CN111960477A - Preparation method of all-solid-state supercapacitor electrode material - Google Patents
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Abstract
The invention provides a preparation method of an all-solid-state supercapacitor electrode material, which adopts three-dimensional porous carbon as a substrate material, and has the advantages of simple preparation process, rich pore channels, large specific surface area, high specific capacity, high rate performance, good cycling stability and the like of the three-dimensional porous carbon material. The iron disulfide/three-dimensional porous carbon composite material prepared by the method is used as an electrode material to prepare a symmetrical all-solid-state supercapacitor, and has the advantages of high specific capacity, excellent cycling stability, high energy density and high power density.
Description
Technical Field
The invention relates to the technical field of energy materials, in particular to a preparation method of an iron disulfide/three-dimensional porous carbon all-solid-state supercapacitor electrode material.
Background
The super capacitor is also called an electrochemical capacitor, and is a green energy storage device for storing charges based on adsorption and desorption or rapid oxidation/reduction reaction of interface ions. Supercapacitors have a greater energy density than conventional capacitors and a higher power density than batteries. Meanwhile, the super capacitor has the advantages of rapid charge and discharge, long service life, wide range of adaptive environment temperature and the like, so that the super capacitor is widely applied to the fields of traffic, energy, military and the like.
Supercapacitors can be classified into electric double charge capacitors or electric double layer capacitors, faraday pseudocapacitors, and hybrid supercapacitors, depending on the principle of operation. The super capacitor mainly comprises four parts, namely a positive electrode, a negative electrode, a diaphragm and electrolyte. When the double-layer capacitor works, electric energy is stored by means of electric double layers formed by electrolyte and charge movement on the surfaces of electrodes, a negative electrode of the capacitor can accumulate a large amount of negative charges when discharging, a positive electrode can accumulate a large amount of positive charges, anions move to the positive electrode, cations move to the negative electrode, and the charging is in an opposite state. It follows that charging and discharging of electric double layer supercapacitors is a physical process of charge transfer, with no chemical reactions taking place. The most common carbon materials in the electric double layer capacitor electrode material mainly include: carbon aerogels, carbon nanotubes, activated carbon, and the like. The energy storage mechanism of the Faraday pseudocapacitance super capacitor mainly depends on oxidation/reduction reaction or chemical desorption and adsorption phenomena participated by electrode materials to finish the storage and application of charges. Different from an electric double layer, the faradaic pseudocapacitance reacts not only on the surface of an electrode and around the electrode, but also inside the electrode, so that a large amount of pseudocapacitance can be generated, and higher capacitance performance can be obtained. The hybrid capacitor is formed by respectively taking an electrode material with an electric double layer as an energy storage mechanism and an electrode material with a Faraday pseudo-capacitance as two electrodes of the super capacitor, so that the hybrid capacitor has different properties between the two electrodes. The hybrid capacitor not only has higher capacitance but also has higher cycling stability.
According to the energy storage principle of the super capacitor, the energy storage of the capacitor mainly depends on the electrode material, so that it is very important to further develop the electrode material with high capacity and good performance. At present, carbon materials, conductive polymer materials, transition metal oxides and transition metal sulfides are common supercapacitor materials. The carbon material is mainly applied to an electric double layer electrode material, and the conductive polymer material, the transition metal oxide and the transition metal sulfide material are mainly applied to a Faraday pseudo capacitor electrode material.
It is well known that a high molecular conductive polymer as a faraday pseudocapacitive electrode material conducts electricity through a conjugated bond system along the polymer backbone. They provide pseudocapacitive behavior through redox reactions that occur not only at the surface, but throughout the entire volume. And it is highly reversible, and because there is no structural change in which a phase change occurs during the redox process, its advantages of low cost, environmental stability and ease of synthesis are favored. However, the conductive polymer is susceptible to volume expansion and contraction during intercalation and deintercalation, often resulting in poor cycle stability. The metal oxide has pseudo-capacitance characteristics, and the main mechanisms are Faraday redox reaction and adsorption and desorption of ions at an electrode/electrolyte interface in the electrochemical reaction process. Both the cell-type electrode material and the pseudocapacitance electrode material are involved in faradaic reactions and there is charge transfer. However, their kinetics and electrochemical behaviour are quite different for both. Due to the unsaturation of the d orbitals, some transition metal d orbitals have special properties, and the transition metal oxides can provide different oxidation states to carry out effective oxidation-reduction reaction, so that the high theoretical specific capacitance is achieved. But oxide preparationHigh-temperature treatment is often needed in the process, so that the material is agglomerated, the size is increased, the specific surface area is reduced, and meanwhile, the conductivity is poor and the conductivity is low. Transition metal sulfide is applied to super capacitor energy storage as a novel pseudo-capacitance material and receives more and more attention. In general, since elemental sulfur is less electronegative relative to oxides, a more flexible structure is obtained when the sulfur atom replaces the oxygen atom, and more redox reactions are likely to occur during the redox process. Meanwhile, metal sulfides have various possible stoichiometric compositions, crystal structures, valence states, and nanocrystalline morphologies, resulting in higher electrochemical activity. Transition metal sulfides generally have better electrical conductivity, mechanical stability, and thermal stability than transition metal oxides. Compared with carbon materials or common transition metal oxides, the rich redox reaction of the transition metal sulfide enables the carbon materials or common transition metal oxides to have higher specific capacitance. In recent years, iron disulfide as an electrode material has the advantages of high theoretical specific capacitance, low preparation cost, wide resource distribution, no toxicity and the like, and is favored. However, in the charge-discharge cycle process, especially in the charge-discharge process under high current density, the volume of the iron disulfide electrode is easy to expand, so that the capacity attenuation is fast, the cycle performance is poor, and the like, thereby seriously restricting the application of the iron disulfide electrode material. Currently, many researchers have compounded iron disulfide with some materials with high conductivity and high specific surface area to improve the problem and prepare iron disulfide composite electrode materials. For example, chinese patent publication No. CN109935779A discloses an iron disulfide positive electrode material, a preparation method thereof, and an alkali metal ion battery, including coating a conductive polymer on the surface of iron disulfide particles, then coating the prepared material on a current collector, and then coating the conductive polymer on the surface of an electrode through electrochemical polymerization. Chinese patent CN110783569A discloses a FeS 2-based composite cathode material, a preparation method thereof and a lithium ion secondary battery, which comprises cobalt nitrate hexahydrate and iron disulfideAdding the mixture into a methanol solution, and uniformly stirring to obtain a mixed solution; and (2) dropwise adding the methanol solution of 2-methylimidazole into the mixed solution while stirring, continuously stirring for 20-30h after dropwise adding is finished, standing, sequentially performing suction filtration, washing and drying to obtain powder, calcining the powder in an inert atmosphere, and finally cooling to room temperature to obtain the catalyst. The FeS2The base composite anode material can effectively solve the problem of the prior FeS2The capacity of the base cathode material is rapidly reduced. Chinese patent CN109037623A discloses a positive electrode material of a magnesium secondary battery and a preparation method thereof, which comprises the steps of adopting ferrous disulfide as a base material, adopting a doped nano carbon material to carry out in-situ carbon coating, and obtaining a final composite material by a one-step hydrothermal method. When the material is applied to a magnesium secondary battery, more channels can be provided for reversible diffusion of magnesium ions, so that the battery has higher charge-discharge specific capacity and excellent cycling stability. Because iron disulfide resources are widely distributed, the advantages of low preparation cost, environmental protection and the like are frequently applied to batteries, and in contrast, the application of the iron disulfide resources in the super capacitor is less.
The invention has the characteristics of simple and efficient preparation method, no environmental pollution and the like, and the prepared iron disulfide composite material has higher capacity and good cycle stability. A plurality of problems faced by the iron disulfide can be hopefully solved by a carbon and iron disulfide compound mode, and the conductivity of the material can be greatly improved. Therefore, it is very important to find a carbon-based material with simple preparation method, low cost, stable structure and large specific surface area.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a preparation method of an all-solid-state supercapacitor electrode material, and particularly provides an iron disulfide/three-dimensional porous carbon symmetrical all-solid-state supercapacitor electrode material with high specific capacity and excellent cycle performance. The three-dimensional porous carbon is used as a substrate material, the three-dimensional porous carbon material has the advantages of simple preparation process, rich pore channels, large specific surface area, high specific capacity, high rate performance, good circulation stability and the like, and then the iron disulfide/three-dimensional porous carbon symmetrical all-solid-state supercapacitor electrode material is synthesized in one step by adopting a hydrothermal method, so that the three-dimensional porous carbon can not only provide a carrier for polyaniline and manganese dioxide, but also prevent material pulverization, reduce the electrical contact between the material and a current collector, simultaneously reduce the side reaction between an electrode and electrolyte, and improve the conductivity of the material to a certain extent. The iron disulfide/three-dimensional porous carbon composite material prepared by the method has the advantages of large specific surface area, good conductivity and high specific capacity. The iron disulfide/three-dimensional porous carbon composite material prepared by the method is used as an electrode material to prepare a symmetrical all-solid-state supercapacitor, and has the advantages of high specific capacity, excellent cycling stability, high energy density and high power density. Meanwhile, the preparation method provided by the invention is simple and efficient to operate, green and environment-friendly, and low in cost, and can better meet the daily life requirements of people.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an iron disulfide/three-dimensional porous carbon all-solid-state supercapacitor electrode material comprises the following steps:
A) preparation of three-dimensional porous carbon: dissolving citric acid and sodium chloride in deionized water, magnetically stirring for several hours, and freeze-drying to obtain white powder; calcining the white powder in a reducing atmosphere to obtain black powder; washing the black powder with deionized water for multiple times to remove the NaCl template, and then carrying out vacuum drying for several hours to obtain the three-dimensional porous carbon;
B) preparing the iron disulfide/three-dimensional porous carbon composite material: simultaneously dissolving the three-dimensional porous carbon and ferric nitrate powder in a small amount of glycol solution of polyvinylpyrrolidone-K30 and stirring for 1 hour; then dropwise adding a small amount of ethylene glycol solution of thiourea into the solution and continuously stirring the solution to form uniform mixed solution; transferring the mixed solution into a high-pressure reaction kettle, heating to 200 ℃, and preserving heat for 24 hours; and finally, repeatedly centrifuging and vacuum drying to obtain the iron disulfide/three-dimensional porous carbon composite material.
Preferably, the mass ratio of the citric acid, the sodium chloride and the deionized water in the step A) is (1-1.5): (8-10): (22-30).
Preferably, the stirring speed in the step A) is 800-1500rpm, and the stirring time is 8-10 hours.
Preferably, the stirring speed in step A) is 950-1050rpm, and the stirring time is 8.5-9.5 hours.
Preferably, the temperature of the calcination in step A) is 750-1000 ℃, and the calcination time is 2-4 hours.
Preferably, the temperature of the calcination in step A) is 750-850 ℃, and the calcination time is 2-3 hours.
Preferably, the temperature of the vacuum drying in the step A) is 40-60 ℃, and the drying time is 8-12 hours.
Preferably, the mass ratio of the porous carbon to the ferric nitrate in the step B) is (2.3-3): (0.2-1.2); the concentration of the ethylene glycol solution of the polyvinylpyrrolidone-K30 is (0.16-0.22) mol/L, and the volume is 12-18 mL; the concentration of the ethylene glycol solution of the thiourea is (0.6-1.0) mol/L, the volume is 8-12mL, and the dropping speed is 0.15-0.25 mL/min.
Preferably, the stirring speed in step B) is 600-1000rpm, and the stirring time is 0.2-0.8 h.
Preferably, the stirring speed in step B) is 650-800rpm, and the stirring time is 0.2-0.5 h.
Preferably, the temperature rising speed in the step B) is 3-8 ℃/min.
Preferably, the centrifugation rate in step B) is 3000-4500 r/min; the vacuum drying temperature is 60-80 ℃, and the drying time is 5-10 hours.
The application of the iron disulfide/three-dimensional porous carbon composite material is used as a symmetrical all-solid-state supercapacitor electrode material.
Compared with the prior art, the invention has the beneficial effects that:
1) the iron disulfide/three-dimensional porous carbon composite material prepared by the invention has better conductivity, higher specific surface area, higher specific capacitance and excellent cycling stability. The method has the advantages of simple synthesis method, low cost, high sample yield and the like, and has good application prospect;
2) the specific capacitance of the iron disulfide/three-dimensional porous carbon composite material prepared by the invention reaches 304Fg-1 under the current density of 4 Ag-1;
3) the iron disulfide/three-dimensional porous carbon composite material prepared by the invention is used as a positive material and a negative material, polyvinyl alcohol-potassium hydroxide gel is used as a working electrolyte to assemble the performance of a symmetrical all-solid-state supercapacitor, the voltage window of the symmetrical all-solid-state supercapacitor is up to 1.7V, and good cycle stability is shown, namely the specific capacitance retention rate is 84.77% after 5000 cycles of constant current charge and discharge.
Drawings
FIG. 1 is a constant current charge and discharge curve diagram of the iron sulfide/three-dimensional porous carbon composite material in example 1 at different current densities;
FIG. 2 is a capacitance retention rate curve of a symmetrical all-solid-state supercapacitor assembled by the iron sulfide/three-dimensional porous carbon composite material as an electrode material in example 1 after 5000 cycles at a current density of 4 Ag-1.
Detailed Description
The following detailed description of the present invention will be made with reference to the accompanying drawings.
Example 1
The invention relates to a preparation method of an all-solid-state supercapacitor electrode material, which is a preparation method of an iron disulfide/three-dimensional porous carbon symmetrical all-solid-state supercapacitor electrode material, and comprises the following steps:
A) preparation of three-dimensional porous carbon: dissolving 2.5g of citric acid and 20.7g of sodium chloride in 70mL of deionized water, magnetically stirring at a stirring speed of 1000rpm for 10 hours, and then freeze-drying to obtain white powder; calcining the white powder for 2 hours at 800 ℃ under a reducing atmosphere to obtain black powder; and washing the black powder with deionized water for multiple times to remove the NaCl template, and then carrying out vacuum drying for 8 hours at 80 ℃ to obtain the three-dimensional porous carbon.
B) Preparing the iron disulfide/three-dimensional porous carbon composite material: simultaneously dissolving 0.27g of three-dimensional porous carbon and 0.1g of ferric nitrate powder in 15mL of glycol solution of polyvinylpyrrolidone-K30 with the concentration of 0.2mol/L, and magnetically stirring at 800rpm for 0.5 hour; then 10mL of ethylene glycol solution of thiourea with the concentration of 0.8mol/L is added dropwise and is continuously stirred into uniform mixed liquid, and the dropping speed is 0.2 mL/min; transferring the mixed solution into a high-pressure reaction kettle, heating to 200 ℃, and preserving heat for 24 hours; and finally, repeatedly centrifuging at the speed of 3000r/min, and carrying out vacuum drying at the temperature of 80 ℃ for 8 hours to obtain the iron disulfide/three-dimensional porous carbon composite material. FIG. 1 is a constant current charge and discharge curve diagram of the iron sulfide/three-dimensional porous carbon composite material in example 1 at different current densities. FIG. 2 is a capacitance retention rate curve of a symmetrical all-solid-state supercapacitor assembled by the iron sulfide/three-dimensional porous carbon composite material as an electrode material in example 1 after 5000 cycles at a current density of 4 Ag-1.
Example 2
A) Preparation of three-dimensional porous carbon: dissolving 2.5g of citric acid and 21.7g of sodium chloride in 70mL of deionized water, magnetically stirring at a stirring speed of 1000rpm for 10 hours, and then freeze-drying to obtain white powder; calcining the white powder for 2 hours at 850 ℃ under a reducing atmosphere to obtain black powder; and washing the black powder with deionized water for multiple times to remove the NaCl template, and then carrying out vacuum drying for 8 hours at 80 ℃ to obtain the three-dimensional porous carbon.
B) Preparing the iron disulfide/three-dimensional porous carbon composite material: simultaneously dissolving 0.27g of three-dimensional porous carbon and 0.2g of ferric nitrate powder in 15mL of glycol solution of polyvinylpyrrolidone-K30 with the concentration of 0.2mol/L, and magnetically stirring at 800rpm for 0.5 hour; then 10mL of ethylene glycol solution of thiourea with the concentration of 0.8mol/L is added dropwise and is continuously stirred into uniform mixed liquid, and the dropping speed is 0.2 mL/min; transferring the mixed solution into a high-pressure reaction kettle, heating to 200 ℃, and preserving heat for 24 hours; and finally, repeatedly centrifuging at the speed of 3000r/min, and carrying out vacuum drying at the temperature of 80 ℃ for 8 hours to obtain the iron disulfide/three-dimensional porous carbon composite material.
Example 3
A) Preparation of three-dimensional porous carbon: dissolving 2.5g of citric acid and 24.7g of sodium chloride in 70mL of deionized water, magnetically stirring at a stirring speed of 1000rpm for 10 hours, and then freeze-drying to obtain white powder; calcining the white powder for 4 hours at 800 ℃ under a reducing atmosphere to obtain black powder; and washing the black powder with deionized water for multiple times to remove the NaCl template, and then carrying out vacuum drying for 8 hours at 80 ℃ to obtain the three-dimensional porous carbon.
B) Preparing the iron disulfide/three-dimensional porous carbon composite material: simultaneously dissolving 0.27g of three-dimensional porous carbon and 0.02g of ferric nitrate powder in 15mL of glycol solution of polyvinylpyrrolidone-K30 with the concentration of 0.2mol/L, and magnetically stirring at 800rpm for 0.5 hour; then 10mL of ethylene glycol solution of thiourea with the concentration of 0.8mol/L is added dropwise and is continuously stirred into uniform mixed liquid, and the dropping speed is 0.2 mL/min; transferring the mixed solution into a high-pressure reaction kettle, heating to 200 ℃, and preserving heat for 24 hours; and finally, repeatedly centrifuging at the speed of 3000r/min, and carrying out vacuum drying at the temperature of 80 ℃ for 8 hours to obtain the iron disulfide/three-dimensional porous carbon composite material.
The above embodiments are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the above embodiments. The methods used in the above examples are conventional methods unless otherwise specified.
Claims (10)
1. A preparation method of an all-solid-state supercapacitor electrode material is characterized by comprising the following steps:
A) preparation of three-dimensional porous carbon: dissolving citric acid and sodium chloride in deionized water, magnetically stirring, and freeze-drying to obtain white powder; calcining the white powder in a reducing atmosphere to obtain black powder; washing the black powder with deionized water for multiple times to remove a NaCl template, and then carrying out vacuum drying to obtain the three-dimensional porous carbon;
B) preparing the iron disulfide/three-dimensional porous carbon composite material: simultaneously dissolving the three-dimensional porous carbon and ferric nitrate powder in a small amount of glycol solution of polyvinylpyrrolidone-K30 and stirring for 1 hour; then dropwise adding ethylene glycol solution of thiourea into the mixture and continuously stirring the mixture to form uniform mixed solution; transferring the mixed solution into a high-pressure reaction kettle, heating to 200 ℃, and preserving heat for 24 hours; and finally, repeatedly centrifuging and vacuum drying to obtain the iron disulfide/three-dimensional porous carbon composite material.
2. The preparation method of the all-solid-state supercapacitor electrode material according to claim 1, wherein the mass ratio of the citric acid, the sodium chloride and the deionized water in the step A) is (1-1.5): (8-10): (22-30).
3. The method as claimed in claim 1, wherein the stirring speed in step A) is 800-1500rpm, and the stirring time is 8-10 hours.
4. The method as claimed in claim 1, wherein the stirring speed in step A) is 950-1050rpm, and the stirring time is 8.5-9.5 hours.
5. The method as claimed in claim 1, wherein the calcination temperature in step A) is 750-1000 ℃ and the calcination time is 2-4 hours.
6. The method as claimed in claim 1, wherein the calcination temperature in step A) is 750-850 ℃ and the calcination time is 2-3 hours.
7. The preparation method of the all-solid-state supercapacitor electrode material according to claim 1, wherein the temperature of the vacuum drying in the step A) is 40-60 ℃, and the drying time is 8-12 hours.
8. The preparation method of the all-solid-state supercapacitor electrode material according to claim 1, wherein the mass ratio of the porous carbon to the ferric nitrate in the step B) is (2.3-3): (0.2-1.2); the concentration of the ethylene glycol solution of the polyvinylpyrrolidone-K30 is (0.16-0.22) mol/L, and the volume is 12-18 mL; the concentration of the ethylene glycol solution of the thiourea is (0.6-1.0) mol/L, the volume is 8-12mL, and the dropping speed is 0.15-0.25 mL/min.
9. The method as claimed in claim 1, wherein the stirring speed in step B) is 600-1000rpm, and the stirring time is 0.2-0.8 h.
10. The preparation method of the all-solid-state supercapacitor electrode material according to claim 1, wherein the temperature rise speed in the step B) is 3-8 ℃/min; the centrifugation speed is 3000-4500 r/min; the temperature of the vacuum drying is 60-80 ℃, and the drying time is 5-10 hours.
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| CN112700968A (en) * | 2020-12-16 | 2021-04-23 | 安徽工业大学 | Preparation method of iron sulfide-carbon composite electrode material, obtained electrode and application thereof |
| CN113930866A (en) * | 2021-10-13 | 2022-01-14 | 广州航海学院 | Supercapacitor electrode material with capsule structure and preparation method and application thereof |
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