CN110350187A - A kind of stratiform ternary sodium-ion battery method for preparing anode material - Google Patents
A kind of stratiform ternary sodium-ion battery method for preparing anode material Download PDFInfo
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- CN110350187A CN110350187A CN201910552194.9A CN201910552194A CN110350187A CN 110350187 A CN110350187 A CN 110350187A CN 201910552194 A CN201910552194 A CN 201910552194A CN 110350187 A CN110350187 A CN 110350187A
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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
- 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
- H01M4/48—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
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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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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of preparation methods of stratiform ternary sodium-ion battery positive material, the present invention is to solve in existing preparation sodium-ion battery positive material technology, energy consumption height, sintering time length and resulting materials rough surface in sintering step, the problems such as circulating battery stability is bad, and a kind of preparation method of stratiform ternary sodium-ion battery positive material is provided.After mixing by presoma and sodium source, containing being sintered in ozone atmosphere, it is substantially shorter sintering time, reduces production cost, and resulting materials surface is smooth, cyclical stability is higher.
Description
Technical field
The present invention relates to a kind of stratiform ternary sodium-ion battery method for preparing anode material, belong to sodium-ion battery anode material
Expect technical field.
Background technique
Energy problem is one of focus of greatest concern of current century, in particular with the non-renewable money such as petroleum gas
Source is increasingly exhausted, therefore is badly in need of exploring new energy system.The regenerated resources such as solar energy, wind energy, water energy have attracted much attention, but this
It is a little newly can systems there is intermittence and region, how to efficiently use these energy and be faced with many technical problems, and scale
Energy-storage system be the key technology solved these problems.In energy storage mode, efficient and convenient electrochemical energy storage mode becomes
The energy storage mode of mainstream.Lithium ion battery has energy density is high, operating voltage is higher, have extended cycle life, self-discharge rate is small etc.
Advantage is used widely in fields such as electric cars.
However, the continuous growth to lithium ion battery demand, gives the huge pressure of lithium resource bring.Sodium element is in the earth's crust
In content 2.75%, there is rich content, it is cheap, and sodium-ion battery and ion battery are anti-with similar electrochemistry
Mechanism is answered, is all that charge and discharge are realized by the deintercalation of ion.Therefore sodium-ion battery is shown boundless in energy storage field
Application prospect.
Stratiform ternary sodium-ion battery positive material (NaNi1-xMxO2, M=Co, Mn, Al, Fe, Cr) theoretical capacity very
Height (about 240m Ah g-1), cyclical stability is preferable, has tempting application prospect in high capacity sodium-ion battery.Usual layer
In two steps, first step coprecipitation prepares presoma for the preparation of shape sodium ion positive electrode, and second presoma is mixed with sodium source
High temperature is sintered in oxygen atmosphere, obtains final products.But in industrialization engineering, the high-temperature sintering process time is longer, and energy consumption is high,
Oxygen utilization rate is low, so that production cost is increased, meanwhile, even if being sintered in oxygen atmosphere, it not can avoid nickelous still
The problems such as oxidation is not thorough causes sodium element to be unable to fully diffuse into presoma lattice forms high-sequential layer structure three
First positive electrode.Thus the tertiary cathode material surface that also will cause acquisition can remain sodium more than a part, just so as to cause ternary
The stoichiometric ratio of pole material is unbalance and the carbon dioxide and water more tender subject in air, and sodium-ion battery is caused to recycle
Stability in the process, the problems such as high rate performance is bad.In view of the above-mentioned problems, a kind of stratiform ternary sodium-ion battery of the present invention is just
Pole material preparation method after mixing with sodium salt by presoma is sintered, due to the oxygen of ozone using in containing ozone atmosphere
The property changed is stronger, is substantially shorter sintering time.This method is with simple to operate, sintering time is shorter, low in cost, gained
The features such as product surface is smooth, cyclical stability is higher.
Summary of the invention
The present invention is to solve above-mentioned deficiency in the prior art, and providing a kind of has simple to operate, sintering
Time is shorter, low in cost, gained surface is smooth, the higher preparation method of cyclical stability.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of stratiform ternary sodium-ion battery method for preparing anode material, described method includes following steps:
S1, ternary anode material precursor and sodium salt are taken, is uniformly mixed to obtain blend, blend is placed in tube furnace；
S2, under suitable ozone atmosphere, by tube furnace with 2~10 DEG C of min-1Heating rate be warming up to 300~700
DEG C, 1~48h is kept the temperature, is slowly cooled to room temperature after reaction, obtains tertiary cathode material.
Preferably, the content of the ozone is 0.1~100%.
Preferably, ternary anode material precursor described in step S1 and the molar ratio of sodium salt are 1:(1~1.2).
Preferably, the sodium salt is one of sodium hydroxide, sodium carbonate and sodium acetate or a variety of.
According to a kind of stratiform ternary sodium-ion battery method for preparing anode material described herein, obtained tertiary cathode
The chemical formula of material is NaNi(1-x-y)CoxMyO2, x+y≤0.7, M Mn, Al, Mg or Fe.
A kind of sodium-ion battery includes tertiary cathode material made from preparation method described herein.
The beneficial effects of the present invention are:
A kind of stratiform ternary sodium-ion battery method for preparing anode material of the present invention, presoma is uniformly mixed with sodium salt
Afterwards, it is sintered using in atmosphere containing ozone, since the oxidisability of ozone is stronger, is substantially shorter sintering time.This method has
Simple to operate, the features such as sintering time is shorter, low in cost, products obtained therefrom surface is smooth, cyclical stability is higher.
Detailed description of the invention
Fig. 1 is the SEM spectrum of tertiary cathode material prepared by the embodiment of the present invention 1；
Fig. 2 is the battery of the preparation of the embodiment of the present invention 1 in 20mA g-1Current density under activation three circulation, then exist
100mA g-1100 charge and discharge cycles curve graphs are recycled under current density.
Specific embodiment
Below by embodiment, in conjunction with attached drawing, explanation, but guarantor of the invention are further described to technical solution of the present invention
It is without being limited thereto to protect range.
Embodiment 1:
S1, by positive electrode material precursor Ni0.60Co0.02Mn0.02(OH)2It according to molar ratio is 1:1.05 with sodium hydroxide
The blend that ratio is uniformly mixed in a reservoir, blend is put into tube furnace；
S2, the gaseous mixture (the volume ratio 1:4 of ozone and air) that 20% ozone and 80% air are passed through into tube furnace, will
Blend is with 2 DEG C of min-1Heating rate be warming up to 650 DEG C, keep the temperature 12h, be slowly cooled to room temperature after reaction, obtain Na
Ni0.60Co0.02Mn0.02O2Tertiary cathode material；
S3, resulting positive electrode is made into slurry, and dresses up button cell according to existing conventional techniques and carries out electrochemistry
Test；
S4, charge-discharge test is carried out to battery using certain current density, 3 times uses 20mA g-1Current density it is living
Electrochemical cell then uses 100mA g-1Current density carry out charge and discharge cycles, voltage range be 1.5~4.1V, charge and discharge when
Between between be divided into 5min, the pattern of material prepared, phase structure and chemical property are as follows:
Attached drawing 1 is the Na Ni of the present embodiment0.60Co0.02Mn0.02O2Tertiary cathode material treated SEM spectrum, map
Show that the material surface is uniform, it is smooth；
Attached drawing 2 is battery manufactured in the present embodiment first in 20mA g-1Current density under activate 3 times, then in 100mA
g-1Current density under cycle performance figure, 100 times circulation after, discharge capacity still has 166mA h g-1, capacity retention ratio is
98.1% (opposite the 4th charge and discharge).
Embodiment 2:
S1, by positive electrode material precursor Ni0.50Co0.02Mn0.03(OH)2It according to molar ratio is 1:1.03 with sodium hydroxide
The blend that ratio is uniformly mixed in a reservoir, blend is put into tube furnace；
S2, the gaseous mixture (the volume ratio 2:3 of ozone and air) that 40% ozone and 60% air are passed through into tube furnace, will
Blend is with 1 DEG C of min-1Heating rate be warming up to 640 DEG C, keep the temperature 13h, be slowly cooled to room temperature after reaction, obtain Na
Ni0.50Co0.02Mn0.03O2Tertiary cathode material.
S3, resulting positive electrode is made into slurry, and dresses up button cell according to existing conventional techniques and carries out electrochemistry
Test.
The button cell that S4, the material assemble is in 1.5~4.1V voltage range, first in 20mA g-1Current density under
Charge and discharge 3 times, discharge capacity 180mA h g for the first time-1, then in 100mA g-1After being recycled 100 times under current density, discharge capacity
Still there is 155mA h g-1, capacity retention ratio is 97% (opposite the 4th charge and discharge).
Embodiment 3:
S1, by positive electrode material precursor Ni1/3Co1/3Mn1/3(OH)2The ratio for being 1:1.1 according to molar ratio with sodium hydroxide
Uniformly mixed blend in a reservoir, blend is put into tube furnace；
S2, the gaseous mixture (the volume ratio 1:9 of ozone and air) that 10% ozone and 90% oxygen are passed through into tube furnace, will
Blend is with 3 DEG C of min-1Heating rate be warming up to 630 DEG C, keep the temperature 10h, be slowly cooled to room temperature after reaction, obtain Na
Ni1/3Co1/3Mn1/3O2Tertiary cathode material.
S3, resulting positive electrode is made into slurry, and existing conventional techniques is installed and dress up button cell progress electrochemistry
Test.
The button cell that S4, the material assemble is in 1.5~4.1V voltage range, first in 20mA g-1Current density under
Charge and discharge 3 times, discharge capacity 178mA h g for the first time-1, then in 100mA g-1After recycling 52 times under current density, discharge capacity is still
There is 150mA h g-1, capacity retention ratio is 98% (opposite the 4th charge and discharge).
Embodiment 4:
S1, by positive electrode material precursor Ni0.8Co0.1Al0.1(OH)2The ratio for being 1:1.15 according to molar ratio with sodium hydroxide
The blend that example is uniformly mixed in a reservoir, blend is put into tube furnace；
S2, the gaseous mixture (the volume ratio 1:1 of ozone and air) that 50% ozone and 50% air are passed through into tube furnace, will
Blend is with 5 DEG C of min-1Heating rate be warming up to 620 DEG C, keep the temperature 8h, be slowly cooled to room temperature after reaction, obtain Na
Ni0.8Co0.1Al0.1O2Tertiary cathode material.
S3, resulting positive electrode is made into slurry, and dresses up button cell according to existing conventional techniques and carries out electrochemistry
Test.
The button cell that S4, the material assemble is in 1.5~4.1V voltage range, first in 20mA g-1Current density under
Charge and discharge 3 times, discharge capacity 188mA h g for the first time-1, then in 100mA g-1After being recycled 100 times under current density, discharge capacity
Still there is 168mA h g-1, capacity retention ratio is 98.2% (opposite the 4th charge and discharge).
In conclusion the obtained tertiary cathode material of the present processes for sodium-ion battery, be remarkably improved sodium from
The cyclical stability of sub- battery, and the preparation method is simple, it is easy to operate, rapidly and efficiently, remarkable in economical benefits.
Embodiment described above is preferred version of the invention, is not intended to limit the present invention in any form,
There are also other variants and remodeling on the premise of not exceeding the technical scheme recorded in the claims.
Claims (6)
1. a kind of stratiform ternary sodium-ion battery method for preparing anode material, which is characterized in that described method includes following steps:
S1, ternary anode material precursor and sodium salt are taken, is uniformly mixed to obtain blend, blend is placed in tube furnace；
S2, under ozone atmosphere, by tube furnace with 2~10 DEG C of min-1Heating rate be warming up to 300~700 DEG C, heat preservation 1~
48h, cooled to room temperature, obtains tertiary cathode material after reaction.
2. stratiform ternary sodium-ion battery method for preparing anode material according to claim 1, which is characterized in that described smelly
The content of oxygen is 0.1~100%.
3. stratiform ternary sodium-ion battery method for preparing anode material according to claim 1, which is characterized in that step S1
Described in ternary anode material precursor and the molar ratio of sodium salt be 1:(1~1.2).
4. stratiform ternary sodium-ion battery method for preparing anode material according to claim 1, which is characterized in that the sodium
Salt is at least one of sodium hydroxide, sodium carbonate and sodium acetate.
5. stratiform ternary sodium-ion battery method for preparing anode material according to any one of claims 1 to 4, feature exist
In the chemical formula of obtained tertiary cathode material is NaNi(1-x-y)CoxMyO2, x+y≤0.7, M are Mn or Al.
6. a kind of sodium-ion battery, which is characterized in that the sodium-ion battery includes described in Claims 1 to 4 any one
The tertiary cathode material of method preparation.
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Cited By (2)
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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 |
| CN114695853A (en) * | 2022-03-21 | 2022-07-01 | 上海电力大学 | Modified layered ternary positive electrode material of sodium-ion battery and preparation method of modified layered ternary positive electrode material |
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