400-600 DEG C,
The pre-sintering time is 6-12h；Again that it is fully calcined in air, calcination temperature is 800-950 DEG C, calcination time 9-15h,
Finally obtain nickel manganese sodium ferrite black powder.
3. the preparation method of O3 type sodium-ion battery positive material according to claim 2, which is characterized in that step (1)
In, the sodium salt is at least one of sodium nitrate, sodium acetate and sodium citrate；The nickel salt is nickel nitrate, nickel acetate and lemon
At least one of lemon acid nickel；The manganese salt is at least one of manganese nitrate, manganese acetate, manganese citrate；The molysite is nitre
Sour iron.
4. the preparation method of O3 type sodium-ion battery positive material according to claim 2 or 3, which is characterized in that step
(2) in, the ratio between amount of substance between citric acid and metal cation is 1.3-1.5:1.
5. the preparation method of O3 type sodium-ion battery positive material according to claim 2 or 3, which is characterized in that step
(3) in, the pH for the mixed liquor that step (2) obtains is adjusted to 2.5-3 using ammonium hydroxide；The temperature of the water-bath is 70-90 DEG C.
6. the preparation method of O3 type sodium-ion battery positive material according to claim 4, which is characterized in that step (3)
In, the pH for the mixed liquor that step (2) obtains is adjusted to 2.5-3 using ammonium hydroxide；The temperature of the water-bath is 70-90 DEG C.
7. according to the preparation method of sodium-ion battery positive material described in claim 2,3 or 6, which is characterized in that step (4)
In, wet gel dry 6-24h in 120-150 DEG C of air dry oven or 80-100 DEG C of vacuum oven.
8. the preparation method of sodium-ion battery positive material according to claim 4, which is characterized in that wet in step (4)
Gel dry 6-24h in 120-150 DEG C of air dry oven or 80-100 DEG C of vacuum oven.
9. according to the preparation method of O3 type sodium-ion battery positive material described in claim 2,3,6 or 8, which is characterized in that
In step (5), using Muffle furnace at 450-500 DEG C pre-burning 9-10h, calcine 12-13h at 880-920 DEG C using tube furnace.
10. a kind of application of O3 type sodium-ion battery positive material as described in claim 1, which is characterized in that with O3 type sodium
For ion battery positive electrode as positive electrode active materials, acetylene black is conductive agent, and Kynoar is binder, according to O3 type sodium
Ion battery positive electrode, acetylene black, Kynoar mass ratio be 7:2:1 mixing, collector is aluminium foil, composition anode；
Electrolyte is the organic solution containing sodium perchlorate, and glass fibre is cathode as diaphragm, metallic sodium piece, is less than in partial pressure of oxygen
Assembled battery in the argon atmosphere of 0.1ppm.
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| CN111268746A (en) * | 2020-02-05 | 2020-06-12 | 中国科学院化学研究所 | Layered positive electrode material of sodium-ion battery, preparation method and application thereof |
| CN111628164A (en) * | 2020-05-22 | 2020-09-04 | 兰州理工大学 | Sodium ion battery positive electrode material and preparation method thereof |
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