CN110911684B - Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof - Google Patents
Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of lithium ion battery cathode materials, and discloses antimony-doped cobalt disulfide-loaded graphene and a preparation method and application thereof. The microstructure of the antimony-doped cobalt disulfide-loaded graphene negative electrode material has a regular columnar structure; the material has excellent charge-discharge cycle performance and conductivity, high rate performance, high stability and high adhesion degree with copper foil, and can be applied to the field of lithium ion batteries as a negative electrode material.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery cathode materials, and particularly relates to antimony-doped cobalt disulfide-loaded graphene and a preparation method and application thereof.
Background
Lithium ion batteries have been applied in large scale in the fields of consumer electronics, electric vehicles, and the like, and are emerging in the field of large-scale energy storage. High energy density, high power density, long life, etc. are basic requirements for lithium ion batteries. The lithium ion battery mainly comprises five major parts, namely a positive electrode material, a negative electrode material, an electrolyte, a diaphragm and a current collector; the performance of the cathode material, which is used as a main place for storing lithium ions in the current lithium ion battery, directly affects the performance of the battery, so that the cathode material plays a decisive role in the performance of the lithium ion battery.
The negative electrode material is a carrier of lithium ions and electrons during the charging process of the battery and plays a role in storing and releasing energy. In the cost of the battery, the negative electrode material accounts for about 5-15 percent and is one of the important raw materials of the lithium ion battery; the global lithium battery cathode material sales amount is about more than ten tons, the production places are mainly China and Japan, and the demand for the cathode material also presents an increasing state according to the increasing trend of energy automobiles at the present stage; at present, the cathode materials of the global lithium batteries still mainly comprise natural/artificial graphite, and novel cathode materials such as MCMB, lithium titanate, silicon-based cathodes, metallic lithium, sulfur-based compounds, cobalt-based compounds and the like are also rapidly growing.
The cobalt disulfide is used as one of the lithium ion battery electrode materials, the theoretical specific capacity of the cobalt disulfide is up to 870mAh/g, which is more than twice of that of the graphite cathode material, and the cobalt disulfide has the characteristics of excellent conductivity, good stability, environmental friendliness, abundant reserves, low price and the like, and is very suitable for being used as the cathode material of the next generation of high-energy lithium ion battery cell; however, the large-scale use of the material is also troubled by the drastic volume change during charge and discharge and the rapid capacity fade brought by the unstable SEI film.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide the antimony-doped cobalt disulfide-loaded graphene, which not only can effectively inhibit the volume expansion effect generated in the charging and discharging process and increase the transmission and conduction performance of electrons, but also can reduce the rate of capacity attenuation; in addition, the antimony-doped cobalt disulfide-loaded graphene negative electrode material has excellent cycle performance and rate performance and high stability.
The invention also aims to provide the preparation method of the antimony-doped cobalt disulfide-loaded graphene, which is simple to manufacture, low in cost, high in yield and suitable for industrial batch production.
The invention also aims to provide application of the antimony-doped cobalt disulfide-loaded graphene,
in order to achieve the purpose, the invention is realized by the following technical scheme:
the antimony-doped cobalt disulfide-loaded graphene is prepared by adding a graphene hydrate into a mixed aqueous solution of soluble cobalt salt and a vulcanizing agent, stirring, pouring into an organic solvent of antimony salt, then carrying out ultrasonic treatment, reacting the obtained antimony-doped mixed solution at 100-300 ℃, then cooling along with a furnace, carrying out suction filtration, and carrying out freeze drying treatment.
Preferably, the antimony salt is more than one of antimony nitrate, antimony sulfate, antimony bromide, antimony trichloride, antimony sulfide, antimony pentachloride or antimony hydroxide.
Preferably, the organic solvent is one or more of methanol, ethanol, toluene, isopropanol, propylene oxide, styrene, perchloroethylene, trichloroethylene, ethylene glycol ether, triethanolamine, benzene, xylene, pentane, hexane, octane, cyclohexane, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichlorobenzene, dichloromethane, diethyl ether, propylene oxide, methyl acetate, ethyl acetate, propyl acetate, acetone, methyl butanone, methyl isobutyl ketone, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, acetonitrile, pyridine or phenol.
Preferably, the soluble cobalt salt is one or more of cobalt chloride, cobalt acetate, cobalt sulfate, cobalt nitrate or hydrates of the above salts; the vulcanizing agent is more than one of sodium sulfide, thioacetamide or L-cysteine.
Preferably, the mass ratio of the antimony salt to the vulcanizing agent is (0.1-1.5): 1; the mass ratio of the graphene hydrate to the soluble cobalt salt to the vulcanizing agent is (1-10): (0.1-1.2): 1.
preferably, the concentration of the antimony salt in the organic solvent is 0.01-0.5 mol/L; the concentration of the soluble cobalt salt in the mixed water solution of the soluble cobalt salt and the vulcanizing agent is 0.01-0.5 mol/L, and the concentration of the vulcanizing agent is 0.01-0.5 mol/L; the concentration of the graphene hydrate is 0.01-0.7 mol/L.
Preferably, the reaction time is 12-48 h, and the stirring time is 10-100 min; the freeze drying time is 6-32 hours; the temperature of the freeze drying is-57 to-30 ℃.
The preparation method of the antimony-doped cobalt disulfide-loaded graphene comprises the following steps:
s1, respectively dissolving soluble cobalt salt and a vulcanizing agent in deionized water to obtain a solution A and a solution B;
s2, adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
s3, dripping graphene hydrate into the solution C, and uniformly stirring to obtain a solution D;
s4, adding antimony salt into an organic solvent to dissolve to obtain a solution E;
s5, adding the solution D into the solution E, and uniformly stirring to obtain a solution F; carrying out ultrasonic treatment on the solution F, carrying out hydrothermal reaction at 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid G; and (4) freeze-drying the solid G to obtain the antimony-doped cobalt disulfide-loaded graphene.
Preferably, in the step S1, the ratio of the mass of the soluble cobalt salt to the volume of the deionized water is (10-20) mg: 1 mL; the mass ratio of the vulcanizing agent to the deionized water is (1-10) mg: 25 mL.
The antimony-doped cobalt disulfide-loaded graphene is applied to the field of lithium ion batteries as a negative electrode material.
Compared with the prior art, the invention has the following beneficial effects:
1. the antimony-doped cobalt disulfide-loaded graphene contains a regular columnar microstructure, can improve the conduction rate of electrons, and has good conductivity, excellent rate performance and cycle performance.
2. According to the antimony-doped cobalt disulfide-loaded graphene, antimony salt, graphene and cobalt disulfide are firstly combined, so that the phenomena of volume expansion and capacity fading over-speed of a battery in the charging and discharging processes are effectively inhibited, the capacity fading rate of the battery in the charging and discharging processes is effectively reduced due to the addition of antimony salt, and the rate capability and the cycle performance of the battery are improved.
3. The antimony-doped cobalt disulfide-loaded graphene disclosed by the invention has excellent charge-discharge cycle performance and conductivity, high rate performance and high stability. The antimony-doped cobalt disulfide-loaded graphene has high adhesion degree with a copper foil current collector, almost completely avoids foil stripping, and can be applied to the field of lithium ion batteries as a negative electrode material.
Drawings
Fig. 1 is a scanning electron microscope picture of antimony-doped cobalt disulfide-loaded graphene prepared in example 1.
Fig. 2 is a rate charge and discharge curve of the antimony doped cobalt disulfide loaded graphene prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. Those skilled in the art should understand that they can make various changes, substitutions and alterations herein without departing from the scope of the invention.
Example 1
1. 0.259g of CoCl hexahydrate2Adding deionized H with 20ml2Stirring and dissolving the mixture in a beaker of O to obtain a pink solution A;
2. 0.275g of L-cysteine was added to a solution containing 30ml of deionized H2Stirring and dissolving the mixture in a beaker of O to obtain a transparent solution B;
3. adding the solution B into the solution A, and stirring for 30min to obtain a yellow-brown solution C;
4. adding 10g of graphene hydrate into the solution C, and stirring for 25min to obtain a black solution D;
5. 0.294g of SbCl3Adding the mixture into 30ml of absolute ethyl alcohol, and stirring and dissolving to obtain a transparent solution E;
6. adding the solution D into the solution E, and uniformly stirring for 25min to obtain a black solution F; carrying out ultrasonic treatment on the obtained solution F for 10min, pouring the solution F into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a heating furnace, carrying out hydrothermal reaction at 220 ℃ for 24h, cooling the solution along with the furnace, and carrying out suction filtration for 6 times to obtain a black solid G; and (3) drying the solid G in a freeze dryer for 26 hours to obtain the antimony-doped cobalt disulfide-loaded graphene.
Fig. 1 is a scanning electron microscope picture of antimony-doped cobalt disulfide-loaded graphene prepared in example 1. As can be seen from fig. 1, a regular columnar structure exists in the microstructure of the antimony-doped cobalt disulfide-loaded graphene, which indicates that the material has good conductivity. Fig. 2 is a rate charge and discharge curve of the antimony doped cobalt disulfide loaded graphene prepared in example 1. As can be seen from fig. 2, the rate capability is increased after being decreased, and after 100 cycles, the charging specific capacity is still about 340mAh/g, which indicates that the antimony-doped cobalt disulfide-loaded graphene has excellent rate capability.
Example 2
1. 0.315g of CoCl hexahydrate230ml of deionized H were added2In O, stirring and dissolving to obtain pink solution A;
2. 0.237g of L-cysteine was added to a solution containing 30ml of deionized H2Stirring and dissolving in O to obtain a transparent solution B;
3. adding the solution B into the solution A, and stirring for 20min to obtain a yellow-brown solution C;
4. adding 8g of graphene hydrate into the solution C, and stirring for 25min to obtain a black solution D;
5. 0.369g of SbCl3Adding the mixture into 40ml of absolute ethyl alcohol, and stirring and dissolving to obtain a transparent solution E;
6. adding the solution D into the solution E, and uniformly stirring for 20min to obtain a black solution F; ultrasonically treating the obtained solution F for 15min, pouring the solution F into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a heating furnace, carrying out hydrothermal reaction at 240 ℃ for 20h, cooling the solution along with the furnace, and carrying out suction filtration for 4 times to obtain a black solid G; and (3) drying the solid G in a freeze dryer for 24 hours to obtain the antimony-doped cobalt disulfide-loaded graphene.
Example 3
1. 0.238g of CoCl hexahydrate2Adding deionized H containing 15ml2Stirring and dissolving the mixture in a beaker of O to obtain a pink solution A;
2. 0.242g of L-cysteine was added to the flask30ml deionised H2Stirring and dissolving the mixture in a beaker of O to obtain a transparent solution B;
3. adding the solution A into the solution B, and stirring for 30min to obtain a yellow-brown solution C;
4. adding 8g of graphene hydrate into the solution C, and stirring for 20min to obtain a black solution D;
5. 0.224g of SbCl3Adding the mixture into 20ml of absolute ethyl alcohol, and stirring and dissolving to obtain a transparent solution E;
6. adding the solution D into the solution E, and uniformly stirring for 25min to obtain a black solution F; ultrasonically treating the obtained solution F for 5min, pouring the solution F into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a heating furnace, carrying out hydrothermal reaction at 210 ℃ for 20h, cooling the solution along with the furnace, and carrying out suction filtration for 4 times to obtain a black solid G; and (3) drying the solid G in a freeze dryer for 24 hours to obtain the antimony-doped cobalt disulfide-loaded graphene.
Example 4
The difference from example 1 is that: in the step 1, cobalt salt is cobalt acetate, a vulcanizing agent in the step 2 is thioacetamide, and antimony salt in the step 5 is antimony sulfate.
Example 5
The difference from example 2 is that: in the step 1, cobalt salt is cobalt sulfate, in the step 2, a vulcanizing agent is sodium sulfide, and in the step 5, antimony salt is antimony bromide.
Example 6
The difference from example 3 is that: in the step 1, cobalt salt is cobalt nitrate, a vulcanizing agent in the step 2 is thioacetamide, and antimony salt in the step 5 is antimony sulfide.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. The antimony-doped cobalt disulfide-loaded graphene for the lithium ion battery is characterized in that graphene hydrate is added into a mixed aqueous solution of soluble cobalt salt and vulcanizing agent L-cysteine, the mixed aqueous solution is stirred and poured into an organic solvent of antimony salt, then ultrasonic treatment is carried out, the obtained antimony-doped mixed solution is subjected to reaction at 100-300 ℃, and then furnace cooling, suction filtration and freeze drying treatment are carried out to obtain the antimony-doped cobalt disulfide-loaded graphene; the mass ratio of the antimony salt to the vulcanizing agent is (0.1-1.5): 1; the mass ratio of the graphene hydrate to the soluble cobalt salt to the vulcanizing agent is (1-10): (0.1-1.2): 1; the antimony-doped cobalt disulfide-loaded graphene contains a regular columnar microstructure; the freeze drying time is 6-32 hours; the temperature of the freeze drying is-57 to-30 ℃; the concentration of the antimony salt in the organic solvent is 0.01-0.5 mol/L; the concentration of the soluble cobalt salt in the mixed water solution of the soluble cobalt salt and the vulcanizing agent L-cysteine is 0.01-0.5 mol/L, and the concentration of the vulcanizing agent L-cysteine is 0.01-0.5 mol/L; the concentration of the graphene hydrate is 0.01-0.7 mol/L.
2. The antimony-doped cobalt disulfide-loaded graphene for a lithium ion battery according to claim 1, wherein the antimony salt is one or more of antimony nitrate, antimony sulfate, antimony bromide, antimony trichloride, antimony sulfide, antimony pentachloride, or antimony hydroxide.
3. The antimony-doped cobalt disulfide-loaded graphene for a lithium ion battery according to claim 1, wherein the organic solvent is one or more of methanol, ethanol, toluene, isopropanol, propylene oxide, styrene, perchloroethylene, trichloroethylene, ethylene glycol ether, triethanolamine, benzene, xylene, pentane, hexane, octane, cyclohexane, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichlorobenzene, dichloromethane, diethyl ether, propylene oxide, methyl acetate, ethyl acetate, propyl acetate, acetone, methyl butanone, methyl isobutyl ketone, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, acetonitrile, pyridine, or phenol.
4. The antimony-doped cobalt disulfide-loaded graphene for a lithium ion battery according to claim 1, wherein the soluble cobalt salt is one or more of cobalt chloride, cobalt acetate, cobalt sulfate, cobalt nitrate, or a hydrate of the above salt.
5. The antimony doped cobalt disulfide loaded graphene for the lithium ion battery according to claim 1, wherein the reaction time is 12-48 h, and the stirring time is 10-100 min.
6. The preparation method of any one of claims 1 to 5, wherein the preparation method comprises the following steps:
s1, respectively dissolving soluble cobalt salt and a vulcanizing agent in deionized water to obtain a solution A and a solution B;
s2, adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
s3, dripping graphene hydrate into the solution C, and uniformly stirring to obtain a solution D;
s4, adding antimony salt into an organic solvent to dissolve to obtain a solution E;
s5, adding the solution D into the solution E, and uniformly stirring to obtain a solution F; carrying out ultrasonic treatment on the solution F, carrying out hydrothermal reaction at 100-300 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid G; and (4) freeze-drying the solid G to obtain the antimony-doped cobalt disulfide-loaded graphene.
7. The method for preparing antimony-doped cobalt disulfide-loaded graphene for a lithium ion battery according to claim 6, wherein the volume ratio of the mass of the soluble cobalt salt to the deionized water in step S1 is (10-20) mg: 1 mL; the mass ratio of the vulcanizing agent to the deionized water is (1-10) mg: 25 mL.
8. The antimony doped cobalt disulfide-loaded graphene as claimed in any one of claims 1 to 5 is applied to the field of lithium ion batteries as a negative electrode material.
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CN112086644B (en) * | 2020-09-01 | 2022-04-01 | 广东工业大学 | Metal sulfide lithium ion negative electrode material and preparation method thereof |
CN113078302B (en) * | 2021-03-09 | 2023-01-10 | 华北电力大学 | Method for preparing sodium-ion battery composite negative electrode material by using large-interlayer-distance two-dimensional layered graphene-like loaded metal sulfide |
CN115028217A (en) * | 2022-05-27 | 2022-09-09 | 慧迈材料科技(广东)有限公司 | Nickel disulfide crossed nanoflower material and preparation method and application thereof |
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