CN115101725A - Preparation method of silicon nanowire electrode and application of silicon nanowire electrode in lithium ion battery - Google Patents
Preparation method of silicon nanowire electrode and application of silicon nanowire electrode in lithium ion battery Download PDFInfo
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- CN115101725A CN115101725A CN202210790268.4A CN202210790268A CN115101725A CN 115101725 A CN115101725 A CN 115101725A CN 202210790268 A CN202210790268 A CN 202210790268A CN 115101725 A CN115101725 A CN 115101725A
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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
Abstract
The invention discloses a preparation method of a silicon nanowire electrode and application thereof in a lithium ion battery. The invention not only simplifies the loading process of the metal catalyst, but also the silicon nanowire electrode prepared in situ has excellent electrochemical performance; in addition, the raw materials used by the invention are low in price, the preparation process is simple and easy to operate, and the method is suitable for quantitatively producing the silicon nanowire electrode.
Description
Technical Field
The invention belongs to the field of electrochemical energy storage, and particularly relates to a preparation method of a silicon nanowire electrode and application of the silicon nanowire electrode in a lithium ion battery.
Background
Lithium ion batteries have been widely used in the fields of small electronic devices, aerospace, and the like because of their advantages of long service life, high specific capacity, environmental friendliness, and the like, and thus have become one of the most important energy storage systems. Commercial lithium ion batteries generally use layered transition metal oxides as the positive electrode and graphite as the negative electrode. Although the specific capacity of the lithium ion battery can be close to a theoretical value at present, the power and energy density of the traditional lithium ion battery can not meet the requirements of consumers gradually along with the rapid development of electric transportation tools such as new energy automobiles and the like. Crystalline silicon can provide up to 3579mAh g at room temperature -1 The theoretical lithium intercalation capacity of the lithium ion battery is far higher than that of graphite (372mAh g) which is most commonly applied in the current lithium ion battery cathode material -1 ). In addition, the silicon also has the advantages of high storage capacity, environmental friendliness, low production cost and the like. Therefore, the silicon negative electrode has excellent application potential in power batteries requiring large capacity and high energy density, but has problems in that: when lithium ions are completely intercalated into the silicon matrix, the silicon matrix undergoes severe volume expansion (>300%), which leads to pulverization of silicon cathode after charging and discharging for many times, thus leading to loss of electric contact between silicon and current collector and rapid attenuation of battery capacity; the volume effect generated by the silicon cathode in the circulation process can cause repeated fracture-regeneration of an SEI film, and further cause reduction of coulombic efficiency and increase of ion transport resistance of the battery.
Therefore, in order to realize commercial application of the silicon negative electrode, it is a first problem to solve the volume effect thereof. Researchers find that the silicon-based material is subjected to nanocrystallization, so that the overall stress of the silicon cathode can be effectively reduced, and the volume effect is relieved. Among many silicon nanomaterials, silicon nanowires have attracted much attention because of their advantages of large specific surface area, short carrier diffusion path, and good fracture resistance. The silicon nanowire is a typical one-dimensional silicon nanomaterial, and the structure of the silicon nanowire is favorable for axial charge transport and enables the radial migration distance of lithium ions to be short. In addition, the silicon nanowire anode material can effectively utilize the space between wires to avoid electrode failure caused by volume effect. In recent years, many researchers choose to grow silicon nanowires in situ on a substrate with excellent conductivity such as stainless steel, and use the silicon nanowires as the negative electrode of a lithium ion battery [ ACS Nano,2019,13, 2307-2315; adv. mater, 2021,33,2105917], in-situ grown silicon nanowires can not only make good electrical contact with the current collector, but also do not require the use of additional binders. Growing silicon nanowires usually requires the use of metal catalysts, and the most common methods for loading the catalyst onto a current collector are: electron beam evaporation, thermal evaporation, magnetron sputtering, etc. [ adv. energy mater, 2011,1, 1154-; j. Mater. chem.A,2014,2,13859-13867 ]. However, the above methods all require expensive coating equipment, and the preparation process is complicated, so that large-scale production is difficult to realize, thereby limiting practical application of silicon nanowire cathodes.
Disclosure of Invention
The invention provides a preparation method of a silicon nanowire electrode, which is low in cost, simple in preparation process and suitable for quantitative production, and application of the silicon nanowire electrode in a lithium ion battery, and aims to solve the problems that the silicon nanowire electrode is high in production cost, long in period, difficult to produce in batches and the like. The silicon nanowire electrode has excellent electrochemical performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the silicon nanowire electrode comprises the following steps:
step 1: stirring the high-porosity conductive matrix in a metal salt solution for 10-60 minutes, taking out and quickly drying at 80-150 ℃, and loading metal salt nanoparticles on the surface of the conductive matrix;
step 2: heating the high-porosity conductive matrix obtained in the step 1 to 400-900 ℃ in a reducing atmosphere, keeping the temperature for 0-30 minutes, introducing silicon source gas, and maintaining the reaction pressure at 1 × 10 3 ～10 4 Pa, keeping the temperature for 0.5-5 hours, passing through the in-situAnd (4) catalyzing and growing the silicon nanowire to prepare the silicon nanowire electrode.
Preferably, in step 1, the metal salt solution is one or a mixture of several of copper salt, iron salt, nickel salt, titanium salt, manganese salt, cobalt salt and aluminum salt solution. The mass concentration of the metal salt solution is 0.01-20%.
Preferably, in step 1, the high-porosity conductive substrate is one of carbon fiber cloth, carbon paper, graphene paper and stainless steel mesh.
Preferably, in step 2, the reducing atmosphere is one of hydrogen gas and argon-hydrogen mixed gas.
Preferably, in step 2, the silicon source gas is one of silicon tetrahydride and silicon tetrachloride.
The method simplifies the loading process of the catalyst, the silicon nanowire grows on the surface of the high-porosity conductive substrate in situ to directly form the silicon nanowire electrode, and the diameter of the silicon nanowire in the electrode is 10-150 nm.
The optimal reaction temperature of the silicon nanowire electrode prepared by the invention is 600 ℃, and in addition, the diameter of the silicon nanowire can be gradually increased along with the increase of the reaction air pressure. Electrochemical tests show that the silicon nanowire with the smallest diameter has the highest specific capacity and the best cycling stability and rate capability. The lithium ion battery is used as a working electrode in a lithium ion battery and has excellent electrochemical performance.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the metal salt solution is used as a catalyst source, the high-porosity conductive matrix with excellent wettability is used as a substrate, and uniform loading of the catalyst can be realized by stirring, so that the traditional catalyst loading process is simplified.
2. The high-porosity conductive matrix used in the invention can be fully infiltrated with electrolyte, thereby effectively improving the electrochemical performance of the silicon nanowire electrode.
3. The method has the advantages of low price of raw materials, simple preparation process and easy operation, and is suitable for the quantitative production of the silicon nanowire electrode.
Drawings
Fig. 1 is an X-ray diffraction pattern of the silicon nanowire electrode prepared in example 1.
FIG. 2a is a 500-fold scanning electron microscope image of a silicon nanowire electrode prepared in example 1; fig. 2b is a 2000-fold scanning electron microscope image of the silicon nanowire electrode prepared in example 1.
FIG. 3a is a 500-fold scanning electron microscope image of a silicon nanowire electrode prepared in example 2; fig. 3b is a 2000-fold scanning electron microscope image of the silicon nanowire electrode prepared in example 2.
FIG. 4a is a transmission electron microscopy topographic map of the silicon nanowire electrode prepared in example 2; FIG. 4b is the high resolution image of the silicon nanowire electrode prepared in example 2 with transmission electron microscope.
FIG. 5a is a 500-fold scanning electron microscope image of a silicon nanowire electrode prepared in example 3; figure 5b is a 2000-fold scanning electron microscope image of the silicon nanowire electrode prepared in example 3.
FIG. 6a is a 500-fold scanning electron microscope image of a silicon nanowire electrode prepared in example 4; fig. 6b is a 2000-fold scanning electron microscope image of the silicon nanowire electrode prepared in example 4.
FIG. 7 is a plot of the S at 0.1mV for the silicon nanowire electrode prepared in example 2 -1 Cyclic voltammogram for the second cycle at the scan rate.
FIG. 8a is a 500-fold scanning electron microscope image of a silicon nanowire electrode prepared in example 5; fig. 8b is a 2000-fold scanning electron microscope image of the silicon nanowire electrode prepared in example 5.
FIG. 9a is a transmission electron microscope topography of a silicon nanowire electrode prepared in example 5; FIG. 9b is the high resolution image of TEM as prepared in example 5.
Fig. 10 is a scanning electron microscope image of 500 times and 2000 times the silicon nanowire electrode prepared in example 6.
Fig. 11 is a cycle performance curve of the silicon nanowire electrode prepared in example 5 at a magnification of 1C.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1:
step 1, stirring a stainless steel net in a 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, then taking out and quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the stainless steel net;
the X-ray diffraction (XRD) test of the silicon nanowire electrode prepared in this example was performed, and the test result is shown in fig. 1, from which it can be seen that a diffraction peak of crystalline silicon appears in the XRD spectrogram of the electrode, indicating that crystalline silicon is successfully prepared by the method.
The scanning electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 2, which shows that the silicon nanowires uniformly grow on the surface of the stainless steel mesh to form the silicon nanowire electrode.
1mol L of the silicon nanowire electrode prepared in the example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a diaphragm -1 The lithium hexafluorophosphate solution (wherein the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) is used as an electrolyte, and the electrolyte is assembled into a CR2025 button cell in a glove box filled with argon gas for electrochemical performance test.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment under 0.1C is 81.7%, the electrode is subjected to a cycle performance test under the multiplying power of 1C, after 50 charge-discharge cycles, the discharge specific capacity can be kept at 67.4%, and in addition, the coulombic efficiency is always kept at about 99% in the whole cycle process.
Example 2:
step 1, stirring a stainless steel net in a 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, then taking out and quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the stainless steel net;
XRD test is carried out on the silicon nanowire electrode prepared in the embodiment, and the test result shows that a diffraction peak of crystalline silicon appears in an XRD spectrogram of the electrode, which indicates that the crystalline silicon is successfully prepared by the method.
The silicon nanowire electrode prepared in this example was subjected to a scanning electron microscope test, and the test result is shown in fig. 3, which shows that the silicon nanowires uniformly grow on the surface of the stainless steel mesh to form the silicon nanowire electrode.
The transmission electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 4, which shows that the diameter of the silicon nanowire is about 45 nm.
1mol L of the silicon nanowire electrode prepared in the example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a diaphragm -1 The lithium hexafluorophosphate solution (wherein the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) is used as an electrolyte, and the electrolyte is assembled into a CR2025 button cell in a glove box filled with argon gas for electrochemical performance test.
The silicon nanowire electrode prepared in the example is 0.1mV s -1 The cyclic voltammogram of the second cycle at the scan rate is shown in fig. 7, from which it can be seen that the cyclic voltammogram shows two oxidation peaks and one reduction peak.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment at 0.1C is 80.8%, the electrode is subjected to a cycle performance test at a multiplying power of 1C, after 50 charge-discharge cycles, the discharge specific capacity can still be kept at 75.8%, and in addition, the coulombic efficiency is always kept at about 99% in the whole cycle process.
Example 3:
step 1, stirring a stainless steel net in a 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, then taking out and quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the stainless steel net;
XRD test is carried out on the silicon nanowire electrode prepared in the embodiment, and the test result shows that a diffraction peak of crystalline silicon appears in an XRD spectrogram of the electrode, which indicates that the crystalline silicon is successfully prepared by the method.
The scanning electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 5, which shows that the silicon nanowires uniformly grow on the surface of the stainless steel mesh to form the silicon nanowire electrode.
1mol L of the silicon nanowire electrode prepared in the example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a diaphragm -1 The lithium hexafluorophosphate solution (in which the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) as an electrolyte was assembled into a CR2025 button cell in an argon-filled glove box for electrochemical performance testing.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment at 0.1C is 78.3%, the electrode is subjected to a cycle performance test at a multiplying power of 1C, after 50 charge-discharge cycles, the discharge specific capacity can be kept at 71.6%, and in addition, the coulombic efficiency is always kept at about 99% in the whole cycle process.
Example 4:
step 1, stirring carbon fiber cloth in 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, taking out and quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the carbon fiber cloth;
XRD test is carried out on the silicon nanowire electrode prepared in the embodiment, and the test result shows that a diffraction peak of crystalline silicon appears in an XRD spectrogram of the electrode, which indicates that the crystalline silicon is successfully prepared by the method.
The silicon nanowire electrode prepared in this example was subjected to a scanning electron microscope test, and the test result is shown in fig. 6, which shows that the silicon nanowires uniformly grow on the surface of the carbon fiber to form the silicon nanowire electrode.
1mol L of the silicon nanowire electrode prepared in the example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a diaphragm -1 The lithium hexafluorophosphate solution (wherein the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) is used as an electrolyte, and the electrolyte is assembled into a CR2025 button cell in a glove box filled with argon gas for electrochemical performance test.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment under 0.1C is 86.3%, the electrode is subjected to a cycle performance test under the multiplying power of 1C, after 50 times of charge-discharge cycles, the discharge specific capacity of the electrode can be kept at 84.7%, and in addition, the coulombic efficiency of the electrode is always kept at about 99% in the whole cycle process.
Example 5:
step 1, stirring a stainless steel mesh in a 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, taking out, quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the stainless steel mesh;
XRD test is carried out on the silicon nanowire electrode prepared in the embodiment, and the test result shows that a diffraction peak of crystalline silicon appears in an XRD spectrogram of the electrode, which indicates that the crystalline silicon is successfully prepared by the method.
The scanning electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 8, which shows that the silicon nanowires uniformly grow on the surface of the stainless steel mesh to form the silicon nanowire electrode.
The transmission electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 9, which shows that the diameter of the silicon nanowire is about 25 nm.
1mol L of the silicon nanowire electrode prepared in the example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a diaphragm -1 The lithium hexafluorophosphate solution (wherein the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) is used as an electrolyte, and the electrolyte is assembled into a CR2025 button cell in a glove box filled with argon gas for electrochemical performance test.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment at 0.1C is 81.3%, the cycle performance of the electrode at the rate of 1C is shown in fig. 11, after 50 times of charge-discharge cycles, the specific discharge capacity of the electrode can be kept at 87.2%, and in addition, the coulombic efficiency of the electrode in the whole cycle process is always kept at about 99%.
Example 6:
step 1, stirring a stainless steel net in a 0.2% copper chloride solution (acetone as a solvent) for 15 minutes, then taking out and quickly drying at 100 ℃, and loading copper chloride nanoparticles on the surface of the stainless steel net;
XRD test is carried out on the silicon nanowire electrode prepared in the embodiment, and the test result shows that a diffraction peak of crystalline silicon appears in an XRD spectrogram of the electrode, which indicates that the crystalline silicon is successfully prepared by the method.
The scanning electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result is shown in fig. 10, which shows that the silicon nanowires uniformly grow on the surface of the stainless steel mesh to form the silicon nanowire electrode.
The transmission electron microscope test was performed on the silicon nanowire electrode prepared in this example, and the test result showed that the diameter of the silicon nanowire was about 100 nm.
1mol L of the silicon nanowire electrode prepared in this example as a working electrode, a metal lithium sheet as a counter electrode, a polypropylene film as a separator -1 The lithium hexafluorophosphate solution (wherein the solvent is a mixture of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1) is used as an electrolyte, and the electrolyte is assembled into a CR2025 button cell in a glove box filled with argon gas for electrochemical performance test.
The first-cycle coulombic efficiency of the silicon nanowire electrode prepared in the embodiment at 0.1C is 76.2%, the electrode is subjected to a cycle performance test at a multiplying power of 1C, after 50 charge-discharge cycles, the discharge specific capacity can be kept at 71.7%, and in addition, the coulombic efficiency is always kept at about 99% in the whole cycle process.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A preparation method of a silicon nanowire electrode is characterized by comprising the following steps:
step 1: stirring the high-porosity conductive matrix in a metal salt solution for 10-60 minutes, taking out, quickly drying at 80-150 ℃, and loading metal salt nanoparticles on the surface of the high-porosity conductive matrix;
step 2: heating the high-porosity conductive matrix obtained in the step 1 to 400-900 ℃ in a reducing atmosphere, keeping the temperature for 0-30 minutes, introducing silicon source gas, and maintaining the reaction pressureForce 1X 10 3 ～10 4 Pa, keeping the temperature for 0.5-5 hours, and growing the silicon nanowire through in-situ catalysis to prepare the silicon nanowire electrode.
2. The method of claim 1, wherein:
in the step 1, the metal salt solution is one or a mixture of more of copper salt, iron salt, nickel salt, titanium salt, manganese salt, cobalt salt and aluminum salt solution; the mass concentration of the metal salt solution is 0.01-20%.
3. The method of claim 1, wherein:
in the step 1, the high-porosity conductive substrate is one of carbon fiber cloth, carbon paper, graphene paper and a stainless steel net.
4. The method of claim 1, wherein:
in the step 2, the reducing atmosphere is one of hydrogen and argon-hydrogen mixed gas.
5. The method of claim 1, wherein:
in step 2, the silicon source gas is one of silicon tetrahydride and silicon tetrachloride.
6. The method of claim 1, wherein:
the diameter of the silicon nanowire electrode is 10-150 nm.
7. The method of claim 1, wherein:
in step 2, the reaction temperature was 600 ℃.
8. Use of a silicon nanowire electrode prepared according to the preparation method of any one of claims 1 to 7, characterized in that:
the silicon nanowire electrode is used as a working electrode of a lithium ion battery.
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