CN108470906A - The method for preparing high-performance sodium-ion battery positive material using double template - Google Patents
The method for preparing high-performance sodium-ion battery positive material using double template Download PDFInfo
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- CN108470906A CN108470906A CN201810175773.1A CN201810175773A CN108470906A CN 108470906 A CN108470906 A CN 108470906A CN 201810175773 A CN201810175773 A CN 201810175773A CN 108470906 A CN108470906 A CN 108470906A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/52—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
- 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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Abstract
The invention discloses it is a kind of using double template prepare high-performance sodium-ion battery positive material method, the specific steps are：Prepare double template solution, aqueous slkali and the transition metal salt solution of polarity high molecular polymer and surfactant；The double template solution of polarity high molecular polymer and surfactant is added in reaction kettle, aqueous slkali is added simultaneously under conditions of 15 70 DEG C of stirrings and transition metal salt solution is reacted, it is aged after reaction, then it cools down, centrifuge washing, it is washed again with detergent, is dried after centrifugation and obtain sheet presoma；Sheet presoma and sodium salt are sintered 6 48h in 600 1200 DEG C after mixing and obtain high-performance sodium-ion battery positive material.Sodium-ion battery positive material obtained by the present invention can improve the chemical property of sodium-ion battery, and sode cell cell positive material is made to have higher specific discharge capacity and preferable cyclical stability.
Description
Technical field
The invention belongs to the preparation of electrochmical power source material and sodium-ion battery positive material technical fields, and in particular to a kind of
The method for preparing high-performance sodium-ion battery positive material using double template.
Background technology
With the development of society, the energy has become the important substance basis that human society is depended on for existence and development, it is economical
High speed development makes the demand of the energy and Efficient Conversion increasingly increase with storage.In addition, regenerative resource such as wind energy and solar energy, though
Have its advantage but disadvantage be also more, have the characteristics that it is efficient, have extended cycle life, maintenance cost is low, at low cost and environmentally protective
Electrochemical energy storage receive the concern of people.Although lithium ion battery receives the favor of people, lithium resource is as fossil energy
Source is equally limited, but the reserves of sodium are far above lithium metal.Sodium rich content in nature, and there is property similar with lithium
Matter, sodium-ion battery equally have many advantages, such as height ratio capacity, and voltage is high, are expected to replace lithium ion battery in certain fields.
But current sodium-ion battery positive material also has many disadvantages, as specific discharge capacity is relatively low, cyclical stability
The deficiencies of poor, remains to be further improved and improves.Therefore, the sodium ion electricity that specific discharge capacity is high and stability is good how is obtained
Pond positive electrode is to solve the problems, such as at present.The present invention can prepare the sodium ion with nanostructure by Prepared By Dual-template Method
Cell positive material, the positive electrode have many advantages, such as specific capacity height, good cycling stability.
Invention content
The present invention is low for current sodium-ion battery positive material specific discharge capacity, cyclical stability is poor problem and provide
A kind of method that Prepared By Dual-template Method prepares high-performance sodium-ion battery positive material, nanoscale sodium-ion battery anode obtained
Material can realize that sodium-ion battery has high charge/discharge capacity, and sodium-ion battery has preferable cyclical stability.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and high-performance sodium ion is prepared using double template
The method of cell positive material, it is characterised in that the specific steps are：
（1）Double template solution, aqueous slkali and the transition metal salt solution of polarity high molecular polymer and surfactant are prepared,
Wherein polarity high molecular polymer is polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, carboxymethyl cellulose, Methyl cellulose
One kind in element, ethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid, polymaleic anhydride or poly-quaternary ammonium salt or
A variety of, surfactant is polyacrylic acid, sodium stearyl sulfate, odium stearate, 4- (2- ethoxys)-piperazine ethanesulfonic acid, alkane
One or more in base glucoside, fatty glyceride, fatty acid sorbitan or polysorbate, alkali is sodium hydroxide, hydrogen-oxygen
One or more in change potassium, sodium carbonate, potassium carbonate or a hydration ammonia, transition metal salt is soluble manganese salt, soluble nickel salt
And soluble cobalt；
（2）The double template solution of polarity high molecular polymer and surfactant is added in reaction kettle, is stirred in 15-70 DEG C
Under conditions of mixing while aqueous slkali is added and transition metal salt solution is reacted, is aged, then cools down after reaction, centrifuges
Washing, then washed with detergent, it is dried after centrifugation and obtains sheet presoma；
（3）Sheet presoma and sodium salt are sintered 6-48h in 600-1200 DEG C after mixing and obtain high-performance sodium-ion battery
Positive electrode, wherein sodium salt are one or more in sodium carbonate, sodium acetate, sodium chloride or sodium nitrate.
Further preferably, the pH value of the double template solution of the polarity high molecular polymer and surfactant is 12-
13, the wherein mass concentration of polarity high molecular polymer is 10-20g/L, and the molar concentration of surfactant is 10-30mol/L.
Further preferably, the soluble manganese salt is one in manganese sulfate, manganese nitrate, manganese chloride, manganese acetate or manganese oxalate
Kind is a variety of, and the soluble nickel salt is one or more, the institute in nickel sulfate, nickel nitrate, nickel chloride, nickel acetate or nickel oxalate
It is one or more in cobaltous sulfate, cobalt nitrate, cobalt chloride, cobalt acetate or cobalt oxalate to state soluble cobalt.
Further preferably, the total mol concentration of transition metal ions is 0.05-0.5mol/L in the transition metal salt,
The molar ratio of middle solubility manganese salt, soluble nickel salt and soluble cobalt is 1-5:1-4:1-2.
Further preferably, the detergent is one or more in deionized water, ethyl alcohol or acetone.
Further preferably, the method for preparing high-performance sodium-ion battery positive material using double template, feature
It is that detailed process is：By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 3:1:The mixing of 1 ratio is dissolved in water and prepares transition gold
Belong to salting liquid, wherein transition metal ions total mol concentration is 0.1mol/L；Sodium hydroxide is dissolved in water preparation molar concentration
The aqueous slkali of 0.2mol/L；Polyvinylpyrrolidone in the double template solution of polarity high molecular polymer and surfactant
The pH value of a concentration of 20g/L, a concentration of 20mmol/L of polyacrylic acid, double-template solution are 13, and 50mL double-template solution is set
In reaction kettle, in 50 DEG C of heating water bath and under conditions of stir, while by 100mL transition metal salt solutions and 100mL alkali solubles
Liquid is added in reaction kettle, reacts 1h, precipitation 1h, centrifugation, ethyl alcohol washing, drying and grinding obtain nanometer sheet presoma；By nanometer
Piece presoma and the sodium carbonate of excess 5wt% calcine 10h in 1000 DEG C after mixing, finally obtained nanoscale sodium-ion battery
Positive electrode.
Sodium-ion battery positive material obtained by the present invention can improve the chemical property of sodium-ion battery, keep sodium electric
Pond cell positive material has higher specific discharge capacity（First discharge specific capacity may be up to 220mAh/g）With preferable cycle
Stability（Specific discharge capacity after recycling 30 times still may be up to 210mAh/g）.
Description of the drawings
Fig. 1 is the XRD diffracting spectrums of sodium-ion battery positive material made from the embodiment of the present invention 1；
Fig. 2 is the SEM figures of sodium-ion battery positive material made from the embodiment of the present invention 1；
Fig. 3 is charging and discharging curve of the sodium-ion battery positive material in 0.1 multiplying power at room temperature made from the embodiment of the present invention 1.
Specific implementation mode
The above of the present 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 the above of the present invention belong to this hair
Bright range.
Embodiment 1
By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 3:1:The mixing of 1 ratio is dissolved in water and prepares transition metal salt solution,
Middle transition metal ions total mol concentration is 0.1mol/L；Sodium hydroxide is dissolved in water and prepares the alkali soluble that molar concentration is 0.2mol/L
Liquid；A concentration of 20g/L of polyvinylpyrrolidone in the double template solution of polarity high molecular polymer and surfactant gathers
The pH value of a concentration of 20mmol/L of acrylic acid, double-template solution are 13,50mL double-template solution are placed in reaction kettle, in water
Under conditions of 50 DEG C of bath heating and stirring, while 100mL transition metal salt solutions and 100mL aqueous slkalis being instilled in reaction kettle,
1h, precipitation 1h are reacted, centrifugation, ethyl alcohol washing, drying and grinding obtain nanometer sheet presoma；By nanometer sheet presoma and excess
The sodium carbonate of 5wt% calcines 10h in 1000 DEG C after mixing, finally obtained nanoscale sodium-ion battery positive material.
Slurry is made in the sodium-ion battery positive material of above-mentioned preparation, is coated on aluminium foil, after 80 DEG C of drying for 24 hours again
Vacuum drying is for 24 hours.With NaClO4For electrolyte, use Celgard 3200 for diaphragm, metallic sodium carries out battery pack as cathode
Dress, button cell model are CR2025.The voltage range of battery constant current charging-discharging test is 1.5-4.2V, test equipment model
Blue electricity CT2001A（Wuhan Jin Nuo Electronics Co., Ltd.s）.The electric discharge specific volume of surveyed positive electrode battery under room temperature in 0.1 multiplying power
Amount is 210mAh/g.
Embodiment 2
By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 1:1:The mixing of 1 ratio is dissolved in water and prepares transition metal salt solution,
Middle transition metal ions total mol concentration is 0.2mol/L；Sodium carbonate is dissolved in water and prepares the alkali soluble that molar concentration is 0.2mol/L
Liquid；A concentration of 10g/L, 4- of carboxymethyl cellulose in the double template solution of polarity high molecular polymer and surfactant
The pH value of a concentration of 10mmol/L of (2- ethoxys)-piperazine ethanesulfonic acid, double-template solution are 12, and 40mL double-template solution is set
In reaction kettle, in 40 DEG C of heating water bath and under conditions of stir, while by 200mL transition metal salt solutions and 200mL alkali solubles
Liquid is added in reaction kettle, reacts 2h, precipitation 1h, centrifugation, deionized water washing, drying and grinding and the sodium nitrate of excess 5wt% in
1000 DEG C of sintering 10h, are finally made nanoscale sodium-ion battery positive material.
Battery makes and test process is with embodiment 1, and gained sodium-ion battery positive material is electric under room temperature in 0.1 multiplying power
The specific discharge capacity in pond is 194mAh/g.
Embodiment 3
By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 4:4:The mixing of 2 ratios is dissolved in water and is configured to transition metal salt solution,
Wherein transition metal ions total mol concentration is 0.2mol/L；Sodium hydroxide is dissolved in water and prepares the alkali that molar concentration is 0.4mol/L
Solution；A concentration of 10g/L of polyacrylamide in the double template solution of polarity high molecular polymer and surfactant, 18
The pH value of a concentration of 30mmol/L of sodium alkyl sulfate, double-template solution are 12, and 50mL double-template solution is placed in reaction kettle,
Reaction kettle is added under conditions of 55 DEG C of heating water bath and stirring, while by 100mL transition metal salt solutions and 100mL aqueous slkalis
In, 2h, precipitation 1h, centrifugation are reacted, deionized water washing is dried and ground with the sodium acetate of excess 5wt% in 1000 DEG C of sintering
Nanoscale sodium-ion battery positive material is finally made in 10h.
Battery makes and test process is with embodiment 1, and gained sodium-ion battery positive material is electric under room temperature in 0.1 multiplying power
The specific discharge capacity in pond is 175.3mAh/g.
Embodiment 4
By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 5:3:The mixing of 2 ratios is dissolved in water and prepares transition metal salt solution,
Middle transition metal ions total mol concentration is 0.5mol/L；Sodium hydroxide is dissolved in water and prepares the alkali soluble that molar concentration is 1.0mol/L
Liquid；A concentration of 20g/L of polyvinyl alcohol, aliphatic acid mountain in the double template solution of polarity high molecular polymer and surfactant
Pears are smooth（Sorbester p17）A concentration of 30mmol/L, the pH value of double-template solution is 13, and 60mL double-template solution is placed in reaction kettle
In, it is added anti-under conditions of 60 DEG C of heating water bath and stirring, while by 150mL transition metal salt solutions and 150mL aqueous slkalis
It answers in kettle, reacts 1h, precipitation 2h, centrifugation, deionized water washing is dried and ground with the sodium carbonate of excess 5wt% in 1100 DEG C of burnings
15h is tied, finally obtained nanoscale sodium-ion battery positive material.
Battery makes and test process is with embodiment 1, and gained sodium-ion battery positive material is electric under room temperature in 0.1 multiplying power
The specific discharge capacity in pond is 162.8mAh/g.
Embodiment above describes the basic principles and main features and advantage of the present invention, and 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 the originals of the present 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 (7)
1. the method for preparing high-performance sodium-ion battery positive material using double template, it is characterised in that the specific steps are：
（1）Double template solution, aqueous slkali and the transition metal salt solution of polarity high molecular polymer and surfactant are prepared,
Wherein polarity high molecular polymer is polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, carboxymethyl cellulose, Methyl cellulose
One kind in element, ethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid, polymaleic anhydride or poly-quaternary ammonium salt or
A variety of, surfactant is polyacrylic acid, sodium stearyl sulfate, odium stearate, 4- (2- ethoxys)-piperazine ethanesulfonic acid, alkane
One or more in base glucoside, fatty glyceride, fatty acid sorbitan or polysorbate, alkali is sodium hydroxide, hydrogen-oxygen
One or more in change potassium, sodium carbonate, potassium carbonate or a hydration ammonia, transition metal salt is soluble manganese salt, soluble nickel salt
And soluble cobalt；
（2）The double template solution of polarity high molecular polymer and surfactant is added in reaction kettle, is stirred in 15-70 DEG C
Under conditions of mixing while aqueous slkali is added and transition metal salt solution is reacted, is aged, then cools down after reaction, centrifuges
Washing, then washed with detergent, it is dried after centrifugation and obtains sheet presoma；
（3）Sheet presoma and sodium salt are sintered 6-48h in 600-1200 DEG C after mixing and obtain high-performance sodium-ion battery
Positive electrode, wherein sodium salt are one or more in sodium carbonate, sodium acetate, sodium chloride or sodium nitrate.
2. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is：The pH value of the double template solution of the polarity high molecular polymer and surfactant is 12-13, and wherein polarity is high
The mass concentration of Molecularly Imprinted Polymer is 10-20g/L, and the molar concentration of surfactant is 10-30mol/L.
3. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is：The pH value of the double template solution of the polarity high molecular polymer and surfactant is 12-13, and wherein polarity is high
The mass concentration of Molecularly Imprinted Polymer is 10-20g/L, and the molar concentration of surfactant is 10-30mol/L.
4. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is：The solubility manganese salt is described to be one or more in manganese sulfate, manganese nitrate, manganese chloride, manganese acetate or manganese oxalate
Soluble nickel salt is one or more, the soluble cobalt in nickel sulfate, nickel nitrate, nickel chloride, nickel acetate or nickel oxalate
It is one or more in cobaltous sulfate, cobalt nitrate, cobalt chloride, cobalt acetate or cobalt oxalate.
5. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is：The total mol concentration of transition metal ions is 0.05-0.5mol/L, wherein soluble manganese in the transition metal salt
The molar ratio of salt, soluble nickel salt and soluble cobalt is 1-5:1-4:1-2.
6. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is：The detergent is one or more in deionized water, ethyl alcohol or acetone.
7. the method according to claim 1 for preparing high-performance sodium-ion battery positive material using double template, special
Sign is that detailed process is：By manganese sulfate, nickel sulfate and cobaltous sulfate according to molar ratio 3:1:The mixing of 1 ratio is dissolved in water and prepares transition
Metal salt solution, wherein transition metal ions total mol concentration are 0.1mol/L；Sodium hydroxide is dissolved in water preparation molar concentration
The aqueous slkali of 0.2mol/L；Polyvinylpyrrolidone in the double template solution of polarity high molecular polymer and surfactant
The pH value of a concentration of 20g/L, a concentration of 20mmol/L of polyacrylic acid, double-template solution are 13, and 50mL double-template solution is set
In reaction kettle, in 50 DEG C of heating water bath and under conditions of stir, while by 100mL transition metal salt solutions and 100mL alkali solubles
Liquid is added in reaction kettle, reacts 1h, precipitation 1h, centrifugation, ethyl alcohol washing, drying and grinding obtain nanometer sheet presoma；By nanometer
Piece presoma and the sodium carbonate of excess 5wt% calcine 10h in 1000 DEG C after mixing, finally obtained nanoscale sodium-ion battery
Positive electrode.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109860540A (en) * | 2018-12-20 | 2019-06-07 | 天津巴莫科技股份有限公司 | A kind of high performance nickel cobalt lithium aluminate cathode material and preparation method thereof |
| CN110429267A (en) * | 2019-08-19 | 2019-11-08 | 河南师范大学 | The method for preparing nanoscale flake sodium-ion battery positive material using multi-template agent |
| CN114804307A (en) * | 2022-03-08 | 2022-07-29 | 曲阜师范大学 | KC pre-intercalated carbon nano sheet (KC-PCN), preparation method, electrode and capacitive deionization |
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| CN110429267A (en) * | 2019-08-19 | 2019-11-08 | 河南师范大学 | The method for preparing nanoscale flake sodium-ion battery positive material using multi-template agent |
| CN114804307A (en) * | 2022-03-08 | 2022-07-29 | 曲阜师范大学 | KC pre-intercalated carbon nano sheet (KC-PCN), preparation method, electrode and capacitive deionization |
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