CN112002880A - Tin-doped cobalt disulfide-loaded MXene material and preparation method thereof - Google Patents
Tin-doped cobalt disulfide-loaded MXene material and preparation method thereof Download PDFInfo
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- CN112002880A CN112002880A CN202010676312.XA CN202010676312A CN112002880A CN 112002880 A CN112002880 A CN 112002880A CN 202010676312 A CN202010676312 A CN 202010676312A CN 112002880 A CN112002880 A CN 112002880A
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Abstract
The embodiment of the invention provides a preparation method of a tin-doped cobalt disulfide-loaded MXene material, which comprises the following steps: adding tin salt into soluble cobalt salt aqueous solution and vulcanizing agent aqueous solution, and uniformly stirring; adding a single-layer MXene aqueous solution, stirring and carrying out ultrasonic treatment to obtain a mixed solution; carrying out hydrothermal reaction on the obtained mixed solution at 110-360 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid; and (4) freeze-drying the obtained solid to obtain the tin-doped cobalt disulfide-loaded MXene material. The tin-doped cobalt disulfide-loaded MXene material provided by the embodiment of the invention not only can effectively improve the rate capability and cycle performance of a battery, but also can effectively inhibit the volume expansion of the battery in the charging and discharging processes; the rate of capacity fading is weakened, and the coulomb effect is 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 new energy, in particular to a tin-doped cobalt disulfide-loaded MXene material and a preparation method thereof.
Background
The development of the lithium ion battery is originated from the 90 s of the last century, is not more than 20 years till now, is a leap of the lithium battery industry in the last 20 years, and the lithium ion battery has more rapid development with the importance of various countries on environment and new energy. A lithium ion battery is a secondary battery system in which two different lithium intercalation compounds capable of reversibly intercalating and deintercalating lithium ions are used as a positive electrode and a negative electrode of the battery, respectively, and lithium ions are deintercalated from the positive electrode and intercalated into the negative electrode through an electrolyte and a separator during charging, and conversely are deintercalated from the negative electrode and intercalated into the positive electrode through the electrolyte and the separator during discharging.
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. Graphite is a current commercialized negative electrode material, but the specific capacity of the graphite reaches the limit due to the structural limitation of the graphite, so that the requirement of an energy automobile cannot be met, and although the specific capacity of a silicon negative electrode is as high as 2700mAh/g, a large volume expansion effect can occur in the charging and discharging process, so that the safety performance is low; therefore, the research of the electrode material meeting the requirement of the energy automobile field is urgently needed.
The cobalt disulfide is used as an electrode material of the lithium ion battery, has the theoretical specific capacity of 870mAh/g, has the advantages of excellent conductivity and multiplying power, environmental friendliness, abundant reserves and the like, and is very suitable for being used as a negative electrode material of a next generation high-energy lithium ion battery cell. However, the cobalt disulfide is accompanied with a large volume expansion effect in the process of lithium ion intercalation/deintercalation, so that the capacity attenuation is too fast in the process of charging and discharging, and the coulombic efficiency is also continuously reduced. Therefore, it is necessary to buffer the volume effect generated during the charge and discharge processes thereof, thereby improving the cycle stability thereof as much as possible.
Disclosure of Invention
The invention provides a tin-doped cobalt disulfide-loaded MXene material and a preparation method thereof, aiming at solving the technical problem that the conventional lithium battery cathode material is not beneficial to use.
The embodiment of the invention provides a preparation method of a tin-doped cobalt disulfide-loaded MXene material, which comprises the following steps:
s1, adding tin 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 and carrying out ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 110-360 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the tin-doped cobalt disulfide-loaded MXene material.
Further, the tin salt includes one or more of crystalline tin tetrachloride, tin hydroxymethane sulfonate, tin 2-hydroxyethyl-1-sulfonate, tin 2-hydroxybutyl-1-sulfonate, tin methane sulfonate, tin ethane sulfonate, tin propane sulfonate, tin 2-propane sulfonate, and tin alkyl sulfonate.
Further, the soluble cobalt salt in the soluble cobalt salt aqueous solution comprises one or more of cobalt naphthenate, cobalt sulfate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride and cobalt acetate cobalt nitrate.
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 tin 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): (0.1-1.8): (1-8): 1.
further, the concentration of the soluble cobalt salt aqueous solution is 0.05-0.2 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 0.05-0.9 mol/L.
Further, the stirring time in the steps S1 and S2 is 10-100 min; the freeze drying time in the step S4 is 12-36 h, and the freeze drying temperature is-47 to-19 ℃.
On the other hand, the invention also provides a tin-doped cobalt disulfide-loaded MXene material, and the tin-doped cobalt disulfide-loaded MXene material is prepared by the preparation method.
The invention has the beneficial effects that: the tin-doped cobalt disulfide-loaded MXene material provided by the embodiment of the invention not only can effectively improve the rate capability and cycle performance of a battery, but also can effectively inhibit the volume expansion of the battery in the charging and discharging processes; the rate of capacity fading is weakened, and the coulomb effect is improved. The MXene-loaded tin-doped cobalt disulfide material has the structure that small flakes and sheets alternately exist, the small flakes are formed by tin-doped cobalt disulfide wafers, the cobalt disulfide matrix grows depending on the surface layer of MXene, the ionic conduction effect can be effectively improved, the transmission and conduction performance of electrons is further increased, and meanwhile, due to the doping of a single-layer loaded MXene and tin elements, the material not only can effectively inhibit the volume effect in the charge and discharge process, but also can effectively inhibit the capacity attenuation in the charge and discharge process, the cycle performance is greatly improved, and the stability of a lithium ion battery is further 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 tin-doped cobalt disulfide-loaded MXene material, which comprises the following steps:
s1, adding tin 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 and carrying out ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 110-360 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the tin-doped cobalt disulfide-loaded MXene material.
The tin-doped cobalt disulfide-loaded MXene material provided by the embodiment of the invention not only can effectively improve the rate capability and cycle performance of a battery, but also can effectively inhibit the volume expansion of the battery in the charging and discharging processes; the rate of capacity fading is weakened, and the coulomb effect is improved. The MXene-loaded tin-doped cobalt disulfide material has the structure that small flakes and sheets alternately exist, the small flakes are formed by tin-doped cobalt disulfide wafers, the cobalt disulfide matrix grows depending on the surface layer of MXene, the ionic conduction effect can be effectively improved, the transmission and conduction performance of electrons is further increased, and meanwhile, due to the doping of a single-layer loaded MXene and tin elements, the material not only can effectively inhibit the volume effect in the charge and discharge process, but also can effectively inhibit the capacity attenuation in the charge and discharge process, the cycle performance is greatly improved, and the stability of a lithium ion battery is further improved. The invention has simple manufacturing method, low cost and high yield, and is suitable for industrial batch production.
The method specifically comprises the following 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 tin salt into deionized water for dissolving, adding the dissolved tin 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 100-360 ℃ for 18-28 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 tin-doped cobalt disulfide-loaded MXene material.
The volume ratio of the mass of the soluble cobalt salt to the deionized water in the above step 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 tin-doped cobalt disulfide-loaded MXene material not only further increases the transmission and conduction performance of electrons; and the capacity attenuation in the charging and discharging process is effectively inhibited, the cycle performance is greatly improved, and the stability is further improved.
In an alternative embodiment, the tin salt comprises one or more of crystalline tin tetrachloride, tin hydroxymethane sulfonate, tin 2-hydroxyethyl-1-sulfonate, tin 2-hydroxybutyl-1-sulfonate, tin methane sulfonate, tin ethane sulfonate, tin propane sulfonate, tin 2-propane sulfonate, and tin alkyl sulfonate.
In an alternative embodiment, the soluble cobalt salt in the aqueous solution of a soluble cobalt salt comprises one or more of cobalt naphthenate, cobalt sulfate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride, and cobalt acetate cobalt nitrate.
In an alternative embodiment, the sulfiding agent in the aqueous sulfiding agent solution comprises one or more of sodium sulfide, potassium sulfide, thiopropionic amine, thioacetamide, and L-cysteine.
In an optional embodiment, the mass ratio of the tin 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): (0.1-1.8): (1-8): 1.
in an optional embodiment, the concentration of the soluble cobalt salt aqueous solution is 0.05-0.2 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 0.05-0.9 mol/L.
In an optional embodiment, the stirring time in the steps S1 and S2 is 10-100 min; the freeze drying time in the step S4 is 12-36 h, and the freeze drying temperature is-47 to-19 ℃.
On the other hand, the invention also provides a tin-doped cobalt disulfide-loaded MXene material, and the tin-doped cobalt disulfide-loaded MXene material is prepared by the preparation method.
The specific embodiment is as follows:
example 1
1. Adding 0.255g of CoCl2 hexahydrate into 10 ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.246g of L-cysteine into 150 ml 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 15min to obtain a yellow-brown solution which is marked as solution C;
4. adding 2.235 g of crystallized tin tetrachloride 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 5.96g of MXene aqueous solution into the solution D, stirring for 25 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 28h, 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 28 hours to obtain the tin-doped cobalt disulfide-loaded MXene material.
Example 2
1. Adding 0.221g of CoCl2 hexahydrate into 30ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.233g 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 30min to obtain a yellow-brown solution which is marked as solution C;
4. adding 2.218g of crystalline stannic chloride into 20ml of deionized water, stirring and dissolving completely, then adding into the solution C, stirring for 13min 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 15mim to obtain a black solution marked as solution E;
6. the solution E is subjected to ultrasonic treatment for 30min 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 tin-doped cobalt disulfide-loaded MXene material.
Example 3
1. Adding 0.235g of CoCl2 hexahydrate into 20ml of deionized water, stirring and dissolving to obtain a pink solution, and marking as a solution A;
2. adding 0.323g of L-cysteine into 30ml 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 10min to obtain a yellow-brown solution which is marked as solution C;
4. adding 0.328g of crystallized tin tetrachloride into 13ml of deionized water, stirring and dissolving completely, then adding into the solution C, and stirring for 20min to obtain a khaki solution which is marked as solution D;
5. adding 6.58g of single-layer MXene aqueous solution into the solution D, and stirring for 20mim 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 tin-doped cobalt disulfide-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. A preparation method of a tin-doped cobalt disulfide-loaded MXene material is characterized by comprising the following steps:
s1, adding tin 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 and carrying out ultrasonic treatment to obtain a mixed solution;
s3, carrying out hydrothermal reaction on the obtained mixed solution at the temperature of 110-360 ℃, cooling along with a furnace, and carrying out suction filtration to obtain a solid;
s4, freeze-drying the obtained solid to obtain the tin-doped cobalt disulfide-loaded MXene material.
2. The method of preparing the tin-doped cobalt disulfide-supported MXene material of claim 1, wherein the tin salt comprises one or more of crystalline tin tetrachloride, tin hydroxymethane sulfonate, tin 2-hydroxyethyl-1-sulfonate, tin 2-hydroxybutyl-1-sulfonate, tin methane sulfonate, tin ethane sulfonate, tin propane sulfonate, tin 2-propane sulfonate, and tin alkyl sulfonate.
3. The method for preparing the tin-doped cobalt disulfide-loaded MXene material of claim 1, wherein the soluble cobalt salt in the aqueous solution of soluble cobalt salt comprises one or more of cobalt naphthenate, cobalt sulfate, cobalt stearate, cobalt neodecanoate, cobalt boroacylate, cobalt chloride and cobalt acetate cobalt nitrate.
4. The method for preparing the tin-doped cobalt disulfide-loaded MXene material of claim 1, wherein the vulcanizing agent in the aqueous vulcanizing agent solution comprises one or more of sodium sulfide, potassium sulfide, thiopropionic amine, thioacetamide and L-cysteine.
5. The preparation method of the tin-doped cobalt disulfide-loaded MXene material as claimed in claim 1, wherein the mass ratio of the tin 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): (0.1-1.8): (1-8): 1.
6. the method for preparing the tin-doped cobalt disulfide-loaded MXene material as claimed in claim 1, wherein the concentration of the soluble cobalt salt aqueous solution is 0.05-0.2 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 0.05-0.9 mol/L.
7. The preparation method of the tin-doped cobalt disulfide-loaded MXene material as claimed in claim 1, wherein the stirring time in steps S1 and S2 is 10-100 min; the freeze drying time in the step S4 is 12-36 h, and the freeze drying temperature is-47 to-19 ℃.
8. The tin-doped cobalt disulfide-loaded MXene material is characterized by being prepared by the preparation method of any one of claims 1-7.
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| CN112467068A (en) * | 2020-12-11 | 2021-03-09 | 燕山大学 | Battery negative electrode material and preparation method and application thereof |
| CN113120970A (en) * | 2021-03-26 | 2021-07-16 | 东南大学 | Method for preparing compound containing crystal water cobalt sulfate and redox graphene |
| CN115924984A (en) * | 2022-08-31 | 2023-04-07 | 青岛大学 | Preparation method of iron ion doped CoS2/MXene heterostructure composite material |
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| CN110911684A (en) * | 2019-11-22 | 2020-03-24 | 广东工业大学 | Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof |
| CN111268671A (en) * | 2020-01-20 | 2020-06-12 | 广东工业大学 | Graphene-loaded tin-doped cobalt disulfide composite material and preparation method and application thereof |
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| CN110416507A (en) * | 2019-07-12 | 2019-11-05 | 广东工业大学 | A kind of three-dimensional flower-shaped cobalt disulfide of primary reconstruction/MXene composite material and preparation method and application |
| CN110911684A (en) * | 2019-11-22 | 2020-03-24 | 广东工业大学 | Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof |
| CN111268671A (en) * | 2020-01-20 | 2020-06-12 | 广东工业大学 | Graphene-loaded tin-doped cobalt disulfide composite material and preparation method and application thereof |
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| CN112467068A (en) * | 2020-12-11 | 2021-03-09 | 燕山大学 | Battery negative electrode material and preparation method and application thereof |
| CN113120970A (en) * | 2021-03-26 | 2021-07-16 | 东南大学 | Method for preparing compound containing crystal water cobalt sulfate and redox graphene |
| CN115924984A (en) * | 2022-08-31 | 2023-04-07 | 青岛大学 | Preparation method of iron ion doped CoS2/MXene heterostructure composite material |
| CN115924984B (en) * | 2022-08-31 | 2023-11-17 | 青岛大学 | Preparation method of iron ion doped CoS2/MXene heterostructure composite material |
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