CN111081983A - Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery - Google Patents
Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery Download PDFInfo
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- CN111081983A CN111081983A CN201911361700.2A CN201911361700A CN111081983A CN 111081983 A CN111081983 A CN 111081983A CN 201911361700 A CN201911361700 A CN 201911361700A CN 111081983 A CN111081983 A CN 111081983A
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- 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
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M4/00—Electrodes
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- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a Co9S8Cutting a self-supporting substrate carbon felt, placing the cut self-supporting substrate carbon felt in a mixed solution of concentrated nitric acid and hydrogen peroxide, standing in a dark place, cleaning and drying the self-supporting substrate carbon felt to obtain a carbon felt sheet A; adding cobalt chloride into deionized water, stirring and dissolving, and then adding ethylenediamine to obtain a solution C; adding thioacetamide into absolute ethyl alcohol with the same volume as deionized water, stirring and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E; immersing the carbon felt A in the solution E and standing to obtain a carbon felt B; placing the carbon felt B into a porcelain boat, placing the porcelain boat into a tubular atmosphere furnace, and calcining the porcelain boat in the tubular atmosphere furnaceBurning and cooling to room temperature to obtain Co9S8A self-supporting cathode of the carbon felt sodium ion battery; the method does not adopt a coating process and has short time consumption.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and relates to Co9S8A preparation method of a self-supporting cathode of a carbon felt sodium ion battery.
Background
Lithium ion batteries have become one of the most interesting energy storage devices in recent years due to their advantages of light weight, small size, high operating voltage, high capacity, long cycle life, etc. Due to the large scale use, the storage of lithium resources on earth is also facing depletion. And the sodium resource has large storage capacity on the earth, abundant resources and easy acquisition, so the preparation cost of the sodium resource is lower than that of a lithium ion battery. Meanwhile, the lithium ion battery has many similarities with the lithium as the I main group element in the periodic table of elements in properties, and the sodium ion battery gradually becomes a research hotspot in recent years due to the characteristics of rich raw material reserves, low price, environmental friendliness and the like, and is considered as an ideal choice for the next generation of energy storage and power batteries.
With the progress of science and technology, the performance requirement on the material is higher and higher, and the performance of the electrode plate of the traditional single material cannot meet the actual requirement, so that people are promoted to research and prepare the composite material, and the purpose of improving the performance is achieved. At present, the composite material is increasingly used as a battery electrode, and has certain advantages in the aspect of electrochemical performance. The selection of a suitable substrate, reaction mode, and reaction conditions determine the performance of the electrode. However, the preparation of the composite material also has certain problems, and a coating process is generally adopted in the preparation process of the electrode plate, so that the time is long.
Disclosure of Invention
The invention aims to provide Co without adopting a film coating process9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery is short in time consumption.
The invention is realized by the following technical scheme:
co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery comprises the following steps:
step 1: placing the carbon felt in a mixed solution of concentrated nitric acid and hydrogen peroxide, standing in a dark place, and then cleaning and drying the carbon felt to obtain a carbon felt sheet A;
step 2: adding 1.2-2 g of cobalt chloride and 5-10 mL of ethylenediamine into 20-30 mL of deionized water, stirring and dissolving to obtain a solution C; adding 1-1.5 g of thioacetamide into absolute ethyl alcohol with the same volume as that of deionized water, stirring and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E and standing to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat, placing the porcelain boat into a tubular atmosphere furnace, calcining at 300-700 ℃, and cooling to room temperature to obtain Co9S8The/carbon felt sodium ion battery self-supporting negative electrode.
Further, the thickness of the carbon felt in the step 1 is 1mm, and the carbon felt is cut into 4 multiplied by 3cm and then placed in a mixed solution of concentrated nitric acid and hydrogen peroxide.
Further, the volume ratio of the concentrated nitric acid to the hydrogen peroxide in the mixed solution in the step 1 is 1: 1-3; standing in dark for 24-48 h.
Further, in the step 1, deionized water and absolute ethyl alcohol are respectively used for cleaning for 3-5 times, and the drying is carried out for 3-6 hours at 60-100 ℃ in a vacuum environment.
Further, the stirring in the step 2 is magnetic stirring at a rotating speed of 400-600 r/min for 1-2 hours.
Further, heating the solution E to 60-100 ℃ in the standing process in the step 3, and keeping the temperature for 12-24 hours.
Further, the calcination in the step 4 is to heat the mixture from room temperature to 300-700 ℃ at a heating rate of 5-10 ℃/min and keep the temperature for 2-4 h.
Further, in the step 4, air in the tubular atmosphere furnace is replaced by inert gas before calcination, the inert gas is kept to circulate in the calcination process, and the air pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0-0.05 Mpa in the calcination heat preservation stage.
Further, the replacement process comprises the steps of inflating the tubular atmosphere furnace for 20min at the flow rate of 70-150 sccm, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 2-5 times.
Furthermore, the flow rate of the inert gas is 300-800 sccm.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a Co9S8The preparation method of the self-supporting cathode of the carbon felt sodium ion battery adopts the carbon felt as a self-supporting body, and the carbon felt has larger specific surface area and can load more active substances; the carbon nanofibers forming the carbon felt are mutually staggered and intertwined to form a huge porous network, so that the volume expansion in the charge and discharge process can be effectively relieved, and the transmission of ions is facilitated; meanwhile, the carbon felt is used as a self-supporting body, so that a coating process in the electrode plate preparation process is omitted, active substances and electrodes are not affected, the preparation process is shortened, the consumed time is short, and the preparation efficiency is improved; the preparation method mainly relates to the procedures of immersing the carbon felt A in the solution E for standing and calcining the carbon felt B, and is simple, easy to control and environment-friendly.
Furthermore, the invention synthesizes nano-sized Co under the liquid phase condition by two-step heating treatment9S8Heat treatment in a subsequent atmosphere furnace to strengthen Co9S8The carbon felt and the carbon felt are combined, the stability of chemical bonds is improved, the carbon felt and the carbon felt can be tightly combined in the charging and discharging process, and the cycle stability and the rate capability of the composite electrode material are improved.
Drawings
FIG. 1 is an XRD pattern of the product prepared in example 1;
FIG. 2 is an SEM photograph of a product of example 1;
FIG. 3 is an SEM image of carbon mat A during preparation of example 1;
FIG. 4 is a graph of cycle test performance of the product prepared in example 1.
Detailed Description
Specific examples are given below.
Example 1
Co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery comprises the following steps:
step 1: cutting a carbon felt with the thickness of 1mm into carbon felt pieces of 4 multiplied by 3cm, and placing the carbon felt pieces in a volume ratio of 1:1, standing for 24 hours in a dark place, respectively cleaning for 4 times by using deionized water and absolute ethyl alcohol, and drying for 3 hours at 100 ℃ in a vacuum environment to obtain a carbon felt A;
step 2: adding 1.2g of cobalt chloride and 5mL of ethylenediamine into 25mL of deionized water, magnetically stirring for 2 hours at the rotating speed of 400r/min, and dissolving to obtain a solution C; adding 1g of thioacetamide into 25mL of absolute ethyl alcohol, magnetically stirring for 2h at the rotating speed of 400r/min, and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E, standing, heating the solution E to 60 ℃, and preserving heat for 24 hours to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat and placing the porcelain boat in a tubular atmosphere furnace, introducing inert gas into the tubular atmosphere furnace to check the air tightness of the tubular atmosphere furnace, inflating the tubular atmosphere furnace for 20min at the flow of 120sccm after ensuring the sealing of the tubular atmosphere furnace, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 3 times, thereby replacing the air in the tubular atmosphere furnace with inert gas. Then heating to 500 ℃ at the heating rate of 5 ℃/min and preserving heat for 2h for calcination; wherein, the flow of inert gas is kept to be 300sccm in the calcining process, and the pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0Mpa in the calcining heat preservation stage; then cooling to room temperature to obtain Co9S8The/carbon felt sodium ion battery self-supporting negative electrode.
As can be seen from FIG. 1, the XRD pattern of the product prepared by the invention, the product and Co with PDF number of 65-17659S8And correspondingly.
As can be seen from fig. 2 and 3, the product prepared by the invention grows on the carbon felt a in a three-dimensional nano sheet structure.
As can be seen from FIG. 4, the product prepared by the invention can reach 586mAh/g after circulating for 200 circles under the current density of 0.1A/g, and the product is proved to have good circulating stability.
Example 2
Co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery comprises the following steps:
step 1: cutting a carbon felt with the thickness of 1mm into carbon felt pieces of 4 multiplied by 3cm, and placing the carbon felt pieces in a volume ratio of 1: 2, standing for 36h in a dark place in the mixed solution of concentrated nitric acid and hydrogen peroxide, respectively cleaning for 5 times by using deionized water and absolute ethyl alcohol, and drying for 5h at 80 ℃ in a vacuum environment to obtain a carbon felt A;
step 2: adding 1.5g of cobalt chloride and 8mL of ethylenediamine into 30mL of deionized water, magnetically stirring for 1.5h at the rotating speed of 500r/min, and dissolving to obtain a solution C; adding 1.2g of thioacetamide into 30mL of absolute ethyl alcohol, magnetically stirring for 1.5h at the rotating speed of 500r/min, and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E, standing, heating the solution E to 80 ℃, and preserving heat for 18 hours to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat and placing the porcelain boat in a tubular atmosphere furnace, introducing inert gas into the tubular atmosphere furnace to check the air tightness of the tubular atmosphere furnace, inflating the tubular atmosphere furnace for 20min at the flow of 100sccm after ensuring the sealing of the tubular atmosphere furnace, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 4 times, thereby replacing the air in the tubular atmosphere furnace with inert gas. Then heating to 600 ℃ at the heating rate of 8 ℃/min and preserving heat for 2h for calcination; wherein, the flow of inert gas is kept to be 600sccm in the calcining process, and the pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0.05Mpa in the calcining heat preservation stage; then cooling to room temperature to obtain Co9S8The/carbon felt sodium ion battery self-supporting negative electrode.
Example 3
Co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery comprises the following steps:
step 1: cutting a carbon felt with the thickness of 1mm into carbon felt pieces of 4 multiplied by 3cm, and placing the carbon felt pieces in a volume ratio of 1: 3, standing for 48h in a dark place in the mixed solution of concentrated nitric acid and hydrogen peroxide, respectively cleaning for 3 times by using deionized water and absolute ethyl alcohol, and drying for 6h at 60 ℃ in a vacuum environment to obtain a carbon felt A;
step 2: adding 2g of cobalt chloride and 10mL of ethylenediamine into 20mL of deionized water, and magnetically stirring for 1 hour at the rotating speed of 600r/min and dissolving to obtain a solution C; adding 1.5g of thioacetamide into 20mL of absolute ethyl alcohol, magnetically stirring for 1h at the rotating speed of 600r/min, and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E, standing, heating the solution E to 100 ℃, and keeping the temperature for 12 hours to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat and placing the porcelain boat in a tubular atmosphere furnace, introducing inert gas into the tubular atmosphere furnace to check the air tightness of the tubular atmosphere furnace, inflating the tubular atmosphere furnace for 20min at a flow of 70sccm after ensuring that the tubular atmosphere furnace is sealed, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 5 times, thereby replacing the air in the tubular atmosphere furnace with inert gas. Then heating to 700 ℃ at the heating rate of 10 ℃/min and preserving heat for 2h for calcination; wherein, the inert gas is kept to flow at the flow rate of 800sccm in the calcining process, and the pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0.02Mpa in the calcining heat preservation stage; then cooling to room temperature to obtain Co9S8The/carbon felt sodium ion battery self-supporting negative electrode.
Example 4
Co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery comprises the following steps:
step 1: cutting a carbon felt with the thickness of 1mm into carbon felt pieces of 4 multiplied by 3cm, and placing the carbon felt pieces in a volume ratio of 1: 2, standing the mixture solution of concentrated nitric acid and hydrogen peroxide for 30 hours in a dark place, respectively cleaning the mixture solution for 4 times by using deionized water and absolute ethyl alcohol, and drying the mixture solution for 4 hours at 70 ℃ in a vacuum environment to obtain a carbon felt A;
step 2: adding 1.2g of cobalt chloride and 5mL of ethylenediamine into 25mL of deionized water, magnetically stirring for 1.2h at the rotating speed of 550r/min, and dissolving to obtain a solution C; adding 1g of thioacetamide into 25mL of absolute ethyl alcohol, magnetically stirring for 1.2h at the rotating speed of 550r/min, and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E, standing, heating the solution E to 80 ℃, and keeping the temperature for 15 hours to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat and placing the porcelain boat in a tubular atmosphere furnace, introducing inert gas into the tubular atmosphere furnace to check the air tightness of the tubular atmosphere furnace, inflating the tubular atmosphere furnace for 20min at the flow of 150sccm after ensuring the sealing of the tubular atmosphere furnace, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 2 times, thereby replacing the air in the tubular atmosphere furnace with inert gas. Then heating to 300 ℃ at the heating rate of 7 ℃/min and preserving heat for 4h for calcination; wherein, the flow of inert gas is kept to be 300sccm in the calcining process, and the pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0.03MPa in the calcining heat preservation stage; then cooling to room temperature to obtain Co9S8The/carbon felt sodium ion battery self-supporting negative electrode.
Claims (10)
1. Co9S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery is characterized by comprising the following steps of:
step 1: placing the carbon felt in a mixed solution of concentrated nitric acid and hydrogen peroxide, standing in a dark place, and then cleaning and drying the carbon felt to obtain a carbon felt sheet A;
step 2: adding 1.2-2 g of cobalt chloride and 5-10 mL of ethylenediamine into 20-30 mL of deionized water, stirring and dissolving to obtain a solution C; adding 1-1.5 g of thioacetamide into absolute ethyl alcohol with the same volume as that of deionized water, stirring and dissolving to obtain a solution D; mixing the solution C and the solution D to obtain a solution E;
and step 3: immersing the carbon felt A in the solution E and standing to obtain a carbon felt B;
and 4, step 4: placing the carbon felt sheet B into a porcelain boat, placing the porcelain boat into a tubular atmosphere furnace, calcining at 300-700 ℃, and cooling to room temperature to obtain Co9S8Sodium carbon feltThe ion battery is a self-supporting cathode.
2. Co according to claim 19S8The preparation method of the self-supporting cathode of the carbon felt sodium ion battery is characterized in that the thickness of the carbon felt in the step 1 is 1mm, and the carbon felt is cut into 4 multiplied by 3cm and then placed in a mixed solution of concentrated nitric acid and hydrogen peroxide.
3. Co according to claim 19S8The preparation method of the self-supporting cathode of the/carbon felt sodium ion battery is characterized in that the volume ratio of the concentrated nitric acid to the hydrogen peroxide in the mixed solution in the step 1 is 1: 1-3; standing in dark for 24-48 h.
4. Co according to claim 19S8The preparation method of the self-supporting cathode of the/carbon felt sodium ion battery is characterized in that in the step 1, deionized water and absolute ethyl alcohol are respectively used for cleaning for 3-5 times, and drying is carried out for 3-6 hours at 60-100 ℃ in a vacuum environment.
5. Co according to claim 19S8The preparation method of the self-supporting cathode of the carbon felt sodium ion battery is characterized in that the stirring in the step 2 is magnetic stirring at the rotating speed of 400-600 r/min for 1-2 hours.
6. Co according to claim 19S8The preparation method of the self-supporting negative electrode of the/carbon felt sodium ion battery is characterized in that the solution E is heated to 60-100 ℃ and is kept warm for 12-24 hours in the standing process in the step 3.
7. Co according to claim 19S8The preparation method of the self-supporting cathode of the/carbon felt sodium ion battery is characterized in that the step 4 of calcining is to heat the cathode to 300-700 ℃ from room temperature at a heating rate of 5-10 ℃/min and keep the temperature for 2-4 h.
8. Co according to claim 79S8The preparation method of the self-supporting cathode of the/carbon felt sodium ion battery is characterized in that in the step 4, air in the tubular atmosphere furnace is replaced by inert gas before calcination, the inert gas is kept to circulate in the calcination process, and the air pressure difference between the inside and the outside of the tubular atmosphere furnace is kept to be 0-0.05 Mpa in the calcination heat preservation stage.
9. Co according to claim 89S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery is characterized in that the replacement process comprises the steps of inflating the tubular atmosphere furnace for 20min at the flow rate of 70-150 sccm, and then exhausting until the internal and external air pressures of the tubular atmosphere furnace are the same; and respectively and alternately repeating the air inflation and the air supply for 2-5 times.
10. Co according to claim 89S8The preparation method of the self-supporting negative electrode of the carbon felt sodium ion battery is characterized in that the flow of the inert gas is 300-800 sccm.
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