CN110061206B - SiO-based nano composite material, negative electrode and preparation method thereof - Google Patents
SiO-based nano composite material, negative electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a SiO-based nano composite material, a negative electrode and a preparation method thereof, wherein the method comprises the following steps: ball milling silicon oxide particle to prepare nano SiO product, using the nano SiO product, ammonium molybdate and thiourea as raw materials, using deionized water and glycol as solvents, and preparing MoS through hydrolysis reaction, self-assembly and high-temperature calcination2SiO-based nanocomposite material coated with SiO characteristics. The preparation process is simple, green and environment-friendly, and easy for batch production, and the obtained SiO-based nanocomposite has excellent electrochemical performance when used as a lithium ion battery cathode.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a SiO-based nano composite material, a cathode and a preparation method thereof.
Background
Lithium ion batteries, as one of the current high-efficiency energy storage devices, have the characteristics of high energy density, long cycle stability and the like, and are therefore widely applied to electronic equipment and electric vehicles. However, the energy density of lithium ion battery technology has reached a bottleneck due to the low capacity limit of commercial anode materials (graphite), and thus a series of high capacity anode materials have been widely studied, in which transition metal sulfides and silicon-oxygen-based materials having high capacity are receiving attention of researchers.
Researches show that the SiO material has certain circulation stability, can provide certain capacity and is green and environment-friendly, so that the SiO material is used as a matrix to be compounded with other materials to form a composite material, and the circulation stability can be improved while the high capacity is ensured through the mutual synergistic effect of substances. The theoretical lithium storage specific capacity of the molybdenum disulfide is about 670mAh/g, and the molybdenum disulfide has higher theoretical lithium storage specific capacity compared with a commercial carbon material (372mAh/g), so that the molybdenum disulfide attracts extensive research and is one of potential materials for future energy storage. However, these high capacity negative electrode materials tend to suffer from severe volume effects, poor electronic conductivity, and agglomeration of nanoparticlesAnd the like, especially the high surface energy of the nanoparticles enables MoS2The nanoplates are intermittently stacked together, impeding the transport of lithium ions and electrons. Thus MoS2When the lithium ion battery cathode material is used as a lithium ion battery cathode material, the problems of poor cycle stability, poor rate capability and the like are solved.
For example, the domestic patent application publication No. CN108987732A discloses a lithium ion battery SiO composite negative electrode material and a preparation method thereof, in the preparation process of the invention, a secondary carbon-coating method is utilized to prepare a SiO/C composite material, organic matter is firstly used for carbon coating of SiO, and then fluorine-containing high polymer material is used for carbon coating of SiO. However, the preparation method of the secondary carbon coating is complicated, and the structure of the composite material is not easy to regulate and control, so that the performance is general. Therefore, a lithium ion battery cathode material which is simple in preparation process, low in cost, high in production efficiency, easy for large-scale production and excellent in electrochemical performance needs to be found.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the primary object of the invention is to provide a SiO-based nanocomposite, a negative electrode and a preparation method thereof, and based on the purpose, the invention at least provides the following technical scheme:
a preparation method of SiO-based nano composite material comprises the following steps:
step 1, taking raw materials containing nano SiO, a surfactant, ammonium molybdate and thiourea to prepare a suspension;
step 2, placing the suspension in a high-pressure hydrothermal reaction kettle for hydrothermal reaction;
step 3, collecting the product obtained by the hydrothermal reaction, and collecting precipitates to obtain a precursor of the SiO-based nanocomposite;
and 4, calcining the precursor at high temperature to obtain the SiO-based nanocomposite.
Further, the step 1 comprises the following sub-steps:
taking a proper amount of glycol and deionized water as a solvent, and adding a surfactant into the solvent to form a solution;
respectively adding nano SiO, ammonium molybdate and thiourea into the solution, and magnetically stirring to form a suspension;
wherein the volume ratio of the ethylene glycol to the deionized water is 1: (3-4).
Further, in the step 1, the nano SiO is added into the solution and then subjected to ultrasonic treatment for 30 to 60 minutes, the ammonium molybdate and thiourea are added into the solution and then subjected to ultrasonic treatment for 20 to 40 minutes, and the magnetic stirring is performed for 1 to 2 hours.
Further, the mass ratio of the thiourea to the ammonium molybdate is (1-1.2): 1. the mass ratio of the ammonium molybdate to the nano SiO is (2.5-4): 1.
further, the mass ratio of the surfactant to the nano SiO is (0.01-0.4): 1.
further, in the step 2, the conditions of the hydrothermal reaction include: preserving heat for 16-24 hours at 150-200 ℃, and then naturally cooling, wherein the filling ratio of the hydrothermal reaction kettle is 50% -75%.
Further, in step 3, the collecting the precipitate includes: centrifuging and collecting a product of the hydrothermal reaction, and drying the product in vacuum at the temperature of 60-80 ℃ for 10-12 hours to obtain a precipitate;
and 4, placing the collected precursor in a protective gas atmosphere, and heating to 320-800 ℃ to calcine for 2-5 hours.
Further, the nano SiO is obtained by the following steps:
taking absolute ethyl alcohol as a solvent, adding silicon oxide particles into the solvent to form a suspension, carrying out vacuum ball milling on the suspension, and then carrying out vacuum drying to obtain the nano SiO.
The SiO-based nano composite material comprises a blocky nano SiO material and MoS growing on the surface of the blocky nano SiO material2Material of said MoS2The material is in a sphere-like shape formed by conglobation of lamellar structures.
An anode comprising the SiO-based nanocomposite.
In general, the invention has at least the following beneficial effects:
(1) the invention provides a preparation method of a SiO-based composite material, which has the advantages that the raw materials are simple and easy to obtain; the synthesis method is relatively common, the process is simple and feasible, the used instruments are relatively common, the requirement on equipment is low, and the cost is low.
(2) The method is realized by mixing a nano SiO matrix and MoS2The prepared SiO-based nano composite material forms a special space structure, the silicon monoxide with certain specific capacity is combined with the molybdenum disulfide to support each other, and the stability of the composite material is improved while the high reversible capacity of the composite material is ensured by utilizing the synergistic effect. The lamellar molybdenum disulfide is uniformly coated on the surface of the silicon monoxide material to present a similar coating structure, so that the agglomeration of the molybdenum disulfide material is effectively relieved while the particle size of the molybdenum disulfide is reduced. The cladding structure enables the composite material to be more stable, and reduces the loss of irreversible capacity.
(3) When the SiO-based nano composite material prepared by the invention is applied to a lithium ion battery cathode material, the SiO-based nano composite material has the advantages of good cycling stability and good rate capability, and can still maintain the reversible specific capacity of 450mAh/g after 500 times of charge-discharge cycles under the current density of 1000 mA/g; in a rate performance test, under the current densities of 2A/g and 4A/g, the average specific discharge capacity can still reach the capacities of 500mAh/g and 430mAh/g, and when the current density is recovered to 100mA/g, the capacity can still be increased, and the material is used as a lithium ion battery cathode material and shows excellent electrochemical performance.
Drawings
FIG. 1 shows SiO/MoS in an embodiment of the present invention2Composite material, nano SiO material and pure MoS2XRD pattern of the material.
FIG. 2 shows an embodiment of the present invention in which the SiO nano-material and the MoS are used2Material and SiO/MoS2SEM image of the composite material.
FIG. 3 shows SiO/MoS in an embodiment of the present invention2Composite material and pure MoS2Ac impedance of the material versus the graph.
FIG. 4 shows SiO/MoS in an embodiment of the present invention2Cycle performance profile of the composite (1000 mAh/g).
FIG. 5 shows SiO/MoS in an embodiment of the present invention2Graph of the rate performance of the composite material.
Detailed Description
Further details of the invention are set forth in the accompanying drawings and the detailed description below, and alternative further embodiments of the invention are described in detail. It is noted that the embodied steps of the present invention are not limited to the presently described embodiments, and that other attempts may be made by those skilled in the art based on specific experimental conditions and facilities without departing from the spirit and scope of the present invention.
Examples
Preparing a nano SiO material: weighing 1-2 g of silicon oxide particles, putting the silicon oxide particles into a 100ml agate ball milling tank, adding grinding beads, wherein the mass ratio of the grinding beads to the added silicon monoxide is (20-50): 1, adding 20-50 ml of absolute ethyl alcohol into the ball milling tank, in the embodiment, the mass of the silicon oxide particles is preferably 1-1.5 g, and the mass ratio of the grinding beads to the added silicon monoxide is preferably (40-50): preferably, the absolute ethyl alcohol is 30-50 ml. And transferring the ball milling tank into a ball mill, setting the ball milling rotation speed to be 200-600 rpm, setting the ball milling time to be 10-24 hours, preferably selecting 500rpm for ball milling for 10 hours in the embodiment, and performing vacuum drying on the ball milling product to obtain the nano SiO material. The nano SiO prepared by the ball milling method has high yield and simple and easy process.
Solution preparation: taking the volume ratio of 1: (3-4), in the embodiment, preferably, the ethylene glycol and the deionized water in a volume ratio of 1:4 are uniformly mixed, as a solvent, cetyltrimethylammonium chloride or cetyltrimethylammonium bromide is added as a surfactant to form a solution, nano-SiO is dispersed into the solution, and ultrasonic treatment is performed at room temperature for 30-60 minutes, preferably, ultrasonic treatment is performed at room temperature for 30 minutes, ammonium molybdate and thiourea are dispersed into the solution, after ultrasonic treatment is performed at room temperature for 20-40 minutes, magnetic stirring is performed for about 1-2 hours to form a suspension, preferably, after ultrasonic treatment is performed at room temperature for 30 minutes, magnetic stirring is performed for about 1 hour to form a suspension, wherein the purpose of ultrasonic treatment at room temperature is to reduce agglomeration of nano-SiO particles, and the nano-SiO particles are more uniformly dispersed by the action of the ethylene glycol.
Wherein, the mass ratio of the nano SiO product to the ammonium molybdate is selected mainly in consideration of MoS2The growth ratio on the surface of the nano SiO is that the MoS is2The SiO surface is coated more uniformly; the addition of the active agent enables the surface of the SiO particle to obtain more active sites, and promotes MoS2Compounding with SiO; the mass ratio of ammonium molybdate to thiourea is mainly selected from MoS2Chemical element proportion of (2) to ensure MoS2And (4) synthesizing. Therefore, the mass ratio of the hexadecyl trimethyl ammonium chloride or the hexadecyl trimethyl ammonium bromide to the nano SiO material is about 0.1-0.3: 1, the mass ratio of the ammonium molybdate to the nano SiO material is 2.5-4: 1, the mass ratio of the thiourea to the ammonium molybdate is 1-1.2: 1, and the mass ratio of the ammonium molybdate to the solvent is 1: 100.
The high-pressure hydrothermal reaction kettle can decompose insoluble substances, can create a high-temperature high-pressure corrosion-resistant high-purity environment for hydrothermal reaction, and obtains a synthetic substance by controlling the temperature, time and solvent of the reaction to obtain a precursor, so that the purpose of experiments is achieved. The invention selects a high-pressure hydrothermal reaction kettle to carry out hydrothermal reaction and self-assembly.
Hydrothermal reaction: the obtained suspension was transferred to a high-pressure hydrothermal reaction vessel to carry out hydrothermal reaction at a temperature of about 180 ℃ for about 24 hours. Wherein the filling amount of the high-pressure hydrothermal reaction kettle is about 70 percent.
And (3) precipitation and collection: cooling the reaction liquid to room temperature, centrifuging the precipitate obtained by the hydrothermal reaction for 4 times by using ethanol, and then drying the precipitate in vacuum at the temperature of 60-80 ℃ for 10-12 hours, preferably at the temperature of 80 ℃ for 12 hours to obtain SiO/MoS2And (3) a composite material precursor.
High-temperature calcination: drying the SiO/MoS in vacuum2Calcining the composite material precursor in an argon atmosphere for 3 hours at 500 ℃ to obtain SiO/MoS2Composite materials, i.e. SiO based nanocomposites.
The obtained SiO-based nano composite material is sequentially subjected to the working procedures of size mixing, coating, drying and the like to prepare the obtained electrode material, and when the obtained electrode material is used as a lithium ion battery cathode, excellent electrochemical performance can be obtained.
FIG. 1 shows SiO/MoS obtained in the example of the present invention2Composite material, nano SiO material and pure MoS2XRD pattern of the material, as can be seen from the peak in FIG. 1, SiO/MoS in the present invention2The composite material has both SiO and MoS2A composite phase of two substances.
As shown in FIG. 2, the diagrams a-b are SEM images of the nano SiO material in the example of the invention, and it can be seen from the SEM images that the nano SiO material has a bulk structure. c-d are pure MoS in the examples of the present invention2SEM image of material from which MoS can be seen2The material is in a sphere-like shape formed by agglomeration of lamellar structures. e-f diagrams show SiO/MoS in the examples of the present invention2SEM image of composite material, from which it can be seen that the SiO/MoS prepared by the present invention2The composite material has a coating structure which mainly comprises a bulk-structure nano SiO material and MoS growing on the surface of the bulk-structure nano SiO material2Material composition of the MoS2The material presents a sphere-like shape formed by conglobation of lamellar structures and grows on the surface of the bulk structure nano SiO material.
FIG. 3 shows SiO/MoS obtained in the example of the present invention2Composite material and pure MoS2AC impedance of materials is compared to a graph, from which it can be seen that for pure MoS2Material comparison, SiO/MoS2The internal resistance value of the composite material is less than that of pure MoS2Material having a smaller mass transfer resistance, from which it can be seen that SiO/MoS2Composite material compared to pure MoS2The material has more excellent electrochemical performance.
FIG. 4 shows an embodiment of the present inventionSiO/MoS2When the composite material is prepared to obtain the negative electrode material as the negative electrode of the lithium ion battery, the charge-discharge cycle chart of 500 cycles under the current density of 1000mA/g is obtained, and the chart shows that SiO/MoS2The first coulombic efficiency of the composite electrode is 75%, the composite electrode can still keep the discharge specific capacity of 450mAh/g after 500 cycles, and stable cycle performance is shown.
FIG. 5 shows SiO/MoS in an embodiment of the present invention2The multiplying power curve of the negative electrode material prepared from the composite material as the negative electrode of the lithium ion battery can be seen from the figure, the capacity of the negative electrode material after multiple charge-discharge cycles under different multiplying powers can still reach the initial cycle standard, and the excellent multiplying power performance is shown.
Therefore, the SiO-based composite material obtained by the preparation method disclosed by the invention combines silicon monoxide and molybdenum dioxide with certain specific capacity, supports each other, utilizes the synergistic effect, ensures the high reversible capacity of the composite material, and also increases the stability of the composite material. The test of the performance shows that the material obtained by the method effectively relieves the agglomeration of the molybdenum disulfide material, the composite material is more stable due to the coating structure, the loss of irreversible capacity is reduced, and the material is a lithium ion battery cathode material with excellent performance.
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 (7)
1. A preparation method of SiO-based nano composite material is characterized by comprising the following steps:
step 1, taking raw materials containing nano SiO, a surfactant, ammonium molybdate and thiourea to prepare a suspension;
step 2, placing the suspension in a high-pressure hydrothermal reaction kettle for hydrothermal reaction;
step 3, collecting precipitates of the hydrothermal reaction product to obtain a precursor of the SiO-based nanocomposite;
step 4, calcining the precursor at high temperature to obtain the SiO-based nanocomposite;
the step 1 comprises the following substeps: taking a proper amount of glycol and deionized water as a solvent, and adding a surfactant into the solvent to form a solution; respectively adding nano SiO, ammonium molybdate and thiourea into the solution, and magnetically stirring to form a suspension; wherein the volume ratio of the ethylene glycol to the deionized water is 1: (3-4);
the mass ratio of the ammonium molybdate to the nano SiO is (2.5-4): 1;
the mass ratio of the surfactant to the nano SiO is (0.01-0.4): 1;
the mass ratio of the thiourea to the ammonium molybdate is (1-1.2): 1;
and 4, placing the collected precursor in a protective gas atmosphere, and heating to 320-800 ℃ to calcine for 2-5 hours.
2. The method according to claim 1, wherein in the step 1, the nano SiO is added to the solution, then the solution is subjected to ultrasonic treatment for 30 to 60 minutes, the ammonium molybdate and thiourea are added, then the solution is subjected to ultrasonic treatment for 20 to 40 minutes, and the magnetic stirring is performed for 1 to 2 hours.
3. The preparation method according to claim 1, wherein in the step 2, the conditions of the hydrothermal reaction include: preserving heat for 16-24 hours at 150-200 ℃, and then naturally cooling, wherein the filling ratio of the high-pressure hydrothermal reaction kettle is 50-75%.
4. The method according to claim 1, wherein the step 3, collecting the precipitate includes: and centrifuging and collecting the product of the hydrothermal reaction, and drying in vacuum at 60-80 ℃ for 10-12 hours to obtain the precursor of the SiO-based nanocomposite.
5. The method according to claim 1, wherein the nano SiO is obtained by:
adding silicon oxide particles into absolute ethyl alcohol, carrying out vacuum ball milling on the formed suspension, and then carrying out vacuum drying to obtain the nano SiO.
6. A SiO-based nanocomposite, characterized in that the SiO-based nanocomposite is obtained by the preparation method of any one of claims 1 to 5, and comprises a bulk nano SiO material and MoS grown on the surface of the bulk nano SiO material2Material of said MoS2The material is in a sphere-like shape formed by conglobation of lamellar structures.
7. A negative electrode, characterized in that it comprises the SiO-based nanocomposite material according to claim 6.
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| CN106532030B (en) * | 2016-12-26 | 2020-03-20 | 惠州亿纬创能电池有限公司 | Calcium molybdate lithium ion battery cathode material and preparation method thereof |
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| CN108963204B (en) * | 2018-06-11 | 2020-11-17 | 华南师范大学 | Preparation method of silicon-based/sulfide negative electrode material with graphene-like sandwich structure |
| CN108878851B (en) * | 2018-07-09 | 2021-01-26 | 郑州轻工业学院 | Preparation method and application of one-dimensional porous diamond hollow tubular alpha-manganese sulfide/molybdenum sulfide @ carbon composite material |
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| CN104037396A (en) * | 2014-05-27 | 2014-09-10 | 中南大学 | Carbon-carbon multi-component negative electrode material and preparation method thereof |
| CN108417404A (en) * | 2016-08-26 | 2018-08-17 | 重庆文理学院 | A kind of preparation method of electrode material for super capacitor |
| WO2018071602A1 (en) * | 2016-10-11 | 2018-04-19 | Everon24 Llc | Rechargeable aluminum ion battery |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
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