CN114094074A - Carbon cloth supported tin disulfide @ carbon flexible composite electrode material and preparation method and application thereof - Google Patents
Carbon cloth supported tin disulfide @ carbon flexible composite electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a carbon cloth supported tin disulfide @ carbon flexible composite electrode material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) dissolving precursors of sulfur and tin into a solvent to obtain a precursor solution, adding a carbon source into the precursor solution, and uniformly stirring to obtain a dispersion liquid; (2) soaking the cleaned and dried carbon cloth into the dispersion liquid, and carrying out solvothermal reaction after soaking; (3) and after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material. The invention also discloses an application of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material in preparation of a sodium ion battery. The carbon cloth supported tin disulfide @ carbon flexible composite electrode material prepared by the invention does not need a binder and a conductive agent, can be directly used as an electrode material, can greatly reduce the mass ratio of inactive substances of a battery, and improves the energy density of the battery.
Description
Technical Field
The invention relates to the technical field of energy and new materials, in particular to a carbon cloth supported tin disulfide @ carbon flexible composite electrode material and a preparation method and application thereof.
Background
Among the novel battery systems, sodium ion batteries are one of the promising battery systems to replace lithium ion batteries because of abundant sources and low price of raw material sodium resources.
However, compared with lithium ion batteries, the radius of sodium ions is larger, and the sodium ions are more difficult to be embedded and removed in battery materials, so that the electrochemical reaction kinetics of the sodium ion batteries is slower, and many cathode materials suitable for the lithium ion batteries cannot be directly used as the cathode materials of the sodium ion batteries. In recent years, negative electrode materials suitable for sodium ion batteries have been widely studied.
In the system of the cathode material, tin-based material (Sn, SnO)2，SnS，SnS2SnSe, etc.) is considered to be an ideal negative electrode material for sodium-ion batteries because of its high theoretical capacity, low cost and low toxicity. The electrochemical reaction process of tin and sodium is alloying reaction (Sn + xNa)++xe-→NaxSn) which is accompanied by a sharp volume expansion, and thus pure tin has poor electrochemical performance as a negative electrode of a sodium ion battery.
Compared with pure tin, tin sulfide is used as a negative electrode material, and SnS firstly occurs in the first sodium intercalation process of the tin sulfidexIrreversibly converted to Na2S and Sn (SnS)x+2xNa++2xe-→Sn 2x-+Na2S, x ═ 1, 2), this process produces Na2S can be used as a buffer layer to relieve volume expansion of tin in alloying reaction. However, the subsequent reaction is consistent with the sodium treatment of tin, and there is a problem of volume expansion.
The nano-structured tin-based sulfide is designed aiming at the problem of volume expansion of a tin-based sulfide cathode, because the stress relaxation of a nano-structured material is faster than that of a material with a large number of crystal domain sizes, and compared with a bulk material, the diffusion distance of sodium ions in nano crystals is shorter, so that the nano-structured tin-based sulfide has higher reaction power. For example, the preparation of tin sulfide nano thin sheets, tin sulfide hollow nanospheres, nanoflowers and other special structures can expose more surfaces and defects of the material and promote the diffusion and migration of sodium ions in the structure.
On the other hand, tin sulfide (SnS and SnS)2) The conductive carbon composite is another method for improving the electrochemical performance of tin sulfide. If a graphene structure is introduced to induce growth of flake stannous sulfide (ACS appl. mater. interfaces 2019,11,41363-41373) with small size, the storage performance of sodium ions can be obviously improved compared with that of a bulk material. A carbon-coated stannous sulfide nanotube (Angew. chem. int. Ed.2017,56, 12202-.
The tin-based material designed above can not be directly used as an electrode material generally, and needs to be further coated on a current collector through a conductive agent and a binder, so that the quality of inactive substances is greatly increased, and the energy density of a battery is reduced.
The flexible electrode material has the advantages of flexibility, no current collector, no conductive agent and the like, and has attracted much attention in recent years when being applied to wearable electronic products and flexible devices.
Disclosure of Invention
The invention provides a carbon cloth supported tin disulfide @ carbon flexible composite electrode material and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of a carbon cloth supported tin disulfide @ carbon flexible composite electrode material comprises the following steps:
(1) dissolving precursors of sulfur and tin into a solvent to obtain a precursor solution, adding a carbon source into the precursor solution, and uniformly stirring to obtain a dispersion liquid;
(2) soaking the cleaned and dried carbon cloth into the dispersion liquid, and carrying out solvothermal reaction after soaking;
(3) and after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material.
Preferably, in the step (1), the molar ratio of the sulfur element to the tin element in the dispersion is 1: 0.01-100; more preferably 1: 0.05 to 16; still more preferably 1: 0.1-6.
In the dispersion liquid, the concentration influence of precursors of sulfur and tin and a carbon source has certain influence on the performance of the electrode material.
Preferably, the concentration of the sulfur precursor in the precursor solution is 0.001-1.0 mol/L; further preferably 0.005 to 0.8 mol/L; more preferably 0.01 to 0.6 mol/L.
Preferably, in the precursor solution, the concentration of the precursor of tin is 0.001-1.0 mol/L; further preferably 0.002 to 0.8 mol/L; more preferably 0.005 to 0.6 mol/L.
Preferably, the concentration of the carbon source in the dispersion liquid is 0.001-1.0 mol/L; further preferably 0.002 to 0.8 mol/L; more preferably 0.003 to 0.6 mol/L.
Preferably, in the step (1), the precursor of sulfur is thioacetamide; the precursor of the tin is tin tetrachloride; the carbon source is sucrose; the solvent is isopropanol.
In the step (2), the cleaning method of the carbon cloth comprises the following steps: soaking the carbon cloth in dilute hydrochloric acid solution for 0.1-48h, cleaning to remove surface impurities, cleaning with deionized water, and drying.
The concentration of the dilute hydrochloric acid is 0.01-5 mol/L; further preferably 0.01 to 3 mol/L; more preferably 0.02 to 2 mol/L.
The soaking time of the carbon cloth in the dilute hydrochloric acid solution is preferably 0.5-40 h; more preferably 1-30 h.
In order to fully infiltrate the precursors of sulfur and tin and the carbon source onto the carbon cloth, preferably, in the step (2), the carbon cloth is infiltrated in the dispersion liquid for 0.1 to 10 hours and then subjected to solvothermal reaction; the soaking time is further preferably 0.2-8 h; the soaking time is more preferably 0.3 to 6 hours.
In the step (2), when the temperature of the solvothermal reaction is too low, the relevant substances cannot be synthesized, preferably, in the step (2), the temperature of the solvothermal reaction is 100-220 ℃; further preferably 120-200 ℃; more preferably 140-.
In the step (2), when the solvothermal reaction time is too short, the relevant substance cannot be synthesized, and when the reaction time is too long, the particles of the relevant substance are too large, so that the performance of the electrode material is reduced.
Preferably, in the step (2), the solvothermal reaction time is 0.1-48 h; further preferably 0.5-40 h; more preferably 1-30 h.
The invention also provides the carbon cloth supported tin disulfide @ carbon flexible composite electrode material prepared by the preparation method.
The invention also discloses an application of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material in preparation of a sodium ion battery.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method provided by the invention realizes that the tin disulfide @ carbon uniformly grows on the surface of the carbon cloth in one step. The tin disulfide and carbon are evenly coated on the surface of the carbon cloth, the introduction of the carbon further increases the charge transmission capability of the tin disulfide, the electrochemical activity of the tin disulfide can be improved by the porous wrinkled structure, and the shedding of the electrode material caused by severe volume change is inhibited.
In addition, the self-supporting electrode prepared by the invention does not need a binder and a conductive agent, can be directly used as an electrode material, can greatly reduce the mass ratio of inactive substances of the battery, and improves the energy density of the battery.
Drawings
FIG. 1 is an SEM image of a carbon cloth supported tin disulfide @ carbon electrode material prepared in example 1; wherein (b) is a partial enlarged view of (a);
FIG. 2 is an XRD pattern of carbon cloth supported tin disulfide @ carbon electrode material prepared in example 1;
FIG. 3 shows the current density of 0.1Ag of the carbon cloth supported tin disulfide @ carbon electrode material prepared in example 1-1Time cycle stability profile;
FIG. 4 shows the current density of 1Ag of the carbon cloth supported tin disulfide @ carbon electrode material prepared in example 1-1Time cycle stability profile;
fig. 5 is a graph of rate performance of the carbon cloth supported tin disulfide @ carbon electrode material prepared in example 1.
Detailed Description
Example 1
Soaking the carbon cloth in 20mL of 1mol/L HCl solution for 24 hours, cleaning to remove surface impurities, cleaning with deionized water, and drying in an oven at 80 ℃ for later use. 0.032g of thioacetamide and 0.043g of SnCl are taken4*5H2Adding O into 35mL of isopropanol to be completely dissolved, adding 0.02g of cane sugar, stirring to be in a uniform state, pouring the solution into a 50mL inner container of a hydrothermal reaction kettle, putting carbon cloth into the reaction kettle, soaking for 4 hours, transferring the hydrothermal reaction kettle into an oven to perform one-step solvothermal reaction, wherein the reaction temperature is 180 ℃, the reaction time is 24 hours, after the reaction is finished, taking out the carbon cloth by using tweezers, washing with deionized water and ethanol for 5 times respectively, and drying in vacuum at 80 ℃ to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material.
Phase characterization is performed on the carbon cloth supported tin disulfide @ carbon composite material prepared in the embodiment, fig. 1 is an SEM of the carbon cloth supported tin disulfide @ carbon composite material, it can be seen that an obvious carbon cloth fiber appearance is obtained, the fiber surface is uniformly covered by rough substances, and it can be observed from an enlarged SEM picture (fig. 1 (b)) that surface substances are aggregated by sheet-like substances with staggered folds, and the composite material has typical characteristics of a layered material. EDS element characterization is carried out on the carbon cloth supported tin disulfide @ carbon composite material, and an EDS element map proves that the surface of the material has carbon element distribution, so that the existence of the carbon material is proved. From the XRD of the carbon cloth supported tin disulfide @ carbon composite material shown in FIG. 2, it can be analyzed that the main diffraction peak corresponds to SnS2Characteristic peak of (2). The (001), (100), (101), (110) and other crystal planes are respectively corresponded. In addition, no obvious carbon diffraction peak exists, and the carbon cloth and the synthesized carbon at the temperature are both amorphous carbon.
And cutting the carbon cloth-supported tin disulfide @ carbon composite electrode material into a wafer with the diameter of 14mm, and assembling the wafer into the R2032 type button cell by using the wafer as a working electrode. With 1MNaClO4The PC solution + 5% Fluorinated Ethylene Carbonate (FEC) additive was the electrolyte and glass fiber Whatman, GF/D) was the septum.
Constant current charge and discharge test is carried out at room temperature in a voltage rangeThe circumference is 0.01-2.50V, and two modes of circulation and multiplying power are adopted. The circulation is 60 times at 0.1A/g current; the multiplying power is respectively tested by adopting currents of 0.3A/g, 0.5A/g, 1A/g, 2A/g and 0.3A/g in sequence, and each current density is tested for 10 times. As a result, as shown in FIG. 3, it can be seen that the first discharge specific capacity of the material was 917mAhg-1The first charging specific capacity is 510mAhg-1The first coulombic efficiency was 55.6%. After 60 times of circulation, the charging specific capacity of the material is 475mAhg-1The capacity retention was first 93%. When the current density is 1Ag-1In the meantime (figure 4), the cycle is 100 times, and the reversible specific capacity still has 371mAhg-1. The rate capability is shown in FIG. 5, and it can be seen that when the current density is 1Ag-1And 2Ag-1Still has 274mAhg-1And 256mAhg-1The specific capacity and the rate capability are stable.
Example 2
Soaking the carbon cloth in 20mL of 2mol/L HCl solution for 24h, cleaning to remove surface impurities, cleaning with deionized water, and drying in an oven at 80 ℃ for later use. 0.064g thioacetamide and 0.056g SnCl were taken4*5H2Adding O into 75mL of isopropanol to be completely dissolved, adding 0.054g of cane sugar, stirring to be in a uniform state, pouring the solution into a 100mL inner container of a hydrothermal reaction kettle, putting carbon cloth into the reaction kettle, soaking for 5 hours, transferring the hydrothermal reaction kettle into an oven to perform one-step solvothermal reaction at 200 ℃ for 10 hours, taking out the carbon cloth by using tweezers after the reaction is finished, washing the carbon cloth for 5 times by using deionized water and ethanol, and drying in vacuum at 80 ℃ to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material.
And cutting the carbon cloth-supported tin disulfide @ carbon composite electrode material into a wafer with the diameter of 14mm, and assembling the wafer into the R2032 type button cell by using the wafer as a working electrode. With 1MNaClO4The PC solution + 5% Fluorinated Ethylene Carbonate (FEC) additive was the electrolyte and glass fiber Whatman, GF/D) was the septum.
Constant current charge and discharge tests are carried out at room temperature, the voltage range is 0.01-2.50V, and two modes of circulation and multiplying power are adopted. The cycle is carried out for 60 times at 0.1A/g current, and the first discharge specific capacity of the material is 756mAhg-1The first charging specific capacity is 433mAhg-1The first coulombic efficiency was 57.2%. After 60 times of circulation, the charging specific capacity of the material is 425mAhg-1The capacity retention was 98% of the first time.
Example 3
Soaking the carbon cloth in 20mL of 1.5mol/L HCl solution for 20h, cleaning to remove surface impurities, cleaning with deionized water, and drying in an oven at 80 ℃ for later use. 0.064g thioacetamide and 0.056g SnCl were taken4*5H2Adding O into 75mL of isopropanol to be completely dissolved, adding 0.037g of cane sugar, stirring to be in a uniform state, pouring the solution into a 100mL inner container of a hydrothermal reaction kettle, putting carbon cloth into the reaction kettle, soaking for 5 hours, transferring the hydrothermal reaction kettle into an oven to perform one-step solvothermal reaction at 200 ℃ for 8 hours, taking out the carbon cloth by using tweezers after the reaction is finished, washing the carbon cloth for 5 times by using deionized water and ethanol, and drying in vacuum at 80 ℃ to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material.
And cutting the carbon cloth-supported tin disulfide @ carbon composite electrode material into a wafer with the diameter of 14mm, and assembling the wafer into the R2032 type button cell by using the wafer as a working electrode. With 1MNaClO4The PC solution + 5% Fluorinated Ethylene Carbonate (FEC) additive was the electrolyte and glass fiber Whatman, GF/D) was the septum.
Constant current charge and discharge tests are carried out at room temperature, the voltage range is 0.01-2.50V, and two modes of circulation and multiplying power are adopted. The cycle is carried out for 60 times at 0.1A/g current, and the first discharge specific capacity of the material is 824mAhg-1The first charging specific capacity is 483mAhg-1The first coulombic efficiency was 58.6%. After the cycle is carried out for 60 times, the charging specific capacity of the material is 462mAhg-1The capacity retention was 95.6% of the first time.
According to the embodiment, the invention provides the preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material, the tin disulfide and the carbon are uniformly coated on the surface of the carbon cloth, the introduction of the carbon further increases the charge transmission capability of the tin disulfide, the electrochemical activity of the tin disulfide can be improved by the porous wrinkled structure, and the dropping of the electrode material caused by severe volume change is inhibited. The self-supporting electrode thus maintains a good cyclic stability.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a carbon cloth supported tin disulfide @ carbon flexible composite electrode material is characterized by comprising the following steps:
(1) dissolving precursors of sulfur and tin into a solvent to obtain a precursor solution, adding a carbon source into the precursor solution, and uniformly stirring to obtain a dispersion liquid;
(2) soaking the cleaned and dried carbon cloth into the dispersion liquid, and carrying out solvothermal reaction after soaking;
(3) and after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the carbon cloth supported tin disulfide @ carbon flexible composite electrode material.
2. The method for preparing the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein in the step (1), the molar ratio of sulfur element to tin element in the dispersion liquid is 1: 0.01-100.
3. The preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein the concentration of a sulfur precursor in the precursor solution is 0.001-1.0 mol/L; the concentration of the tin precursor is 0.001-1.0 mol/L.
4. The preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein the concentration of the carbon source in the dispersion liquid is 0.001-1.0 mol/L.
5. The preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein in the step (1), the precursor of sulfur is thioacetamide; the precursor of the tin is tin tetrachloride; the carbon source is sucrose; the solvent is isopropanol.
6. The preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein in the step (2), the cleaning method of the carbon cloth is as follows: soaking the carbon cloth in dilute hydrochloric acid solution for 0.1-48h, cleaning to remove surface impurities, cleaning with deionized water, and drying.
7. The preparation method of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein in the step (2), the carbon cloth is soaked in the dispersion liquid for 0.1-10h and then subjected to solvothermal reaction.
8. The method for preparing the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as claimed in claim 1, wherein in the step (2), the temperature of the solvothermal reaction is 100-220 ℃; the solvothermal reaction time is 0.1-48 h.
9. The carbon cloth supported tin disulfide @ carbon flexible composite electrode material is characterized by being prepared by the preparation method of any one of claims 1-8.
10. The use of the carbon cloth supported tin disulfide @ carbon flexible composite electrode material as defined in claim 9 in the preparation of a sodium ion battery.
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Application publication date: 20220225 |