CN112072081A - MXene material loaded with cobalt molybdenum sulfide and preparation method thereof - Google Patents
MXene material loaded with cobalt molybdenum sulfide and preparation method thereof Download PDFInfo
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- CN112072081A CN112072081A CN202010677167.7A CN202010677167A CN112072081A CN 112072081 A CN112072081 A CN 112072081A CN 202010677167 A CN202010677167 A CN 202010677167A CN 112072081 A CN112072081 A CN 112072081A
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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
- H01M4/362—Composites
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 embodiment of the invention provides a cobalt molybdenum sulfide loaded MXene material and a preparation method thereof, wherein the preparation method comprises the following steps: adding molybdenum salt into soluble cobalt salt aqueous solution and vulcanizing agent aqueous solution, and uniformly stirring; adding a single-layer MXene aqueous solution, uniformly stirring and performing ultrasonic treatment; carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid; and freeze-drying the obtained solid to obtain the MXene material loaded with the cobalt molybdenum sulfide. The micro-structure of the cobalt molybdenum sulfide loaded MXene material provided by the embodiment of the invention is that pellets and sheets or rods alternately exist, the sheets and the rods are embedded around the pellets, the ion conduction effect is effectively improved, and the essence is that cobalt disulfide is used as a matrix, and the MXene material and molybdenum element are doped, so that the volume effect in the charging and discharging process is effectively inhibited, and the multiplying power performance and the cycle performance of the material are greatly improved. The invention has simple manufacturing method, low cost and high yield, and is suitable for industrial batch production.
Description
Technical Field
The invention relates to the field of lithium ion battery cathode materials, in particular to a cobalt molybdenum sulfide loaded MXene material and a preparation method thereof.
Background
With the increasing prominence of the problems of energy crisis, environmental pollution and the like, sustainable energy development is developed, the establishment of a low-carbon society becomes a critical need, and the lithium ion battery is concerned as a novel high-energy green battery. The lithium ion battery is developed on the basis of a secondary lithium battery, not only preserves the main advantages of high voltage and high capacity of the lithium battery, but also has the remarkable characteristics of long cycle life and good safety performance, and has wide application prospects in various aspects such as portable electronic equipment, electric automobiles, space technology, national defense industry and the like.
The negative electrode of the lithium ion battery is formed by uniformly coating a paste adhesive prepared from a negative electrode active material, a binder and an additive on two sides of a copper foil, drying and rolling. There are two types of lithium ion battery negative electrode materials that are currently commercialized. One type is a carbon material such as natural graphite, synthetic graphite, mesocarbon microbeads (MCMB), and the like. Compared with natural graphite, the MCMB has superior electrochemical performance, and the main reason is that the outer surfaces of the particles are all edge surfaces of a graphite structure, the reaction activity is uniform, a stable SEI film is easy to form, and lithium is easy to be inserted and extracted. The other is Si cathode, Sn base alloy, however, the alloy cathode material has the problems of high capacity accompanied by high volume change and pulverization along with volume expansion.
Disclosure of Invention
The invention provides a cobalt molybdenum sulfide loaded MXene material and a preparation method thereof, aiming at solving the technical problem that the existing lithium battery cathode material is not beneficial to use.
The embodiment of the invention provides a preparation method of a cobalt molybdenum sulfide loaded MXene material, which comprises the following steps:
s1, adding molybdenum salt into the soluble cobalt salt aqueous solution and the vulcanizing agent aqueous solution, and uniformly stirring;
s2, adding a single-layer MXene aqueous solution, stirring uniformly and performing ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the MXene material loaded with the cobalt molybdenum sulfide.
Further, the molybdenum salt includes one or more of sodium molybdate, potassium molybdate, ammonium molybdate, lithium molybdate, molybdenum phosphate, molybdenum dialkyldithiocarbamate, molybdenum sulfate, molybdenum acetate, molybdenum nitrate, and molybdenum dialkyldithiophosphate.
Further, the soluble cobalt salt in the aqueous solution of the soluble cobalt salt comprises one or more of cobalt butyrate, cobalt sulfate, cobalt propionate, cobalt nitrate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride, cobalt naphthenate and cobalt acetate.
Further, the vulcanizing agent in the vulcanizing agent aqueous solution comprises one or more of sodium sulfide, potassium sulfide, thiopropionic amine, thioacetamide and L-cysteine.
Further, the mass ratio of the molybdenum salt, the soluble cobalt salt, the single-layer MXene aqueous solution and the vulcanizing agent in the vulcanizing agent aqueous solution is (0.1-1.5): (0.1-1.5): (1-8): 1.
further, the concentration of the soluble cobalt salt water solution is 0.05-0.5 mol/L; the concentration of the vulcanizing agent aqueous solution is 0.05-0.5 mol/L, and the concentration of the single-layer MXene aqueous solution is 0.05-1.0 mol/L.
Further, in the steps S1 and S2, the stirring time is 10-100 min; in the step S4, the freeze drying time is 10-30 h; the temperature of freeze drying is-57 to-29 ℃.
On the other hand, the invention also provides an MXene material loaded with the cobalt molybdenum sulfide, and the MXene material loaded with the cobalt molybdenum sulfide is prepared by the preparation method.
The invention has the beneficial effects that: the MXene material loaded by the cobalt molybdenum sulfide prepared by the embodiment of the invention can effectively improve the rate capability and the cycle performance of the battery, and can effectively inhibit the volume expansion of the battery in the charging and discharging processes at the early stage; the rate of capacity fading is weakened, and the coulomb effect is improved. The MXene material loaded by the cobalt molybdenate has a spherical and flaky or rodlike microstructure which alternately exists, the flaky and rodlike shapes are embedded around the spherical shape, the ion conduction effect is effectively improved, cobalt disulfide is used as a matrix, and the MXene material and molybdenum element are doped, so that the volume effect in the charge-discharge process is effectively inhibited, and the rate capability and the cycle performance of the MXene material can be greatly improved. The invention has simple manufacturing method, low cost and high yield, and is suitable for industrial batch production.
Detailed Description
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," and the like are used merely for convenience in describing and simplifying the description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be considered as limiting.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The present invention will be described in further detail with reference to the following embodiments.
The embodiment of the invention provides a preparation method of a cobalt molybdenum sulfide loaded MXene material, which comprises the following steps:
s1, adding molybdenum salt into the soluble cobalt salt aqueous solution and the vulcanizing agent aqueous solution, and uniformly stirring;
s2, adding a single-layer MXene aqueous solution, stirring uniformly and performing ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the MXene material loaded with the cobalt molybdenum sulfide.
The MXene material loaded by the cobalt molybdenum sulfide not only further increases the transmission and conduction performance of electrons; and capacity attenuation in the charging and discharging process can be effectively inhibited in the early stage of the lithium battery, the cycle performance is greatly improved, and the stability is further improved.
Specifically, the preparation method comprises the following specific steps:
respectively dissolving soluble cobalt salt and a vulcanizing agent in deionized water to respectively obtain a solution A and a solution B; pouring the solution B into the solution A, and uniformly stirring to obtain a solution C;
adding molybdenum salt into deionized water for dissolving, adding the molybdenum salt into the solution C, and uniformly stirring to obtain a solution D;
pouring the monolayer MXene aqueous solution into the solution D, and uniformly stirring to obtain a solution E;
the solution E is subjected to ultrasonic treatment and then poured into a stainless steel reaction kettle, is subjected to hydrothermal reaction at the temperature of 100-300 ℃ for 15-30 hours, is cooled along with a furnace, is taken out, and is subjected to suction filtration to obtain a solid F; and (4) freeze-drying the solid F to obtain the cobalt molybdenum sulfide loaded MXene material.
In the method, the volume ratio of the mass of the soluble cobalt salt to the volume of the deionized water is (1-10): 1 mg/mL; the mass ratio of the vulcanizing agent to the deionized water is (5-35): 10 mg/mL; the mass ratio of the tin salt to the deionized water is (5-25): 5 mg/mL.
The MXene material loaded by the cobalt molybdenum sulfide prepared by the embodiment of the invention can effectively improve the rate capability and the cycle performance of the battery, and can effectively inhibit the volume expansion of the battery in the charging and discharging processes at the early stage; the rate of capacity fading is weakened, and the coulomb effect is improved. The MXene material loaded by the cobalt molybdenate has a spherical and flaky or rodlike microstructure which alternately exists, the flaky and rodlike shapes are embedded around the spherical shape, the ion conduction effect is effectively improved, cobalt disulfide is used as a matrix, and the MXene material and molybdenum element are doped, so that the volume effect in the charge-discharge process is effectively inhibited, and the rate capability and the cycle performance of the MXene material can be greatly improved. The invention has simple manufacturing method, low cost and high yield, and is suitable for industrial batch production.
In an alternative embodiment, the molybdenum salt comprises one or more of sodium molybdate, potassium molybdate, ammonium molybdate, lithium molybdate, molybdenum phosphate, molybdenum dialkyldithiocarbamate, molybdenum sulfate, molybdenum acetate, molybdenum nitrate, and molybdenum dialkyldithiophosphate.
Further, the soluble cobalt salt in the aqueous solution of the soluble cobalt salt comprises one or more of cobalt butyrate, cobalt sulfate, cobalt propionate, cobalt nitrate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride, cobalt naphthenate and cobalt acetate.
Further, the vulcanizing agent in the vulcanizing agent aqueous solution comprises one or more of sodium sulfide, potassium sulfide, thiopropionic amine, thioacetamide and L-cysteine.
Further, the mass ratio of the molybdenum salt, the soluble cobalt salt, the single-layer MXene aqueous solution and the vulcanizing agent in the vulcanizing agent aqueous solution is (0.1-1.5): (0.1-1.5): (1-8): 1.
further, the concentration of the soluble cobalt salt water solution is 0.05-0.5 mol/L; the concentration of the vulcanizing agent aqueous solution is 0.05-0.5 mol/L, and the concentration of the single-layer MXene aqueous solution is 0.05-1.0 mol/L.
Further, in the steps S1 and S2, the stirring time is 10-100 min; in the step S4, the freeze drying time is 10-30 h; the temperature of freeze drying is-57 to-29 ℃.
On the other hand, the invention also provides an MXene material loaded with the cobalt molybdenum sulfide, and the MXene material loaded with the cobalt molybdenum sulfide is prepared by the preparation method.
The MXene material loaded by the cobalt molybdenum sulfide prepared by the embodiment of the invention can effectively improve the rate capability and the cycle performance of the battery, and can effectively inhibit the volume expansion of the battery in the charging and discharging processes at the early stage; the rate of capacity fading is weakened, and the coulomb effect is improved. The MXene material loaded by the cobalt molybdenate has a spherical and flaky or rodlike microstructure which alternately exists, the flaky and rodlike shapes are embedded around the spherical shape, the ion conduction effect is effectively improved, cobalt disulfide is used as a matrix, and the MXene material and molybdenum element are doped, so that the volume effect in the charge-discharge process is effectively inhibited, and the rate capability and the cycle performance of the MXene material can be greatly improved. The invention has simple manufacturing method, low cost and high yield, and is suitable for industrial batch production.
The specific embodiment is as follows:
example 1
1. Adding 0.253g of CoCl2 hexahydrate into 10ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.244g of L-cysteine into 150ml of deionized water, stirring and dissolving to obtain a transparent solution, and marking as a solution B;
3. adding the solution B into the solution A, and stirring for 13min to obtain a yellow-brown solution which is marked as solution C;
4. adding 2.235g of sodium molybdate into 20ml of deionized water, stirring and dissolving completely, then adding into the solution C, and stirring for 15min to obtain a khaki solution which is marked as solution D;
5. adding 5.98g of MXene aqueous solution into the solution D, stirring for 23 mm to obtain a black solution, and marking as a solution E;
6. the solution E is subjected to ultrasonic treatment for 15min and then poured into a stainless steel reaction kettle, then placed in a heating furnace for hydrothermal reaction at 210 ℃ for 24h, cooled along with the furnace, and subjected to suction filtration for 4 times to obtain a black solid F;
7. and (3) drying the solid F in a freeze dryer for 24 hours to obtain the cobalt molybdenum sulfide loaded MXene material.
Example 2
1. Adding 0.231 g of CoCl2 hexahydrate into 10ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.223 g of L-cysteine into 20ml of deionized water, stirring and dissolving to obtain a transparent solution, and marking as a solution B;
3. pouring the solution B into the solution A, and stirring for 20 min to obtain a yellow-brown solution which is marked as solution C;
4. adding 2.228 g of ammonium molybdate into 20ml of deionized water, stirring and dissolving completely, then adding into the solution C, and stirring for 13min to obtain a khaki solution which is marked as solution D;
5. adding 6.0g of single-layer MXene aqueous solution into the solution D, and stirring for 15 mim to obtain a black solution marked as solution E;
6. the solution E is subjected to ultrasonic treatment for 30 min and then poured into a stainless steel reaction kettle, then placed in a heating furnace for hydrothermal reaction at 200 ℃ for 26h, cooled along with the furnace, and subjected to suction filtration for 5 times to obtain a black solid F;
7. and (3) drying the solid F in a freeze dryer for 24 hours to obtain the cobalt molybdenum sulfide loaded MXene material.
Example 3
1. Adding 0.235g of CoCl2 hexahydrate into 15 ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.313g of L-cysteine into 30 ml of deionized water, stirring and dissolving to obtain a transparent solution, and marking as a solution B;
3. pouring the solution B into the solution A, and stirring for 10 min to obtain a yellow-brown solution which is marked as solution C;
4. adding 0.328g of sodium molybdate into 15 ml of deionized water, stirring and dissolving completely, then adding into the solution C, stirring for 20 min to obtain a khaki solution, and marking as a solution D;
5. adding 6.0g of single-layer MXene aqueous solution into the solution D, and stirring for 20 mim to obtain a black solution marked as solution E;
6. the solution E is subjected to ultrasonic treatment for 15min and then poured into a stainless steel reaction kettle, then placed in a heating furnace for hydrothermal reaction at 200 ℃ for 20h, cooled along with the furnace, and subjected to suction filtration for 8 times to obtain a black solid F;
7. and (3) drying the solid F in a freeze dryer for 20 hours to obtain the cobalt molybdenum sulfide loaded MXene material.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.
Claims (8)
1. The preparation method of the MXene material loaded with the cobalt molybdenum sulfide is characterized by comprising the following steps of:
s1, adding molybdenum salt into the soluble cobalt salt aqueous solution and the vulcanizing agent aqueous solution, and uniformly stirring;
s2, adding a single-layer MXene aqueous solution, stirring uniformly and performing ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the MXene material loaded with the cobalt molybdenum sulfide.
2. The method of preparing the cobalt thiomolybdate supported MXene material of claim 1, wherein the molybdenum salt comprises one or more of sodium molybdate, potassium molybdate, ammonium molybdate, lithium molybdate, molybdenum phosphate, molybdenum dialkyldithiocarbamate, molybdenum sulfate, molybdenum acetate, molybdenum nitrate, and molybdenum dialkyldithiophosphate.
3. The method for preparing the MXene material loaded with cobalt thiomolybdate of claim 1, wherein the soluble cobalt salt in the aqueous solution of the soluble cobalt salt comprises one or more of cobalt butyrate, cobalt sulfate, cobalt propionate, cobalt nitrate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride, cobalt naphthenate, and cobalt acetate.
4. The method for preparing the MXene material loaded with cobalt thiomolybdate of claim 1, wherein the sulfiding agent in the sulfiding agent aqueous solution comprises one or more of sodium sulfide, potassium sulfide, amine thiopropionate, thioacetamide and L-cysteine.
5. The method for preparing the MXene material loaded with the cobalt molybdenate according to claim 1, wherein the mass ratio of the molybdenum salt, the soluble cobalt salt, the single-layer MXene aqueous solution to the vulcanizing agent in the vulcanizing agent aqueous solution is (0.1-1.5): (0.1-1.5): (1-8): 1.
6. the method for preparing the MXene material loaded with the cobalt molybdenum sulfide as claimed in claim 1, wherein the concentration of the soluble cobalt salt aqueous solution is 0.05-0.5 mol/L; the concentration of the vulcanizing agent aqueous solution is 0.05-0.5 mol/L, and the concentration of the single-layer MXene aqueous solution is 0.05-1.0 mol/L.
7. The method for preparing the MXene material loaded with the cobalt molybdenum sulfide as claimed in claim 1, wherein in the steps S1 and S2, the stirring time is 10-100 min; in the step S4, the freeze drying time is 10-30 h; the temperature of freeze drying is-57 to-29 ℃.
8. The MXene material loaded with the cobalt molybdenum sulfide is characterized by being prepared by the preparation method of any one of claims 1 to 7.
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Application publication date: 20201211 |