CN110336010A - The preparation method of the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping with strong interaction - Google Patents
The preparation method of the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping with strong interaction Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping with strong interaction, prepare polarity high molecule polymer template agent solution, aqueous slkali, the anion salt solution of doping and transition metal salt solution respectively；Transition metal salt solution and aqueous slkali and the anion salt solution of doping are added in polarity high molecule polymer template agent solution and are stirred to react simultaneously, nano-sheet nanometer presoma can be obtained in refrigerated separation, washing after ageing；Presoma and sodium salt, lithium salts and the cationic salts of doping are subjected to high temperature sintering after mixing, the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping is obtained after natural cooling.Preparation process of the present invention is simple, and can be improved the stability of sodium-ion battery positive material structure, obtains preferable specific capacity and cyclical stability.
Description
Technical field
The invention belongs to the preparation technical fields of sodium-ion battery positive material, and in particular to one kind has strong interaction
The miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping preparation method.
Background technique
The large-scale use of fossil energy brings energy problem and environmental problem, and the development of clean energy resource is then because of tool
Having time, space discontinuity are subject to certain restrictions, therefore need to develop high safety, the extensive storage of long-life, low cost
It can be with distributed energy storage material.In today that lithium ion battery is used widely, although playing alleviation to a certain extent
The effect of energy shortage, but due to price reasons, the application in terms of extensive energy stores is by biggish limitation.It is based on
Advantage in terms of sodium-ion battery raw material reserves and cost is expected to be answered in the fields such as extensive energy storage and distributed energy storage
With.Sodium-ion battery is because having working principle similar with lithium ion battery, will if can effectively utilize sodium-ion battery
It can contribute to environmentally protective and sustainable development.Nowadays have many enterprises both at home and abroad to start to be laid out energy storage sodium ion electricity
Pond.
But the industrialization of sodium-ion battery is faced with a series of problems, if its positive electrode is in high-energy density, circulation
Stability, cycle life, high transformation efficiency and low cost etc. are difficult to take into account.Make to improve the circulation of sodium-ion battery
With performances such as service life and energy densities, the present invention uses the zwitterion doping vario-property nanoscale sodium ion with strong interaction
Cell positive material, the sodium-ion battery positive material after the doping show excellent chemical property.
Summary of the invention
The present invention is provided for current sodium-ion battery positive material cyclical stability difference and the low problem of energy density
The preparation method of the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping with strong interaction a kind of, this method
Nanoscale sodium-ion battery positive material obtained shows higher energy density and preferable cyclical stability.
The present invention is that have similar structure and property according to sodium and lithium on the basis of early-stage study, using similar to lithium
The preparation method of ion battery positive electrode is modified sodium-ion battery positive material.Using polarity high molecular polymer as template
Agent mixes transition metal salt solution, aqueous slkali and the anion salt of doping solution with polarity high molecule polymer template agent
Chemical precipitation reaction is carried out afterwards, obtains nano lamellar presoma through ageing after isothermal reaction, centrifuge washing is dry, by nanometer layer
It is sintered after shape presoma and sodium salt, lithium salts and the cationic salts of doping ground and mixed, high performance sodium ion electricity can be obtained
Pond positive electrode.The sodium-ion battery positive material has the characteristics that energy density height and good cycling stability, for realize sodium from
The further application of sub- battery lays the foundation.
The present invention adopts the following technical scheme that there is the cation-anion co-doping of strong interaction to solve above-mentioned technical problem
The preparation method of miscellaneous nanoscale sodium-ion battery positive material, it is characterised in that detailed process are as follows:
Step S1: anion salt solution, aqueous slkali and the transition of polarity high molecule polymer template agent solution, doping are prepared respectively
Metal salt solution；
The polarity high molecular polymer is polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, citric acid, carboxymethyl cellulose
Element, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, 4- (2- ethoxy)-piperazine ethanesulfonic acid, polyacrylamide, poly- third
One of olefin(e) acid, polymaleic anhydride or poly-quaternary ammonium salt are a variety of；
The anion adulterated in the anion salt solution of the doping is Cl-、Br-、I-、S2-Or Se2-One of or it is a variety of；
The aqueous slkali is one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or ammonium hydroxide or a variety of；
The transition metal salt is soluble nickel salt, soluble cobalt and soluble manganese salt；
Step S2: transition metal salt solution, the anion salt solution of doping and aqueous slkali are added to polarity high molecular polymer
Be stirred to react 0.5-5 hours in template solution in 15-70 DEG C, be aged 0.5-24 hours after reaction, then with detergent from
Drying and grinding obtains nano-sheet presoma after heart washing；
Step S3: nano-sheet presoma is uniformly mixed with sodium salt, lithium salts and the cationic salts of doping, is burnt in 500-1200 DEG C
Knot 6-48 hours obtains having the miscellaneous nanoscale sodium-ion battery anode of the cation-anion co-doping of strong interaction after natural cooling
Material；
The sodium salt is one of sodium carbonate, sodium acetate, sodium chloride or sodium nitrate or a variety of；
The lithium salts is lithium carbonate；
The cation adulterated in the cationic salts of the doping is Mg2+、Zn2+、Ag+、Cu2+、Ti4+、Al3+、Cr4+Or Fe3+In
It is one or more.
Preferably, soluble nickel salt described in step S1 is in nickel sulfate, nickel nitrate, hydrochloric acid nickel, nickel acetate or nickel oxalate
It is one or more, soluble cobalt is one of cobaltous sulfate, cobalt nitrate, hydrochloric acid cobalt, cobalt acetate or cobalt oxalate or a variety of, can
Dissolubility manganese salt is one of manganese sulfate, manganese nitrate, hydrochloric acid manganese, manganese acetate or manganese oxalate or a variety of.
Preferably, the pH value of aqueous slkali described in step S1 is 8-14.
Preferably, OH in the total mole number and aqueous slkali of metal ion in transition metal salt solution described in step S2-'s
The ratio between molal quantity is 1:0.8-1.4, and the anion mol number adulterated in the anion salt solution of doping is transition metal salt solution
The 0.8%-5% of middle metal ion total mole number.
Preferably, the cation mole number adulterated in the cationic salts of doping described in step S3 is nano-sheet presoma
The 0.8%-5% of molal quantity.
Preferably, the combustion atmosphere of sintering process described in step S3 is one of air, oxygen or nitrogen or a variety of.
Compared with the prior art, the invention has the following beneficial effects: nanoscale sodium-ion battery produced by the present invention can
The chemical property of sodium-ion battery is effectively improved, so that sodium-ion battery has preferable cyclical stability and higher energy
Density, first discharge specific capacity is 127.7mAh/g under 0.5C multiplying power.
Detailed description of the invention
Fig. 1 is the XRD diagram of nano-sheet presoma made from the embodiment of the present invention 1；
Fig. 2 is the SEM figure of nano-sheet presoma made from the embodiment of the present invention 2；
Fig. 3 is 0.5C times at room temperature of sodium-ion battery of the preparation of sodium-ion battery positive material made from the embodiment of the present invention 3
Cycle performance figure under rate；
Fig. 4 is the multiplying power of the sodium-ion battery of the preparation of sodium-ion battery positive material made from the embodiment of the present invention 3 at room temperature
Performance map.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Manganese sulfate, nickel sulfate and cobaltous sulfate are dissolved in water according to the ratio mixing of molar ratio 3:1:1 and obtain transition metal salt solution；
Sodium hydroxide is dissolved in water according to 0.8 times that molal quantity is metal ion total mole number in transition metal salt solution and prepares alkali soluble
Liquid, the pH value of the aqueous slkali are 13；Sodium bromide is configured to bromine according to 3% of metal ion total mole number in transition metal salt solution
Change sodium solution；The concentration of polyvinylpyrrolidone is 1g/L, 4- (2- ethoxy)-in polarity high molecule polymer template agent solution
The concentration of piperazine ethanesulfonic acid is 36mmol/L；Under 50 DEG C of water bath conditions, at the same by transition metal salt solution, sodium bromide solution and
Aqueous slkali instills in polarity high molecule polymer template agent solution, and 2h is stirred to react in 50 DEG C, 2h is aged, with deionized water and second
Alcohol centrifuge washing, grinding obtains nano-sheet presoma after 100 DEG C of dryings, and tests its microstructure using XRD, such as schemes
Shown in 1；Nano-sheet presoma is mixed with the zinc nitrate of sodium carbonate, lithium carbonate and nano-sheet presoma molal quantity 3%
It is even, in 900 DEG C of sintering 10h, sodium-ion battery positive material is obtained after natural cooling.
Embodiment 2
Manganese sulfate, nickel sulfate and cobaltous sulfate are dissolved in water according to the ratio mixing of molar ratio 3:1:1 and obtain transition metal salt solution；
Sodium hydroxide is dissolved in water according to 1.4 times that molal quantity is metal ion total mole number in transition metal salt solution and prepares alkali soluble
Liquid, the pH value of the aqueous slkali are 13；Vulcanized sodium is configured to sulphur according to 5% of metal ion total mole number in transition metal salt solution
Change sodium solution；The concentration of polyvinylpyrrolidone is 1.5g/L, 4- (2- hydroxyl second in polarity high molecule polymer template agent solution
Base)-piperazine ethanesulfonic acid concentration be 36mmol/L；Under 50 DEG C of water bath conditions, at the same transition metal salt solution, vulcanized sodium is molten
Liquid and aqueous slkali instill in polarity high molecule polymer template agent solution, and 1.5h is stirred to react in 50 DEG C, are aged 2h, use deionization
Water and ethyl alcohol centrifuge washing, grinding obtains nano-sheet presoma after 60 DEG C of dryings, tests its microscopic appearance by SEM,
As shown in Figure 2.As shown in Figure 2, the microcosmic upper flaky texture that uniform particle sizes are presented of obtained nano-sheet precursor, average thickness
Degree is about 18nm.
Embodiment 3
Manganese sulfate, nickel sulfate and cobaltous sulfate are dissolved in water according to the ratio mixing of molar ratio 3:1:1 and obtain transition metal salt solution；
Sodium hydroxide is dissolved in water according to 1 times that molal quantity is metal ion total mole number in transition metal salt solution and obtains aqueous slkali,
The pH value of the aqueous slkali is 12；Sodium bromide is configured to sodium bromide according to 5% of metal ion total mole number in transition metal salt solution
Solution；The concentration of polyvinylpyrrolidone is 2g/L, 4- (2- ethoxy)-piperazine in polarity high molecule polymer template agent solution
The concentration of ethanesulfonic acid is 32mmol/L；Under 50 DEG C of water bath conditions, while by transition metal salt solution, sodium bromide solution and alkali soluble
Drop enters in polarity high molecule polymer template agent solution, is stirred to react 2h in 50 DEG C, is aged 3h, with deionized water and ethyl alcohol from
Heart washing, grinding obtains nano-sheet presoma after 100 DEG C of dryings；By nano-sheet presoma and sodium carbonate, lithium carbonate
It is uniformly mixed with the silver nitrate of nano-sheet presoma molal quantity 5%, in 800 DEG C of sintering 16h, nanometer is obtained after natural cooling
Grade stratiform sodium-ion battery positive material.
Slurry is made in the grinding of nano-grade sodium-ion battery positive material made from embodiment 3, carries out battery assembly,
Button cell model is CR2032, and the voltage range of battery constant current charging-discharging test is 1.5-4.2V, and test equipment model is new
Weir charge/discharge instrument (Neware CT-4008W, China), at room temperature, cycle performance is as shown in figure 3, surveyed positive electrode
First discharge specific capacity of the sodium-ion battery obtained under 0.5C multiplying power is 127.7mAh/g, and high rate performance is as shown in Figure 4.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (6)
1. the preparation method of the miscellaneous nanoscale sodium-ion battery positive material of cation-anion co-doping with strong interaction, feature
It is detailed process are as follows:
Step S1: anion salt solution, aqueous slkali and the transition of polarity high molecule polymer template agent solution, doping are prepared respectively
Metal salt solution；
The polarity high molecular polymer is polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, citric acid, carboxymethyl cellulose
Element, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, 4- (2- ethoxy)-piperazine ethanesulfonic acid, polyacrylamide, poly- third
One of olefin(e) acid, polymaleic anhydride or poly-quaternary ammonium salt are a variety of；
The anion adulterated in the anion salt solution of the doping is Cl-、Br-、I-、S2-Or Se2-One of or it is a variety of；
The aqueous slkali is one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or ammonium hydroxide or a variety of；
The transition metal salt is soluble nickel salt, soluble cobalt and soluble manganese salt；
Step S2: transition metal salt solution, the anion salt solution of doping and aqueous slkali are added to polarity high molecular polymer
Be stirred to react 0.5-5 hours in template solution in 15-70 DEG C, be aged 0.5-24 hours after reaction, then with detergent from
Drying and grinding obtains nano-sheet presoma after heart washing；
Step S3: nano-sheet presoma is uniformly mixed with sodium salt, lithium salts and the cationic salts of doping, is burnt in 500-1200 DEG C
Knot 6-48 hours obtains having the miscellaneous nanoscale sodium-ion battery anode of the cation-anion co-doping of strong interaction after natural cooling
Material；
The sodium salt is one of sodium carbonate, sodium acetate, sodium chloride or sodium nitrate or a variety of；
The lithium salts is lithium carbonate；
The cation adulterated in the cationic salts of the doping is Mg2+、Zn2+、Ag+、Cu2+、Ti4+、Al3+、Cr4+Or Fe3+In
It is one or more.
2. the miscellaneous nanoscale sodium-ion battery anode material of the cation-anion co-doping according to claim 1 with strong interaction
The preparation method of material, it is characterised in that: the soluble nickel salt described in step S1 is nickel sulfate, nickel nitrate, hydrochloric acid nickel, acetic acid
One of nickel or nickel oxalate are a variety of, and soluble cobalt is in cobaltous sulfate, cobalt nitrate, hydrochloric acid cobalt, cobalt acetate or cobalt oxalate
One or more, soluble manganese salt is one of manganese sulfate, manganese nitrate, hydrochloric acid manganese, manganese acetate or manganese oxalate or a variety of.
3. the miscellaneous nanoscale sodium-ion battery anode material of the cation-anion co-doping according to claim 1 with strong interaction
The preparation method of material, it is characterised in that: the pH value of aqueous slkali described in step S1 is 8-14.
4. the miscellaneous nanoscale sodium-ion battery anode material of the cation-anion co-doping according to claim 1 with strong interaction
The preparation method of material, it is characterised in that: the total mole number and alkali soluble of metal ion in transition metal salt solution described in step S2
OH in liquid-The ratio between molal quantity be 1:0.8-1.4, the anion mol number adulterated in the anion salt solution of doping is transition gold
Belong to the 0.8%-5% of metal ion total mole number in salting liquid.
5. the miscellaneous nanoscale sodium-ion battery anode material of the cation-anion co-doping according to claim 1 with strong interaction
The preparation method of material, it is characterised in that: the cation mole number adulterated in the cationic salts of doping described in step S3 is nanometer
The 0.8%-5% of sheet presoma molal quantity.
6. the miscellaneous nanoscale sodium-ion battery anode material of the cation-anion co-doping according to claim 1 with strong interaction
The preparation method of material, it is characterised in that: in step S3 the combustion atmosphere of sintering process be one of air, oxygen or nitrogen or
It is a variety of.
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| CN113659129A (en) * | 2021-08-18 | 2021-11-16 | 浙江帕瓦新能源股份有限公司 | Multi-element doped ternary precursor and preparation method thereof |
| CN114656001A (en) * | 2022-05-23 | 2022-06-24 | 天津蓝天太阳科技有限公司 | Anion-cation co-doped nickel-manganese-based material and application thereof in positive electrode of sodium ion battery |
| CN115448378A (en) * | 2022-07-21 | 2022-12-09 | 广州大学 | Preparation method of monodisperse nano-sheet high-nickel ternary composite precursor |
| CN117509758A (en) * | 2023-12-22 | 2024-02-06 | 四川轻化工大学 | Preparation and application of nickel-manganese-based sodium-electricity positive electrode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113659129A (en) * | 2021-08-18 | 2021-11-16 | 浙江帕瓦新能源股份有限公司 | Multi-element doped ternary precursor and preparation method thereof |
| CN114656001A (en) * | 2022-05-23 | 2022-06-24 | 天津蓝天太阳科技有限公司 | Anion-cation co-doped nickel-manganese-based material and application thereof in positive electrode of sodium ion battery |
| CN115448378A (en) * | 2022-07-21 | 2022-12-09 | 广州大学 | Preparation method of monodisperse nano-sheet high-nickel ternary composite precursor |
| CN115448378B (en) * | 2022-07-21 | 2024-04-05 | 广州大学 | Preparation method of monodisperse nano-sheet-shaped high-nickel ternary composite precursor |
| CN117509758A (en) * | 2023-12-22 | 2024-02-06 | 四川轻化工大学 | Preparation and application of nickel-manganese-based sodium-electricity positive electrode material |
| CN117509758B (en) * | 2023-12-22 | 2024-07-16 | 四川轻化工大学 | Preparation and application of nickel-manganese-based sodium-electricity positive electrode material |
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Application publication date: 20191015 |