CN111682191A - Polyion liquid loaded high-dispersion nano antimony-based potassium ion battery cathode material and preparation method thereof - Google Patents
Polyion liquid loaded high-dispersion nano antimony-based potassium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN111682191A CN111682191A CN202010601325.0A CN202010601325A CN111682191A CN 111682191 A CN111682191 A CN 111682191A CN 202010601325 A CN202010601325 A CN 202010601325A CN 111682191 A CN111682191 A CN 111682191A
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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 provides a polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery cathode material and a preparation method thereof, wherein antimony nanoparticles in the cathode material are uniformly dispersed in a polyion liquid network structure, polyion liquid is obtained by cross-linking polymerization of micromolecule ionic liquid, the antimony nanoparticles are obtained by reduction of antimony chloride, and the particle size of the antimony nanoparticles is 5-10 nm. The invention adopts vinyl functionalized imidazolium ionic liquid, divinylbenzene, antimony trichloride and azodiisobutyronitrile as raw materials, adopts absolute ethyl alcohol as a solvent and sodium borohydride as a reducing agent, and adopts a free radical initiated polymerization method to reduce and prepare the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery cathode material.
Description
Technical Field
The invention relates to the technical field of inorganic energy storage materials, in particular to a polyion liquid loaded high-dispersion nano antimony-based potassium ion battery cathode material and a preparation method thereof.
Background
The lithium ion battery is widely applied to portable equipment, new energy automobiles, large-scale energy storage and the like, however, the lithium ion battery exceeds the exploitation limit of lithium resources, and the earth crust abundance of the potassium element is far greater than that of lithium and the electrochemical potential is low, so that the potassium ion battery has a wide development prospect in the field of energy storage. Antimony is an important negative electrode material of a potassium ion battery, however, the antimony has large volume change (about 400%) in the charging and discharging processes due to the large radius of potassium ions, and the capacity fading is fast, so that the application of the antimony in the potassium ion battery is limited.
The currently prepared antimony-based potassium ion battery negative electrode material has the problems of large active material particles and easy pulverization in the charging and discharging process, and meanwhile, the antimony has poor dispersibility in the composite material and the theoretical specific capacity of the material cannot be fully utilized. The preparation methods with good potassium storage performance reported so far generally have the problems of complex process, difficult large-scale preparation and the like, so that the development of the high-dispersion antimony-based nano material with simple process for the cathode material of the potassium ion battery is necessary.
Disclosure of Invention
The invention provides a polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery cathode material and a preparation method thereof.
The technical scheme for realizing the invention is as follows:
a polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material is characterized in that antimony nanoparticles in the negative electrode material are uniformly dispersed in a polyion liquid network structure, polyion liquid is obtained by cross-linking polymerization of micromolecule ionic liquid, the antimony nanoparticles are obtained by reduction of antimony chloride, and the particle size of the antimony nanoparticles is 5-10 nm.
The micromolecular ionic liquid is imidazolium ionic liquid.
The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) dissolving imidazolium ionic liquid, a cross-linking agent and antimony trichloride in absolute ethyl alcohol, and fully stirring and uniformly mixing for a period of time to obtain a mixed solution;
(2) adding an initiator into the mixed solution obtained in the step (1), heating in an oil bath and stirring, and initiating a polymerization reaction by a free radical to obtain a blocky solid material;
(3) dripping sodium borohydride solution into the massive solid material obtained in the step (2), stirring at normal temperature for reaction, and reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying in a vacuum box, and uniformly grinding to obtain the polyion liquid loaded high-dispersion nano antimony-based negative electrode material.
The cation of the imidazolium ionic liquid in the step (1) is imidazolium containing a vinyl functional group, and the anion is at least one of halogen anion, carboxylate radical, nitrate radical or sulfate radical.
The 3-substituent of the cation is at least one of methyl, ethyl, butyl, hexyl, octyl, hydroxyethyl, dihydroxypropyl and long-chain substituent containing hydroxyl or ether bond.
The cross-linking agent in the step (1) is at least one of divinylbenzene, ethylene glycol dimethacrylate and divinyl imidazolium ionic liquid, and the initiator in the step (2) is azobisisobutyronitrile.
The mass ratio of the imidazolium ionic liquid to the cross-linking agent to the antimony trichloride to the initiator is (1-3) to (0.5-3): 3: 1.
in the step (1), the addition amount of the absolute ethyl alcohol accounts for 60-80% of the total mass of the mixed solution, and the time for uniformly mixing is 1-5 h.
The temperature of the oil bath in the step (2) is 65-100 ℃, and the heating and stirring time is 5-15 h; in the step (3), the reduction reaction temperature is 20-30 ℃, and the reaction time is 3-5 h under normal temperature stirring; in the step (4), the vacuum drying temperature is 60-90 ℃, and the drying time is 5-10 h.
The invention has the beneficial effects that:
(1) the particle size of the antimony-based composite material particles obtained by the method is only 5-10 nm, and the antimony-based composite material particles are uniformly dispersed in the polyion liquid, so that the volume change of metal antimony in the charge-discharge process can be effectively relieved, and the electrochemical performance of the material is remarkably improved.
(2) The preparation method is simple in preparation process, easy to control in process and suitable for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is an X-ray diffraction diagram of the polyion liquid-supported high-dispersion nano antimony-based potassium ion battery negative electrode material in example 1 of the present invention.
Fig. 2 is a transmission electron microscope image of the polyion liquid-loaded high-dispersion nano antimony-based potassium ion battery negative electrode material in example 1 of the present invention.
Fig. 3 is a cycle performance curve of the polyion liquid-loaded high-dispersion nano antimony-based potassium ion battery negative electrode material in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The preparation method of the polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) firstly, 2.5 g of 1-butyl-3-vinyl imidazolium bromide, 0.5 g of divinylbenzene and 3.0 g of antimony trichloride are dissolved in 15 mL of absolute ethyl alcohol, and the solution is fully stirred for 2 hours;
(2) adding 1.0 g of azobisisobutyronitrile into the mixed solution, heating in an oil bath at 75 ℃, stirring for 10 hours, and carrying out polymerization reaction to obtain a white massive solid material;
(3) adding excessive sodium borohydride solution, stirring at normal temperature for reaction for 3 h, and reacting Sb3+Fully reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying the black solid powder material in a vacuum box for 8 hours at the temperature of 60 ℃, and uniformly grinding the black solid powder material with an agate mortar to obtain the polyion liquid-loaded high-dispersion nano antimony-based negative electrode material.
The main diffraction peaks recognizable in FIG. 1 all correspond one-to-one to the standard card of antimony metal (JCPDS number 35-0732), and no miscellaneous peaks are present.
In fig. 2, the antimony nanoparticles are uniformly dispersed in the polyion liquid network structure.
Fig. 3 is a cycle performance curve of the polyion liquid-loaded high-dispersion nano antimony-based potassium ion battery negative electrode material in example 1 of the present invention. In the voltage range of 0.01-2.0V, 100 mA g-1Under the current density, the initial reversible specific capacity of the electrode material is 520 mA h g-1After 100 charge-discharge cycles, the capacity retention rate was 61.9%. The composite material shows excellent capacity retention rate and has excellent electrochemical performance.
Example 2
The preparation method of the polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) firstly, 3 g of 1-hydroxyethyl-3-vinylimidazolium nitrate, 0.5 g of divinylbenzene and 3.0 g of antimony trichloride are dissolved in 15 mL of absolute ethyl alcohol, and the solution is fully stirred for 5 hours;
(2) adding 1.0 g of azobisisobutyronitrile into the mixed solution, heating in an oil bath at 100 ℃, stirring for 5 hours, and carrying out polymerization reaction to obtain a white massive solid material;
(3) adding excessive sodium borohydride solution, stirring at normal temperature for reaction for 3 h, and reacting Sb3+Fully reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying the black solid powder material in a vacuum box for 10 hours at the temperature of 60 ℃, and uniformly grinding the black solid powder material with an agate mortar to obtain the polyion liquid-loaded high-dispersion nano antimony-based negative electrode material.
Example 3
The preparation method of the polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) firstly, 1 g of 1-hexyl-3-vinyl imidazolium sulfate, 3 g of ethylene glycol dimethacrylate and 3.0 g of antimony trichloride are dissolved in 15 mL of absolute ethyl alcohol, and the solution is fully stirred for 1 h;
(2) adding 1.0 g of azobisisobutyronitrile into the mixed solution, heating in an oil bath at 65 ℃, stirring for 15 hours, and carrying out polymerization reaction to obtain a white massive solid material;
(3) adding excessive sodium borohydride solution, stirring at normal temperature for 5h, and reacting Sb3+Fully reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying the black solid powder material in a vacuum box for 5 hours at the temperature of 90 ℃, and uniformly grinding the black solid powder material with an agate mortar to obtain the polyion liquid-loaded high-dispersion nano antimony-based negative electrode material.
Example 4
The preparation method of the polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) firstly, 2 g of 1-dihydroxypropyl-3-vinyl imidazolium carboxylate, 1.5 g of divinyl imidazolium and 3.0 g of antimony trichloride are dissolved in 15 mL of absolute ethyl alcohol, and the solution is fully stirred for 3 hours;
(2) adding 1.0 g of azobisisobutyronitrile into the mixed solution, heating in an oil bath at 85 ℃, stirring for 10 hours, and carrying out polymerization reaction to obtain a white massive solid material;
(3) adding excessive sodium borohydride solution, stirring at normal temperature for 5h, and reacting Sb3+Fully reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying the black solid powder material in a vacuum box at 75 ℃ for 7 hours, and uniformly grinding the black solid powder material with an agate mortar to obtain the polyion liquid-loaded high-dispersion nano antimony-based negative electrode material.
Example 5
The preparation method of the polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material comprises the following steps:
(1) firstly, 2.0 g of 1-ethyl-3-vinyl imidazolium chloride salt, 2.0 g of ethylene glycol dimethacrylate and 3.0 g of antimony trichloride are dissolved in 15 mL of absolute ethyl alcohol, and the solution is fully stirred for 1 h;
(2) adding 1.0 g of azobisisobutyronitrile into the mixed solution, heating in an oil bath at 85 ℃, stirring for 8 hours, and carrying out polymerization reaction to obtain a white massive solid material;
(3) adding excessive sodium borohydride solution, stirring at normal temperature for 5h, and reacting Sb3+Fully reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying the black solid powder material in a vacuum box for 7 hours at the temperature of 80 ℃, and uniformly grinding the black solid powder material with an agate mortar to obtain the polyion liquid-loaded high-dispersion nano antimony-based negative electrode material.
When the composite material is used as the negative electrode material of the potassium ion battery, on one hand, the uniformly dispersed nano antimony is not easy to agglomerate in the embedding and removing processes of potassium ions, so that the stable cycle performance of the potassium ion battery is ensured; on the other hand, the polyion liquid can play a role in buffering severe volume change of antimony in the charging and discharging processes, and stability of the material is guaranteed.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A polyion liquid loaded high-dispersion nanometer antimony-based potassium ion battery negative electrode material is characterized in that: antimony nanoparticles in the negative electrode material are uniformly dispersed in a polyion liquid network structure, the polyion liquid is obtained by cross-linking polymerization of small molecular ionic liquid, the antimony nanoparticles are obtained by reduction of antimony chloride, and the particle size of the antimony nanoparticles is 5-10 nm.
2. The polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material as claimed in claim 1, characterized in that: the micromolecular ionic liquid is imidazolium ionic liquid.
3. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material as claimed in claim 1 or 2, is characterized by comprising the following steps:
(1) dissolving imidazolium ionic liquid, a cross-linking agent and antimony trichloride in absolute ethyl alcohol, and fully stirring and uniformly mixing for a period of time to obtain a mixed solution;
(2) adding an initiator into the mixed solution obtained in the step (1), heating in an oil bath and stirring, and initiating a polymerization reaction by a free radical to obtain a blocky solid material;
(3) dripping sodium borohydride solution into the massive solid material obtained in the step (2), stirring at normal temperature for reaction, and reducing to obtain a black solid powder material;
(4) soaking and washing the obtained black solid powder material with deionized water, drying in a vacuum box, and uniformly grinding to obtain the polyion liquid loaded high-dispersion nano antimony-based negative electrode material.
4. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 3, characterized by comprising the following steps: the cation of the imidazolium ionic liquid in the step (1) is imidazolium containing a vinyl functional group, and the anion is at least one of halogen anion, carboxylate radical, nitrate radical or sulfate radical.
5. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 4, characterized by comprising the following steps: the 3-substituent of the cation is at least one of methyl, ethyl, butyl, hexyl, octyl, hydroxyethyl, dihydroxypropyl and long-chain substituent containing hydroxyl or ether bond.
6. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 3, characterized by comprising the following steps: the cross-linking agent in the step (1) is at least one of divinylbenzene, ethylene glycol dimethacrylate and divinyl imidazolium ionic liquid, and the initiator in the step (2) is azobisisobutyronitrile.
7. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 3, characterized by comprising the following steps: the mass ratio of the imidazolium ionic liquid to the cross-linking agent to the antimony trichloride to the initiator is (1-3) to (0.5-3): 3: 1.
8. the preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 3, characterized by comprising the following steps: in the step (1), the addition amount of the absolute ethyl alcohol accounts for 60-80% of the mass of the mixed solution, and the stirring and mixing time is 1-5 h.
9. The preparation method of the polyion liquid loaded high-dispersion nano antimony-based potassium ion battery negative electrode material according to claim 3, characterized by comprising the following steps: the temperature of the oil bath in the step (2) is 65-100 ℃, and the heating and stirring time is 5-15 h; in the step (3), the reduction reaction temperature is 20-30 ℃, and the reaction time is 3-5 h under normal temperature stirring; in the step (4), the vacuum drying temperature is 60-90 ℃, and the drying time is 5-10 h.
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