CN112038626A - Tin-carbon composite material for lithium ion battery cathode and preparation method thereof - Google Patents
Tin-carbon composite material for lithium ion battery cathode and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention provides a tin-carbon composite material for a lithium ion battery cathode and a preparation method thereof; the method comprises the following steps: s1, dissolving a tin source in water, adding water-soluble inorganic salt and a carbon source, and physically mixing to form a uniformly mixed solution; s2, freeze-drying the solution obtained in the step S1 to obtain white powder; s3, grinding the white powder dried in the step S2, and carrying out carbonization treatment under a protective atmosphere to obtain black powder; s4, washing and drying the black powder obtained in the step S3 to obtain honeycomb SnO2@ C composite material. The tin-carbon composite material prepared by the method has excellent electrochemical performance, and the nano-sized SnO can be well formed by the honeycomb-shaped carbon network2The particles are wrapped, so that the buffering SnO is favorably realized2The volume expansion of the particles during charging, and the conductive network formed at the same time can provide fast ion transmissionEffective passage and ensures rapid transfer of electrons; the preparation process is simple, the cost is low, and the environment is not polluted.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery preparation, and particularly relates to a tin-carbon composite material for a lithium ion battery cathode and a preparation method thereof.
Background
In recent years, with the rapid development of electronic products, electric equipment and new energy automobiles, people are eagerly expected to develop a lithium ion battery with high specific capacity, high power, long cycle life and environmental friendliness. The cathode material as an important component of the lithium ion battery directly influences the energy density and the service life of the battery. At present, the commercial lithium ion battery cathode material is mainly graphite, the theoretical capacity of the lithium ion battery cathode material is about 372mA h/g, and the requirement of a power battery on the high-energy-density cathode material cannot be met, so that the research and development of the cathode material which is high in specific capacity, low in price and environment-friendly is urgent. The tin oxide has the advantages of high theoretical specific capacity (790mA h/g), large resource storage capacity and environmental friendliness, and is expected to replace graphite to become a novel anode material.
However, SnO2The negative electrode also has some inherent disadvantages, its irreversible lithium intercalation during the first cycle leading to lower coulombic efficiency; meanwhile, severe volume expansion and contraction can be generated in the process of continuously inserting and extracting lithium, and stress is generated, so that cracking and pulverization failure are generated; and SnO2The conductivity of the conductive material is poor, and the charging and discharging under a large current cannot be met. These disadvantages lead to SnO2Has poor electrochemical performance, and seriously hinders the commercial application of the catalyst.
To solve the above SnO2The negative electrode has the defects, and the currently researched methods comprise synthesizing nano structures such as nano linear, nano sheet, nano tube, nano rod, hollow nano rod and the like, and alloying tin-based negative electrode materials orThe tin oxide is compounded with carbon, but the methods generally have the problems of complex synthesis process and high cost, and the cycle performance still needs to be improved.
Therefore, there is a need in the art to develop a novel SnO2The cathode material has the advantages of small volume expansion, good conductivity, simple preparation process, low preparation cost and the like, and has good application prospect.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a tin-carbon composite material for a lithium ion battery cathode, which utilizes water-soluble inorganic salt as a template, combines a freeze drying process and synthesizes honeycomb-shaped tin-carbon composite SnO in situ by a simple one-step method2the/C cathode material has the advantages of simple preparation method, excellent electrochemical performance and the like.
The invention provides a preparation method of a tin-carbon composite material for a lithium ion battery cathode, which comprises the following steps: s1, dissolving a tin source in water, adding water-soluble inorganic salt and a carbon source, and physically mixing to form a uniformly mixed solution; s2, freeze-drying the solution obtained in the step S1 to obtain white powder; s3, grinding the white powder dried in the step S2, and carrying out carbonization treatment under a protective atmosphere to obtain black powder; s4, washing and drying the black powder obtained in the step S3 to obtain honeycomb SnO2@ C composite material.
Wherein the tin source comprises SnCl4·5H2O and Na2SnO3One kind of (1).
The water-soluble inorganic salt forms a template with a honeycomb-shaped porous appearance. The water-soluble inorganic salt includes sodium salt, potassium salt, sodium salt such as sodium chloride, sodium sulfate, sodium carbonate, etc.; such as potassium chloride, potassium sulfate, potassium carbonate, and the like.
The carbon source is mainly an organic substance containing carbon elements, and the types of the carbon source are not limited, and include citric acid, dopamine hydrochloride, glucose, polyphosphoric acid melamine and the like.
The tin source is as follows: water-soluble inorganic salts: the molar ratio of the carbon source is 1-3: 20-100: 4-8; the water content is 10-30 ml.
Preferably, the freeze-drying temperature in the step S2 is-30 to-60 ℃, and the drying time is 24 to 72 hours. .
Preferably, the protective atmosphere in step S3 is an inert gas, such as nitrogen, argon, etc., and the carbonization process includes: raising the temperature from room temperature to 450-750 ℃ at a heating rate of 1-5 ℃/min, preserving the temperature for 2-5 h, and naturally cooling to the room temperature.
Preferably, the step S4 is vacuum drying, the temperature of the vacuum drying is 60-100 ℃, and the time of the vacuum drying is 10-24 hours.
Different from the prior art that Na needs to be added+The tin source, the sodium salt and the carbon source are physically mixed, then are subjected to freeze drying, and are subjected to primary calcination and primary washing and drying to obtain the final product, namely the cellular three-dimensional SnO2@ C composite material.
The invention also provides a tin-carbon composite material for the negative electrode of the lithium ion battery, which comprises the following components: after freeze drying, the cellular porous shape provided by water-soluble inorganic salt is taken as a template, and nano tin oxide particles are attached to the carbon nano-sheet to form SnO with a three-dimensional cellular three-dimensional structure2@ C composite material.
The invention has the beneficial effects that: (1) honeycomb-shaped tin-carbon composite negative electrode material SnO2@ C has a high reversible capacity, 890mA h/g after 500 cycles. (2) In-situ synthesis of tin-carbon composite SnO by one-step method2The @ C matrix greatly simplifies the process; the water-soluble inorganic salt is used as a template to form a honeycomb shape, so that the environment is not polluted, and the honeycomb shape can be easily removed by using water. (3) The nano-sized SnO can be well bonded by forming such a honeycomb-shaped carbon network2The particles are wrapped, so that the buffering SnO is favorably realized2The volume of the particles expands during charging, and the conductive network formed at the same time can provide a quick and effective channel for ion transmission and ensure quick transfer of electrons. (4) The preparation process is simple, the cost is low, and the method is expected to become a large-scale production.
Drawings
FIG. 1 shows a tin-carbon composite anode material SnO prepared in example 1 of the present invention2SEM picture of @ C.
FIG. 2 shows a tin-carbon composite anode material SnO prepared in example 1 of the present invention2XRD pattern of @ C.
FIG. 3 shows a tin-carbon composite anode material SnO prepared in example 1 of the present invention2@ C is the cycling curve at 500mA/g current density after assembly into a half cell.
FIG. 4 shows the use of commercial nano SnO in comparative example 1 of the present invention2Cycling curves at 500mA/g current density after the particles were assembled into half cells as negative electrode materials.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments and with reference to the attached drawings, it should be emphasized that the following description is only exemplary and is not intended to limit the scope and application of the present invention.
Example 1:
15ml of deionized water is prepared, 2mmol of SnCl is added4·5H2O, and completely dissolved by magnetic stirring for 10 min. Subsequently 85mmol NaCl and 6mmol citric acid were added during magnetic stirring. After vigorous stirring for 30min, a homogeneous, colorless, transparent solution was obtained. The solution was rapidly cooled by liquid nitrogen and freeze dried at-50 ℃ for 48 h. Grinding the dried white powder, heating to 550 ℃ from room temperature at a heating rate of 3 ℃/min under the argon atmosphere, preserving heat for 3h, and naturally cooling to room temperature. Washing and filtering the obtained black powder with deionized water for at least three times respectively, and drying in vacuum at 60 ℃ for 12h to obtain a target product SnO2@C。
Honeycomb-shaped tin-carbon composite negative electrode material SnO2Basic characterization of @ C:
the morphology of the negative electrode material is characterized by a scanning electron microscope (Hitachi S4700 model of Hitachi, Japan), and as shown in figure 1, the particle diameter of the material is between 100 and 300nm, and the pore diameter of a honeycomb is between 0.2 and 1 mu m.
The crystal structure of the negative electrode material was analyzed by an X-ray diffractometer (model D/Max2500/PC), and the results are shown in FIG. 2. As can be seen from the figure, the material conforms to SnO2Crystal peak of (2).
Honeycomb bodySnO (stannic-carbon) composite cathode material2Electrochemical characterization of @ C:
weighing 0.16g of the obtained negative electrode material, 0.02g of carbon black as a conductive agent, 0.02g of polyvinylidene fluoride (PVDF) as a binder, uniformly grinding, dropwise adding a proper amount of NMP, continuously grinding to paste, uniformly coating on a copper foil, obtaining a negative electrode sheet after vacuum drying at 80 ℃ for 12 hours, and assembling the negative electrode sheet into a button cell in an argon-protected glove box by taking a metal lithium sheet as a counter electrode, a glass fiber membrane as a diaphragm and a 1M Ethylene Carbonate (EC)/diethyl carbonate (DEC) solution of LiPF6 (volume ratio of 1: 1) as an electrolyte.
The assembled battery is subjected to constant-current charge and discharge test on a Xinwei charge and discharge tester, the voltage range is 0.01-3.0V, and the test temperature is 25 ℃. FIG. 3 is a plot of the cycling at a current density of 500mA/g, over 500 cycles, with a capacity of 890mA h/g, notably, synthesized SnO2The @ C composite material continuously attenuates in the first 100 circles, the capacity of the composite material continuously rises after a period of time circulation, the composite material is stable until 450 circles, the composite material is continuously maintained, no obvious attenuation exists, and the composite material has a relatively good capacity retention rate.
Example 2
The other conditions were the same as in example 1 except that the temperature of carbonization in the third step was 450 ℃. The assembly process of the button cell is the same as that of example 1, and the obtained negative electrode material has a capacity of 257mA h/g after 200 cycles at a current density of 500 mA/g.
Example 3
The other conditions were the same as in example 1 except that the temperature of carbonization in the third step was 650 ℃. The assembly process of the button cell is the same as that of the example 1, and the obtained negative electrode material has 657mA h/g of capacity after 200 cycles under the current density of 500mA/g and has good capacity retention rate.
Example 4
The other conditions were the same as in example 1 except that the tin source added in the first step was Na2SnO3. The assembly process of the button cell is the same as that of the example 1, the obtained negative electrode material is cycled for 200 circles under the current density of 500mA/g, and the capacity is 373mA h/g。
Example 5
The other conditions were the same as in example 1 except that the carbon source added in the first step was dopamine hydrochloride. The assembly process of the button cell is the same as that of the example 1, the obtained negative electrode material is cycled for 200 circles under the current density of 500mA/g, and the capacity is 465mA h/g.
Example 6
The other conditions were the same as in example 1 except that the sodium salt added in the first step was sodium carbonate. The assembly process of the button cell is the same as that of the example 1, and the obtained negative electrode material has a capacity of 512mA h/g after 200 cycles under the current density of 500mA/g, and has good capacity retention rate.
Example 7
The other conditions were the same as in example 1 except that the citric acid added in the first step was 8 mmol. The assembly process of the button cell was the same as in example 1, and the obtained negative electrode material had a capacity of 468mA h/g after 200 cycles at a current density of 500 mA/g.
Comparative example 1
And a commercial SnO2 material (Aladdin reagent) is used as a negative electrode material of the lithium ion battery to assemble the button battery. The assembly process of button cell is the same as example 1, fig. 4 is commercial SnO2Cycling performance of the material at a current density of 500 mA/g: purchased SnO in a cyclical Process2The discharge specific capacity of the material is rapidly attenuated, and the specific capacity after 200 cycles of 200 cycles under the current density of 500mA/g is only 95mA h/g.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and these substitutions and modifications should be considered to fall within the scope of the invention.
Claims (10)
1. A preparation method of a tin-carbon composite material for a lithium ion battery cathode is characterized by comprising the following steps:
s1, dissolving a tin source in water, adding water-soluble inorganic salt and a carbon source, and physically mixing to form a uniformly mixed solution;
s2, freeze-drying the solution obtained in the step S1 to obtain white powder;
s3, grinding the white powder dried in the step S2, and carrying out carbonization treatment under a protective atmosphere to obtain black powder;
s4, washing and drying the black powder obtained in the step S3 to obtain honeycomb SnO2@ C composite material.
2. The method of claim 1, wherein the tin source comprises SnCl4·5H2O and Na2SnO3One kind of (1).
3. The method of claim 1, wherein the water-soluble inorganic salt forms a template of a cellular porous morphology, the water-soluble inorganic salt comprising a sodium salt, a potassium salt, the sodium salt comprising one of sodium chloride, sodium sulfate, and sodium carbonate; the potassium salt comprises one of potassium chloride and potassium carbonate.
4. The method of claim 1, wherein the carbon source comprises one of citric acid, dopamine hydrochloride, glucose, and melamine polyphosphate.
5. The method of claim 1, wherein the lyophilization temperature in step S2 is-30 to-60 ℃, and the drying time is 24 to 72 hours.
6. The method of claim 1, wherein the protective atmosphere is an inert gas.
7. The method according to claim 1, wherein the carbonization treatment in step S3 is performed by: raising the temperature from room temperature to 450-750 ℃ at a heating rate of 1-5 ℃/min, preserving the temperature for 2-5 h, and naturally cooling to the room temperature.
8. The method according to claim 1, wherein the drying in step S4 is vacuum drying at 60-100 ℃ for 10-24 h.
9. A tin-carbon composite material for a negative electrode of a lithium ion battery is characterized by comprising: after freeze drying, the cellular porous shape provided by water-soluble inorganic salt is taken as a template, and nano tin oxide particles are attached to the carbon nano-sheet to form SnO with a three-dimensional cellular three-dimensional structure2@ C composite material.
10. The tin-carbon composite material for a negative electrode of a lithium ion battery according to claim 9, wherein the size of the tin oxide particle is 100 to 300nm, and the pore diameter of the honeycomb is 0.2 to 1 μm.
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Cited By (7)
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| CN111477860A (en) * | 2020-05-11 | 2020-07-31 | 广西师范大学 | Preparation method of GaSn/NC composite material |
| CN112479258A (en) * | 2020-12-17 | 2021-03-12 | 陕西科技大学 | Molybdenum disulfide-carbon hollow sphere and preparation method and application thereof |
| CN112599738A (en) * | 2020-12-14 | 2021-04-02 | 大连海事大学 | Tin-carbon composite material for lithium ion battery cathode and preparation method and application thereof |
| CN112952060A (en) * | 2021-02-26 | 2021-06-11 | 广东工业大学 | Vanadium diselenide/carbon cellulose composite material and preparation method and application thereof |
| CN114314644A (en) * | 2021-11-23 | 2022-04-12 | 惠州锂威新能源科技有限公司 | Preparation method of SnO2@ C-P composite electrode material |
| CN114551833A (en) * | 2022-02-23 | 2022-05-27 | 安徽师范大学 | Coral-shaped tin dioxide @ carbon composite nanomaterial and preparation method thereof, semi-solid negative electrode slurry and semi-solid lithium ion battery |
| CN114944480A (en) * | 2022-06-12 | 2022-08-26 | 青海师范大学 | Preparation method of honeycomb porous tin-carbon composite material |
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Application publication date: 20201204 |