CN113113592B - Preparation method of sulfur/carbon nanotube/carbon nanofiber composite electrode material - Google Patents
Preparation method of sulfur/carbon nanotube/carbon nanofiber composite electrode material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 61
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 61
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 55
- 239000011593 sulfur Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000002134 carbon nanofiber Substances 0.000 title claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920002749 Bacterial cellulose Polymers 0.000 claims abstract description 52
- 239000005016 bacterial cellulose Substances 0.000 claims abstract description 52
- 239000000017 hydrogel Substances 0.000 claims abstract description 38
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 23
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 23
- 239000004964 aerogel Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- 239000012300 argon atmosphere Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 8
- 238000000151 deposition Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000008104 plant cellulose Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 1
- XKTYXVDYIKIYJP-UHFFFAOYSA-N 3h-dioxole Chemical compound C1OOC=C1 XKTYXVDYIKIYJP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a sulfur/carbon nano tube/carbon nano fiber composite electrode material, which comprises the following steps: step S1, preparing a sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material; step S2, converting the bacterial cellulose in the sulfur/carbon nanotube/bacterial cellulose hydrogel composite material into carbon nanofibers, thereby forming a sulfur/carbon nanotube/carbon nanofiber aerogel composite material. By adopting the technical scheme of the invention, the carbon nanofiber net structure can be constructed, and the sulfur in the structure is effectively coated by the nano particles, so that the electronic conductivity in the electrode is increased, and the transmission efficiency of electrons in the electrode is improved. The technical scheme can provide a novel preparation method for manufacturing the electrode material.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a sulfur/carbon nanotube/carbon nanofiber composite material.
Background
The problem of energy shortage has become more and more serious over the past decades. With the development of science and technology, people put higher demands on energy storage systems and chemical power sources. The elemental sulfur has rich reserves in the earth, and has the characteristics of low price, environmental friendliness and the like. The lithium-sulfur battery using sulfur as the anode material has higher material theoretical specific capacity and battery theoretical specific energy which respectively reach 1675m Ah/g and 2600 Wh/kg. And thus is considered to be one of the most promising next-generation lithium ion batteries.
Lithium sulfur batteries have three major problems: 1. lithium polysulfide is easily dissolved in organic electrolyte and causes 'shuttle effect', which causes active substance loss and reduces the electrochemical performance of the battery; 2. sulfur is used as a non-conductive substance, so that the conductivity is very poor, and the high-rate performance of the battery is not facilitated; 3. during charging and discharging of sulfur, the volume of sulfur expands and shrinks greatly, and the battery may be damaged.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a preparation method of a sulfur/carbon nanotube/carbon nanofiber composite electrode material. The scheme does not need to add a binder in the process of preparing the electrode, and is applied to the lithium-sulfur battery.
In order to solve the technical problems in the prior art, the technical scheme of the invention is as follows:
a preparation method of a sulfur/carbon nano tube/carbon nano fiber composite electrode material is used for preparing a lithium-sulfur battery positive electrode material of a sulfur self-supporting composite material by utilizing bacterial cellulose hydrogel, and comprises the following steps:
step S1, preparing a sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material;
step S2, converting the bacterial cellulose in the sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material into carbon nano fibers, thereby forming a sulfur/carbon nano tube/carbon nano fiber aerogel composite material;
wherein the step S1 further comprises the steps of:
s10: repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel;
s11: preparing sodium thiosulfate and a carbon nano tube aqueous solution, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution.
The step S2 further includes the steps of:
s20: stirring the absorbed bacterial cellulose in dilute hydrochloric acid, and reacting with sodium thiosulfate to generate sulfur which is deposited on the carbon nano tube to obtain sulfur/carbon nano tube/bacterial cellulose hydrogel;
s21: and (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 2-4 hours, and then self-heating and cooling to obtain the finished sulfur/carbon nanotube/carbon nanofiber composite material.
Preferably, in step S11, the mass ratio of the sodium thiosulfate to the carbon nanotubes to the water is 1:0.6:80 at room temperature.
Preferably, in step S21, the mixture is heated to 50-100 ℃ at a rate of 2 ℃/min for 2 hours under the protection of argon atmosphere.
The invention also discloses a lithium-sulfur battery, and the positive electrode material of the lithium-sulfur battery adopts a sulfur/carbon nano tube/carbon nano fiber composite material.
Compared with the prior art, the invention has the following beneficial effects:
(1) the bacterial cellulose has fine structure which can reach the nanometer level, and is converted into a carbon nanofiber mesh structure after high-temperature carbonization, and the mesh structure is favorable for the transmission of electrons in the electrode and lithium ions in the electrolyte.
(2) The carbon nano tube enables sulfur particles to be effectively coated by the carbon material, so that the electronic conductivity of the electrode can be improved, and the shuttle effect can be inhibited.
(3) The constructed positive electrode is a self-supporting electrode, so that a conductive agent and an adhesive are not required to be added, the electronic conduction of the electrode is facilitated, the content and the loading capacity of active substances in the electrode are improved, and the battery installation process can be simplified.
Drawings
FIG. 1 is a flow chart of the steps of the method of preparing the sulfur/carbon nanotube/carbon nanofiber composite of the present invention;
fig. 2 is an SEM image of the sulfur/carbon nanotube/carbon nanofiber composite of instantiation 1 of the present invention, as observed under a scanning electron microscope;
the following specific embodiments will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
In order to better explain the process and scheme of the present invention, the following invention is further described with reference to the accompanying drawings and examples. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
Compared with plant cellulose, the bacterial cellulose has high crystallinity (up to 95 percent and 65 percent of plant cellulose) and high polymerization degree (DP value of 2000-8000), and has strong water absorption capacity, high tensile strength and controllability during synthesis. By utilizing the technical characteristics, the invention provides a method for preparing a lithium-sulfur battery positive electrode material of a sulfur/carbon nano tube/carbon nano fiber composite material by utilizing bacterial cellulose hydrogel, and the method is shown in figure 1 and comprises the following steps:
step S1, preparing a sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material;
step S2, converting the bacterial cellulose in the sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material into carbon nano fibers, thereby forming a sulfur/carbon nano tube/carbon nano fiber aerogel composite material;
wherein the step S1 further comprises the steps of:
s10: repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel;
s11: preparing sodium thiosulfate and a carbon nano tube aqueous solution, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution.
The step S2 further includes the steps of:
s20: stirring the absorbed bacterial cellulose in dilute hydrochloric acid, and reacting with sodium thiosulfate to generate sulfur which is deposited on the carbon nano tube to obtain sulfur/carbon nano tube/bacterial cellulose hydrogel;
s21: and (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 2-4 hours, and then self-heating and cooling to obtain the finished sulfur/carbon nanotube/carbon nanofiber composite material.
In the technical scheme, the carbon nano tube enables sulfur to be better coated, and then the original moisture of the bacterial cellulose is removed; and then heating and drying to prepare the sulfur/carbon nano tube/carbon nano fiber composite material.
EXAMPLE 1
And repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel. Preparing sodium thiosulfate and carbon nano tube aqueous solution according to the mass ratio of 7:10.2:14 at room temperature, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution. And then, putting the well absorbed bacterial cellulose into dilute hydrochloric acid for stirring, reacting with sodium thiosulfate to generate sulfur, and depositing the sulfur on the carbon nano tube to obtain the sulfur/carbon nano tube/bacterial cellulose hydrogel. And (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 2 hours, and taking out after self-heating and cooling to obtain the sulfur/carbon nanotube/carbon nanofiber composite material.
Instantiation 2 bacterial cellulose hydrogel was repeatedly rinsed in deionized water to remove impurities and water from the hydrogel. Preparing sodium thiosulfate and carbon nano tube aqueous solution according to the mass ratio of 2:4.6:5 at room temperature, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution. And then, putting the well absorbed bacterial cellulose into dilute hydrochloric acid for stirring, reacting with sodium thiosulfate to generate sulfur, and depositing the sulfur on the carbon nano tube to obtain the sulfur/carbon nano tube/bacterial cellulose hydrogel. And (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 2 hours, and taking out after self-heating and cooling to obtain the sulfur/carbon nanotube/carbon nanofiber composite material.
Instantiation 3
And repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel. Preparing sodium thiosulfate and carbon nano tube aqueous solution according to the mass ratio of 7:10.2:14 at room temperature, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution. And then, putting the well absorbed bacterial cellulose into dilute hydrochloric acid for stirring, reacting with sodium thiosulfate to generate sulfur, and depositing the sulfur on the carbon nano tube to obtain the sulfur/carbon nano tube/bacterial cellulose hydrogel. And (3) putting the hydrogel into a tube furnace, heating to 70-120 ℃ under the protection of an argon atmosphere, drying for 2 hours, and taking out after self-heating and cooling to obtain the sulfur/carbon nanotube/carbon nanofiber composite material.
Instantiation 4
And repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel. Preparing sodium thiosulfate and carbon nano tube aqueous solution at room temperature according to the mass ratio of 9:11.6:16:360, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution. And then, putting the well absorbed bacterial cellulose into dilute hydrochloric acid for stirring, reacting with sodium thiosulfate to generate sulfur, and depositing the sulfur on the carbon nano tube to obtain the sulfur/carbon nano tube/bacterial cellulose hydrogel. And (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 4 hours, and taking out after self-heating and cooling to obtain the sulfur/carbon nanotube/carbon nanofiber composite material.
Fig. 2 is an SEM image of the sulfur/carbon nanotube/carbon nanofiber composite material of instantiation 1 of the present invention, which is observed under a scanning electron microscope, and can be seen from the image.
Further, the sulfur/carbon nanotube/carbon nanofiber composite material obtained above was cut into circular electrode sheets having a diameter of 16mm, and batteries were assembled.
The specific assembly process is as follows: the cells were assembled using LIR2032 coin cells in a glove box filled with argon protection at a humidity and oxygen concentration below 1 ppm. The composite material of sulfur/carbon nano tube/carbon nano fiber is a positive electrode, Celgard2325 is used as a diaphragm, and 1mLiTFSI is dissolved in 1, 3-Dioxolane (DOL) and ethylene glycol dimethyl ether (DME) (volume ratio is 1:1) to be used as electrolyte.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. A preparation method of a sulfur/carbon nanotube/carbon nanofiber composite electrode material is characterized by comprising the following steps:
step S1, preparing a sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material;
step S2, converting the bacterial cellulose in the sodium thiosulfate/carbon nano tube/bacterial cellulose hydrogel composite material into carbon nano fibers, thereby forming a sulfur/carbon nano tube/carbon nano fiber aerogel composite material;
wherein the step S1 further comprises the steps of:
s10: repeatedly washing the bacterial cellulose hydrogel in deionized water to remove impurities and remove water in the hydrogel;
s11: preparing sodium thiosulfate and a carbon nano tube aqueous solution, and soaking the bacterial cellulose in the solution for 30-50 minutes to enable the bacterial cellulose to fully absorb the solution;
the step S2 further includes the steps of:
s20: stirring the absorbed bacterial cellulose in dilute hydrochloric acid, and reacting with sodium thiosulfate to generate sulfur which is deposited on the carbon nano tube to obtain sulfur/carbon nano tube/bacterial cellulose hydrogel;
s21: and (3) putting the hydrogel into a tube furnace, heating to 50-100 ℃ under the protection of an argon atmosphere, drying for 2-4 hours, and then self-heating and cooling to obtain the finished sulfur/carbon nanotube/carbon nanofiber composite material.
2. The method for preparing a sulfur/carbon nanotube/carbon nanofiber composite electrode material as claimed in claim 1, wherein in step S11, the mass ratio of sodium thiosulfate to carbon nanotube to water is 1:0.6: 80.
3. The method for preparing a sulfur/carbon nanotube/carbon nanofiber composite electrode material according to claim 1, wherein in step S21, heating is performed at a rate of 2 ℃/min to 50 ℃ to 100 ℃ for 2 hours under an argon atmosphere.
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