CN111952553A - Preparation method of sulfur/sisal fiber activated carbon lithium-sulfur battery positive electrode material - Google Patents
Preparation method of sulfur/sisal fiber activated carbon lithium-sulfur battery positive electrode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material, and belongs to the technical field of lithium sulfur batteries. The preparation method comprises the following steps: 1) cleaning and cutting the sisal fibers into small segments, and carrying out pretreatment on the sisal fibers, including carbonization, ball milling and hydrothermal reaction to obtain sisal fiber activated carbon powder; 2) mixing Na2S2O3Uniformly mixing the solution and the acid solution with the sisal fiber activated carbon powder, uniformly stirring, transferring to a high-pressure reaction kettle, carrying out hydrothermal treatment for 6h at the temperature of 100-180 ℃, filtering, cleaning and drying the sample obtained after the reaction to obtain a black powder sample, namely the sulfur/sisal fiber activated carbon lithium sulfur batteryAnd (3) a positive electrode material. The elemental sulfur is embedded into the abundant porous structure of the sisal fiber active carbon, so that the utilization rate of active substances is improved, and the prepared sulfur/sisal fiber active carbon lithium sulfur battery positive electrode material has good electrochemical performance.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of lithium-sulfur batteries, in particular to a preparation method of a sulfur/sisal fiber activated carbon positive electrode material of a lithium-sulfur battery.
[ background of the invention ]
With the development of society, energy problems are increasingly prominent, environmental problems are increasingly severe, and sustainable development becomes a consensus of the whole society. In order to harmoniously develop human and nature, various countries in the world shift scientific and technological strength and capital into development and application of new energy and renewable energy. The popularization of various portable electronic devices and the development of new energy power devices such as electric vehicles and the like have made urgent demands for high-capacity lithium secondary batteries.
The sulfur-containing anode material is a research object with higher specific capacity in the anode material, the specific capacity of most of the sulfur-containing anode materials can reach more than 500mAh/g, the sulfur-containing anode material meets the requirement of a high-specific-energy battery, and the sulfur content is further improved to increase the specific capacity.
[ summary of the invention ]
The invention aims at the problems and provides a preparation method of a sulfur/sisal fiber activated carbon lithium-sulfur battery positive electrode material. The method utilizes cheap, easily available, green and environment-friendly elemental sulfur to be compounded with the sisal fiber activated carbon material, and by means of the abundant porous structure of the sisal fiber activated carbon, elemental sulfur is embedded into the porous structure of the activated carbon, so that the reaction area is increased, the dissolution of a sulfur electrode discharge product is reduced, the utilization rate of the active substance is increased, the cycle reversibility of the lithium-sulfur battery is improved, and the prepared sulfur/sisal fiber activated carbon lithium-sulfur battery anode material has good electrochemical performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material comprises the following steps:
(1) cleaning and shearing sisal fiber into small segments with the length of about 1-2cm, placing the segments into a crucible, calcining for 2h in a tubular furnace with inert gas as protective gas, wherein the calcining temperature is 700-: putting the obtained powder sample into a forced air dryer, heating to 120-140 ℃, carrying out hydrothermal treatment for 5-6h, naturally cooling, washing and drying to obtain sisal fiber activated carbon powder;
(2) mixing different concentrations of Na2S2O3And (2) uniformly mixing the solution and the acid solution with the sisal fiber activated carbon powder obtained in the step (1), uniformly stirring, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, moving the reaction kettle into a blast drying box, carrying out hydrothermal treatment for 6 hours again at the temperature of 100-.
Preferably, the specific process of further processing the powder sample obtained in step (1) is as follows: putting 70mL of distilled water into a beaker, adding 1g of powder sample, uniformly stirring, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an air-blast drying box, carrying out hydrothermal treatment at the temperature of 120-140 ℃ for 5-6h, naturally cooling, filtering, washing with absolute ethyl alcohol, and drying in the air-blast drying box at the temperature of 80 ℃ for 12h to obtain the sisal fiber activated carbon powder sample.
Preferably, the acid solution is sulfuric acid, nitric acid or hydrochloric acid.
Preferably, Na in step (2)2S2O3The solution and acid solution were added in 35mL each, the Na being2S2O3The concentration of the solution and the acid solution is 0.5-1mol/L, and Na2S2O3The solution and the acid solution are evenly stirred with the sisal fiber activated carbon powder at the temperature of 60-80 ℃.
Preferably, Na in step (2)2S2O3The mixture of the solution and the acid solution with the sisal fiber activated carbon powder obtained in the step (1) is specifically as follows: dissolving sodium thiosulfate pentahydrate in deionized water to prepare 35mL of Na with the concentration of 0.5-1mol/L2S2O3After the solution, Na will be filled2S2O3Placing the solution beaker in water bath at 60-80 deg.C, and dripping 35mL of solution with concentration of 0.5-1m into the beaker while stirringAnd (3) adding the sisal fiber activated carbon powder obtained in the step (1) into the alcoholic/L sulfuric acid solution, and continuously stirring the solution uniformly on a magnetic stirrer in an accelerated manner. This step is to make Na2S2O3The solution and the sulfuric acid solution are more fully mixed, the reaction rate of reactants is improved, and the hydrothermal time required by the subsequent hydrothermal reaction is greatly shortened.
Preferably, step (2) further comprises sieving the black powder sample with a 200-mesh sieve after drying.
Preferably, the inert gas is one of nitrogen, argon and helium.
By adopting the technical scheme, the invention has the beneficial effects that:
in the invention, the sisal fiber activated carbon is porous carbon with strong adsorbability, and the high specific surface area, the high surface activity and the high adsorption capacity of the activated carbon are determined by the porous characteristic of the sisal fiber activated carbon. After the elemental sulfur is compounded with the sisal fiber activated carbon material, on one hand, the elemental sulfur dispersed in the sisal fiber activated carbon improves the specific capacity of the anode material, and the microporous structure of the sisal fiber activated carbon can effectively inhibit the elemental sulfur and a discharge product thereof from being irreversibly dissolved into an electrolyte, so that the reaction activity is enhanced, and the utilization rate of the active substance is improved; on the other hand, the sisal fiber activated carbon has good electronic conductivity, the conductivity of elemental sulfur is integrally improved, and the combination of the sisal fiber activated carbon and the elemental sulfur can enable the prepared sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material to have good electrochemical performance.
Electrochemical tests show that the sulfur/sisal fiber active carbon lithium sulfur battery positive electrode material prepared by the method has higher specific capacity and good cycling stability. The first discharge specific capacity of the composite material is 1223mAh/g, and after the first charge-discharge cycle, the charge-discharge efficiency can still reach 90%.
[ description of the drawings ]
FIG. 1 is an XRD pattern of various embodiments of the present invention;
fig. 2 is an SEM image of the composite cathode material prepared in example 5 of the present invention.
FIG. 3 is a graph comparing electrochemical cycling performance of examples 1-5 of the present invention.
Fig. 4 is an SEM image of the composite cathode material prepared in example 10 of the present invention.
FIG. 5 is a graph comparing electrochemical cycling performance of examples 6-10 of the present invention.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material comprises the following steps:
(1) cleaning and cutting sisal fiber into small sections with the length of about 2cm, placing the small sections into a crucible, carbonizing the small sections for 2 hours in a tube furnace by taking nitrogen as protective gas, wherein the carbonizing temperature is 900 ℃, the heating rate is 3 ℃/min, after the furnace temperature is naturally cooled to the room temperature, ball-milling the obtained carbon material for 5 hours in a planetary ball mill at the rotating speed of 35r/s, and preparing a powder sample.
(2) The prepared powder samples were further processed: putting 70mL of distilled water in a beaker, adding 1g of powder sample, transferring the powder sample into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an air-blast drying oven, carrying out hydrothermal treatment for 6h at 140 ℃, filtering and washing the powder with absolute ethyl alcohol after the reaction kettle is naturally cooled, and drying the powder for 12h at 80 ℃ in the air-blast drying oven to obtain the sisal fiber activated carbon powder.
(3) Dissolving sodium thiosulfate pentahydrate in deionized water to prepare 35mL of Na with the concentration of 0.5mol/L2S2O3After the solution, Na will be filled2S2O3Placing the solution beaker in a water bath at 80 ℃, dropwise adding 35mL of 0.5mol/L sulfuric acid solution into the beaker during stirring, finally adding the sisal fiber activated carbon powder obtained in the step (2), and continuously stirring by magnetic forceAccelerating and stirring evenly on the device to obtain mixed liquid. And after uniformly stirring, transferring the mixed solution into a polytetrafluoroethylene lining of a high-pressure reaction kettle, transferring the reaction kettle into an air-blowing drying oven, placing the reaction kettle into the air-blowing drying oven at the temperature of 100 ℃ for hydrothermal reaction for 6 hours again, filtering and cleaning a sample obtained by the reaction after the reaction is naturally cooled, and drying the sample in a vacuum drying oven at the temperature of 80 ℃ to obtain the sulfur/sisal fiber activated carbon composite anode material with different hydrothermal temperatures, wherein the mark is 1-100-0.5.
(4) Preparing a battery: mixing 0.32g of the composite positive electrode material obtained in the step (3), 0.04g of acetylene black and 0.04g of PVDF (polyvinylidene fluoride), adding NMP (N-methyl-2-pyrrolidone) as a solvent, stirring to paste, uniformly coating on a copper foil with the thickness of 10 mu m, then putting the copper foil into an air drying box, drying for 4h at 60 ℃, transferring the copper foil into a vacuum drying box, drying for 12h at 110 ℃, punching the copper foil into a 16mm circular pole piece by using a manual punching machine, taking the circular pole piece as a positive pole, a lithium piece as a negative pole, a microporous polypropylene film as a diaphragm, 1mol/L of LiPF6/EC (ethylene carbonate) + DMC (dimethyl carbonate) + DEC (diethyl carbonate) as an electrolyte (LiPF 6 in the electrolyte is a solute, the volume ratio of the solvent EC + DMC + DEC is 1:1:1), assembling a battery with the simulation model of CR2025 in a glove box filled with argon gas, after sealing, the mixture is placed in a ventilated place and kept stand for 12 hours.
Example 2
In this example, the temperature was the same as in example 1 except for the hydrothermal reaction temperature in step (3).
In this example, the hydrothermal reaction temperature in step (3) was 120 ℃. The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 3-120-0.5.
Example 3
In this example, the temperature was the same as in example 1 except for the hydrothermal reaction temperature in step (3).
In this example, the temperature of the hydrothermal reaction in step (3) was 140 ℃. The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 5-140-0.5.
Example 4
In this example, the temperature was the same as in example 1 except for the hydrothermal reaction temperature in step (3).
In this example, the temperature of the hydrothermal reaction in step (3) was 160 ℃. The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 7-160-0.5.
Example 5
In this example, the temperature was the same as in example 1 except for the hydrothermal reaction temperature in step (3).
In this example, the temperature of the hydrothermal reaction in step (3) was 180 ℃. The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 9-180-0.5.
And the morphology of the composite cathode material obtained in the embodiment is also obtained through a scanning electron microscope, such as an SEM image shown in fig. 2.
In examples 2 to 5, the electrode preparation and the battery assembly were the same as in example 1.
Electrochemical tests were performed on the batteries manufactured in examples 1 to 5 at room temperature using a battery tester. The current density is set to 50mA/g, and the voltage testing range is 0.01-3V.
As shown in fig. 3, electrochemical tests show that the sulfur/sisal fiber activated carbon composite material prepared by hydrothermal method at 180 ℃ has the highest specific discharge capacity of 1191mAh/g as the cathode material under the condition that the current density is 50mA/g, and obviously, the theoretical specific capacity is increased along with the increase of the hydrothermal temperature.
Example 6
In this example, Na in step (3) was removed2S2O3The solution and sulfuric acid solution were the same as in example 1 except that the concentrations were changed.
In this example, Na in step (3)2S2O3The concentration of the solution and the sulfuric acid solution are both 1 mol/L.
The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 2-100-1.0.
Example 7
In this example, Na in step (3) was removed2S2O3In addition to the concentration of the solution and the sulfuric acid solution being changed,the rest is the same as in example 2.
In this example, Na in step (3)2S2O3The concentration of the solution and the sulfuric acid solution are both 1 mol/L.
The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 4-120-1.0.
Example 8
In this example, Na in step (3) was removed2S2O3The solution and sulfuric acid solution were the same as in example 3 except that the concentrations were changed.
In this example, Na in step (3)2S2O3The concentration of the solution and the sulfuric acid solution are both 1 mol/L.
The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 6-140-1.0.
Example 9
In this example, Na in step (3) was removed2S2O3The solution and sulfuric acid solution were the same as in example 4 except that the concentrations were changed.
In this example, Na in step (3)2S2O3The concentration of the solution and the sulfuric acid solution are both 1 mol/L.
The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is recorded as 8-160-1.0.
Example 10
In this example, Na in step (3) was removed2S2O3The same procedure as in example 5 was repeated except that the concentrations of the solution and the sulfuric acid solution were changed.
In this example, Na in step (3)2S2O3The concentration of the solution and the sulfuric acid solution are both 1 mol/L.
The sulfur/sisal fiber activated carbon composite cathode material prepared in the embodiment is marked as 10-180-1.0.
And the morphology of the composite cathode material obtained in the embodiment is also obtained through a scanning electron microscope, such as an SEM image shown in fig. 4.
In order to verify the composition and the like of the prepared cathode material, the XRD test was also performed on the cathode material prepared in each example, as shown in fig. 1.
Examples 6-10, electrode preparation, cell assembly and electrochemical testing were the same as in example 1. Electrochemical tests were performed at room temperature on the batteries obtained in examples 6 to 10 using a battery tester. The current density is set to 50mA/g, and the voltage testing range is 0.01-3V.
As shown in FIG. 5, electrochemical tests showed that Na of example 10 was obtained at a current density of 50mA/g2S2O3The concentrations of the solution and the sulfuric acid solution are both 1mol/L, the composite cathode material prepared at the hydrothermal temperature of 180 ℃ has excellent electrochemical performance, the first discharge specific capacity is 1223mAh/g, the charge transfer resistance is 100 omega, although the capacity is attenuated after the first charge and discharge, the capacity is gradually stabilized along with the increase of the cycle number, and the charge and discharge efficiency is about 90%.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (7)
1. A preparation method of a sulfur/sisal fiber activated carbon lithium-sulfur battery positive electrode material is characterized by comprising the following steps:
(1) cleaning and shearing sisal fiber into small segments with the length of about 1-2cm, placing the segments into a crucible, calcining for 2h in a tubular furnace with inert gas as protective gas, wherein the calcining temperature is 700-: putting the obtained powder sample into a forced air dryer, heating to 120-140 ℃, carrying out hydrothermal treatment for 5-6h, naturally cooling, washing and drying to obtain sisal fiber activated carbon powder;
(2) mixing different concentrations of Na2S2O3And (2) uniformly mixing the solution and the acid solution with the sisal fiber activated carbon powder obtained in the step (1), uniformly stirring, transferring the mixture into a polytetrafluoroethylene lining of a high-pressure reaction kettle, moving the reaction kettle into a blast drying box, carrying out hydrothermal treatment for 6 hours again at the temperature of 100-.
2. The method for preparing the sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material as claimed in claim 1, wherein the specific process of further processing the obtained powder sample in step (1) is as follows: putting 70mL of distilled water into a beaker, adding 1g of powder sample, uniformly stirring, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an air-blast drying box, carrying out hydrothermal treatment at the temperature of 120-140 ℃ for 5-6h, naturally cooling, filtering, washing with absolute ethyl alcohol, and drying in the air-blast drying box at the temperature of 80 ℃ for 12h to obtain the sisal fiber activated carbon powder sample.
3. The method for preparing a sulfur/sisal fiber activated carbon lithium sulfur battery cathode material as claimed in claim 1, wherein the acid solution is sulfuric acid, nitric acid or hydrochloric acid.
4. The method for preparing the sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material as claimed in claim 1, wherein Na in step (2)2S2O3The solution and acid solution were added in 35mL each, the Na being2S2O3The concentration of the solution and the acid solution is 0.5-1mol/L, and Na2S2O3The solution and the acid solution are evenly stirred with the sisal fiber activated carbon powder at the temperature of 60-80 ℃.
5. The method for preparing the sulfur/sisal fiber activated carbon lithium sulfur battery positive electrode material as claimed in claim 4, wherein Na in step (2)2S2O3Solutions and acid solutionsThe mixing with the sisal fiber active carbon powder obtained in the step (1) is specifically as follows: dissolving sodium thiosulfate pentahydrate in deionized water to prepare 35mL of Na with the concentration of 0.5-1mol/L2S2O3After the solution, Na will be filled2S2O3Putting the beaker of the solution into a water bath at 60-80 ℃, dripping 35mL of sulfuric acid solution with the concentration of 0.5-1mol/L into the beaker in the stirring process, finally adding the sisal fiber activated carbon powder obtained in the step (1), and continuously and uniformly stirring on a magnetic stirrer in an accelerated manner.
6. The method for preparing the sulfur/sisal fiber activated carbon lithium sulfur battery cathode material as claimed in claim 1, wherein the step (2) further comprises sieving the black powder sample with a 200-mesh sieve after drying.
7. The method for preparing the sulfur/sisal fiber activated carbon lithium sulfur battery cathode material as claimed in claim 1, wherein the inert gas is one of nitrogen, argon and helium.
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| CN114899374A (en) * | 2022-05-07 | 2022-08-12 | 桂林理工大学 | Graphene oxide/sulfur/sisal fiber activated carbon lithium-sulfur battery composite positive electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441280A (en) * | 2013-09-13 | 2013-12-11 | 桂林理工大学 | Method for preparing negative pole material of lithium ion battery through hydrothermally activated sisal carbon fibers |
| CN107123801A (en) * | 2017-05-18 | 2017-09-01 | 中南大学 | A kind of method that lithium-sulfur cell sulphur/carbon composite anode material is prepared based on monkey grass |
| CN107732177A (en) * | 2017-09-26 | 2018-02-23 | 桂林理工大学 | The preparation method of sulphur/sisal carbon composite cathode material for lithium ion cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441280A (en) * | 2013-09-13 | 2013-12-11 | 桂林理工大学 | Method for preparing negative pole material of lithium ion battery through hydrothermally activated sisal carbon fibers |
| CN107123801A (en) * | 2017-05-18 | 2017-09-01 | 中南大学 | A kind of method that lithium-sulfur cell sulphur/carbon composite anode material is prepared based on monkey grass |
| CN107732177A (en) * | 2017-09-26 | 2018-02-23 | 桂林理工大学 | The preparation method of sulphur/sisal carbon composite cathode material for lithium ion cell |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114899374A (en) * | 2022-05-07 | 2022-08-12 | 桂林理工大学 | Graphene oxide/sulfur/sisal fiber activated carbon lithium-sulfur battery composite positive electrode material and preparation method thereof |
| CN114899374B (en) * | 2022-05-07 | 2023-09-22 | 桂林理工大学 | Composite positive electrode material of lithium-sulfur battery and preparation method thereof |
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Application publication date: 20201117 Assignee: Guangxi shimaoda Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000494 Denomination of invention: Preparation method of sulfur/sisal fiber activated carbon cathode material for lithium sulfur battery Granted publication date: 20220408 License type: Common License Record date: 20221229 |
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