CN111740093A - Method for preparing reduced graphene/aminated column [5] arene/sulfur serving as lithium-sulfur positive electrode material - Google Patents
Method for preparing reduced graphene/aminated column [5] arene/sulfur serving as lithium-sulfur positive electrode material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 49
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 22
- 239000011593 sulfur Substances 0.000 title claims abstract description 22
- 150000004945 aromatic hydrocarbons Chemical class 0.000 title claims abstract description 20
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 10
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims abstract description 9
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 28
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 18
- 235000010323 ascorbic acid Nutrition 0.000 claims description 11
- 229960005070 ascorbic acid Drugs 0.000 claims description 11
- 239000011668 ascorbic acid Substances 0.000 claims description 11
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 11
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000010406 cathode material Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000005576 amination reaction Methods 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 229920001021 polysulfide Polymers 0.000 abstract description 6
- 239000005077 polysulfide Substances 0.000 abstract description 6
- 150000008117 polysulfides Polymers 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 125000003277 amino group Chemical group 0.000 abstract description 2
- 239000010405 anode material Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- H01M2004/028—Positive electrodes
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Abstract
The invention discloses a method for preparing reduced graphene/aminated column [5] arene/sulfur serving as a lithium-sulfur positive electrode material, and belongs to the field of chemical batteries. The reduced graphene/aminated column [5] arene/sulfur is used as a lithium sulfur positive electrode material, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide are used for promoting bonding between amine groups on aminated column [5] arene and rich oxygen-containing functional groups on the surface of graphene oxide, and the aminated column arene inhibits polysulfide dissolution from physical constraint and chemical adsorption. The anode material synthesized by the method has the advantages of high capacity, good rate capability and long cycle life.
Description
Technical Field
The invention belongs to the field of chemical batteries, and particularly relates to a method for preparing reduced graphene/aminated column [5] arene/sulfur serving as a lithium-sulfur positive electrode material.
Background
The development of electric vehicles to reduce the dependence of vehicles on non-renewable petrochemical resources and simultaneously reduce the emission of environmental pollution exhaust gas, and promote electrification, is widely considered to be the most reasonable and reliable method at present. Lead-acid batteries are large in mass and volume, low in energy density, short in service life, slow in charging speed, and have been severely limited in production and use in many countries due to their large manufacturing pollution and unsuitability for the development of electric vehicles.
In contrast, lithium-sulfur batteries have the characteristics of relatively low self-discharge, very high capacity density, low toxicity, low cost, and environmental friendliness, and thus are very promising cathode materials. The factors influencing the specific cycle size and service life of lithium-sulfur batteries are mainly the positive electrode composite material. Therefore, the search and development of new positive electrode materials for lithium-sulfur batteries has been a problem that needs to be solved. Elemental sulfur is a very promising positive electrode material due to the characteristics of low toxicity, low cost and environmental friendliness. However, the lithium-sulfur battery still has the problems of poor battery cyclicity, low coulombic efficiency, high self-discharge rate and the like in the discharging process, and the practical step of the lithium-sulfur battery is delayed.
The original graphene has excellent conductivity, can improve the conductivity of sulfur after being compounded with elemental sulfur, is beneficial to electron and ion transfer in the charging and discharging processes, has the advantages of high capacity, good rate capability and long cycle life due to the function of inhibiting polysulfide dissolution from physical constraint and chemical adsorption of aminated column [5] arene, and provides reference for theoretical research and further development of lithium-sulfur batteries.
Disclosure of Invention
The invention aims to provide a method for preparing reduced graphene/aminated column [5] arene/sulfur with good cycling stability as a lithium-sulfur positive electrode material.
The technical solution for realizing the purpose of the invention is as follows:
a method for preparing reduced graphene/aminated column [5] arene/sulfur serving as a lithium-sulfur positive electrode material comprises the following steps:
1) synthesis of GO @ AP 5A supermolecular graphene composite material
Adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS) into a graphene oxide solution, performing ultrasonic homogenization, stirring for more than 30min, adding amination column [5] arene (AP [5] A), continuously stirring for 0.5-1 h, heating to a certain temperature and keeping the temperature constant, and dialyzing a product after reaction to obtain a GO @ AP [5] A supramolecular graphene composite material;
2) synthesis of reduced graphene/aminated column [5] arene/sulfur as lithium-sulfur cathode material (rGO @ AP [5] A @ S)
Adding Ascorbic Acid (AA) as a reducing agent into the GO @ AP 5A supermolecule graphene composite material to reduce GO, stirring for more than 2h at room temperature, adding a concentrated hydrochloric acid solution, slowly dropwise adding a sodium thiosulfate aqueous solution to provide a sulfur source, slowly stirring for more than 6h to enable the concentrated hydrochloric acid and the sodium thiosulfate to react to generate elemental sulfur, collecting liquid, and centrifuging to obtain the cathode material.
Preferably, in the step 1), the mass ratio of the amination column [5] arene to the graphene oxide is 1: 1-2, and the ratio is that the amination column arene is distributed on the surface of the graphene oxide moderately and uniformly.
Preferably, in the step 1), the mass ratio of the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC) to the N-hydroxysuccinimide (NHS) is 5: 4.
preferably, in step 1), the temperature is raised to 60-90 ℃ and kept constant for 2-3 h, wherein the temperature is the optimal temperature for combining GO and AP 5A, and the structures of the GO and AP 5A are not damaged.
Preferably, in the step 2), the molar ratio of the concentrated hydrochloric acid to the sodium thiosulfate is 2: 1-5: 1, and the sodium thiosulfate is fully reduced in the ratio, so that the sulfur yield is high.
Compared with the prior art, the invention has the advantages that: (1) the reduced graphene has excellent conductivity, and the conductivity of sulfur can be improved after the reduced graphene is compounded with elemental sulfur. (2) The rGO @ AP 5A @ S material prepared by the method is a supermolecular main body AP 5A with uniform and dense distribution, effectively inhibits the dissolution of polysulfide, and has the advantages of high capacity, good rate capability and long cycle life.
Drawings
FIG. 1 is a scanning electron micrograph of a rGO @ AP [5] A @ S composite prepared according to example 1 of the present invention.
FIG. 2 is a transmission electron micrograph of a rGO @ AP [5] A @ S composite prepared according to example 1 of the present invention.
FIG. 3 is a Raman plot of the rGO @ AP 5A composite prepared using example 1 of the present invention.
FIG. 4 is a graph of the charge-discharge cycle performance of a lithium-sulfur battery cathode material made from the rGO @ AP [5] A @ S composite material prepared in example 1 of the present invention.
Detailed Description
The invention is further elucidated with reference to the figures and embodiments.
The conception of the invention is as follows: the reduced graphene has excellent conductivity, and can improve the conductivity of sulfur after being compounded with elemental sulfur, so that the reduced graphene is beneficial to electron and ion transfer in the charge and discharge processes, and the aminated pillared aromatic hydrocarbon inhibits the dissolution of polysulfide from physical constraint and chemical adsorption. The battery anode material synthesized by the method has the advantages of high capacity, good rate capability and long cycle life, and provides reference for theoretical research and further development of the lithium-sulfur battery.
Therefore, the aminated column [5] arene is used for inhibiting the dissolution of polysulfide, the cycle performance of the lithium-sulfur battery is improved, and the rGO @ AP [5] A @ S supermolecule graphene composite sulfur material is prepared. Firstly, EDC and NHS are added to promote the bonding between amine groups on AP 5A and rich oxygen-containing functional groups on the surface of graphene oxide, then Ascorbic Acid (AA) is adopted as a reducing agent to reduce Graphene Oxide (GO) into reduced graphene (rGO) and concentrated hydrochloric acid and sodium thiosulfate are used for in-situ synthesis of S nanoparticles.
Example 1
1) Preparation GO @ AP [5]]A supramolecular graphene composite material: placing 40 mL of graphene oxide solution with the concentration of 1mg/mL into a round-bottom flask, adding 10 mg of EDC and 8 mg of NHS, then carrying out ultrasonic treatment for 30 minutes, stirring for half an hour, and then adding AP [5]]A40mg, stirring for 30min,oil bath heating 90oCAnd kept at the constant temperature for 2 hours. Then taking the reacted product to dialyze for two days to obtain GO @ AP [5]A supramolecular graphene composite material.
2) Preparing rGO @ AP [5] A @ S supramolecular graphene composite sulfur material: and putting the product GO @ AP 5A into a round bottom flask, adding 10 mg Ascorbic Acid (AA) into the round bottom flask, carrying out magnetic stirring reduction, stirring the mixture at room temperature for 2 hours, adding 2mL concentrated hydrochloric acid into the solution, slowly dropwise adding 10 mL of prepared 5mg/mL sodium thiosulfate aqueous solution into the solution, slowly stirring the solution for 6 hours, collecting the liquid, and centrifuging the collected liquid to obtain the rGO @ AP 5A @ S supramolecular graphene composite sulfur material.
Example 2
1) Preparation GO @ AP [5]]A supramolecular graphene composite material: placing 60 mL of graphene oxide solution with the concentration of 1mg/mL into a round-bottom flask, adding 12 mg of EDC and 10 mg of NHS, then carrying out ultrasonic treatment for 30 minutes, stirring for half an hour, and then adding AP [5]]A60mg, stirring for 30min, heating in oil bath 90oCAnd kept at the constant temperature for 2 hours. Then taking the reacted product to dialyze for two days to obtain GO @ AP [5]A supramolecular graphene composite material.
2) Preparing rGO @ AP [5] A @ S supramolecular graphene composite sulfur material: putting the product GO @ AP 5A into a round bottom flask, adding 10 mg Ascorbic Acid (AA) into the round bottom flask, carrying out magnetic stirring reduction, stirring the mixture for 2 hours at room temperature, adding 2mL concentrated hydrochloric acid solution into the solution, slowly dripping 10 mL of prepared 5mg/mL sodium thiosulfate aqueous solution into the solution, slowly stirring the solution for 6 hours, collecting the liquid, and centrifuging the collected liquid to obtain the rGO @ AP 5A @ S supramolecular graphene composite sulfur material.
Example 3
1) Preparation GO @ AP [5]]A supramolecular graphene composite material: placing 80 mL of graphene oxide solution with the concentration of 1mg/mL into a round-bottom flask, adding 20 mg of EDC and 16 mg of NHS, then carrying out ultrasonic treatment for 30 minutes, stirring for half an hour, and then adding AP [5]]A80 mg, stirring for 30min, heating in oil bath for 90 minoCAnd kept at the constant temperature for 2 hours. Then taking the reacted product to dialyze for two days to obtain GO @ AP [5]A supramolecular graphene composite material.
2) Preparing rGO @ AP [5] A @ S supramolecular graphene composite sulfur material: putting the product GO @ AP 5A into a round bottom flask, adding 10 mg Ascorbic Acid (AA) into the round bottom flask, carrying out magnetic stirring reduction, stirring the mixture for 2 hours at room temperature, adding 2mL concentrated hydrochloric acid solution into the solution, slowly dripping 10 mL of prepared 5mg/mL sodium thiosulfate aqueous solution into the solution, slowly stirring the solution for 6 hours, collecting the liquid, and centrifuging the collected liquid to obtain the rGO @ AP 5A @ S supramolecular graphene composite sulfur material.
FIG. 1 shows a scanning electron micrograph of the rGO @ AP [5] A @ S composite prepared in example 1 of the present invention. Therefore, the prepared graphene material has a smooth surface and uniformly distributed small luck spheres in the shape.
FIG. 2 shows a transmission electron micrograph of the rGO @ AP [5] A @ S composite prepared in example 1 of the present invention. The graphene sheet layer is thin, and elemental sulfur is uniformly dispersed on the surface of graphene in the form of small particles.
FIG. 3 is rGO @ AP [5] prepared using example 1 of the present invention]Raman graph of a composite material. . The GO strength ratio (I)D/IG) Is 0.85 and rGO @ AP [5]]Intensity ratio of A (I)D/IG) Is 0.93. The increase in intensity ratio is shown to be due to AP [5]]The addition of a results in an increase in rGO surface defects, i.e. active sites, which can increase polysulfide adsorption.
FIG. 4 is a graph of the performance of the GO @ AP [5] A @ S composite made using example 1 of the present invention cycled 200 cycles at 1.0C. As can be seen from the figure, the initial discharge specific capacity is 988.79 mAh/g, the cycling stability is good, the capacity is hardly attenuated after 200 circles, and the capacity is stabilized at 937.54 mAh/g.
Claims (5)
1. A method for preparing reduced graphene/aminated column [5] arene/sulfur serving as a lithium-sulfur positive electrode material is characterized by comprising the following steps:
1) synthesis of GO @ AP 5A supermolecular graphene composite material
Adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide into a graphene oxide solution, performing ultrasonic homogenization, stirring for more than 30min, adding amination column [5] arene, continuously stirring for 0.5-1 h, heating to a certain temperature, keeping the temperature constant, and dialyzing a product after reaction to obtain a GO @ AP [5] A supramolecular graphene composite material;
2) synthesis of reduced graphene/aminated column [5] arene/sulfur as lithium-sulfur cathode material
Adding ascorbic acid as a reducing agent into the GO @ AP 5A supermolecule graphene composite material, stirring for more than 2h at room temperature, adding concentrated hydrochloric acid, slowly dropwise adding a sodium thiosulfate aqueous solution, slowly stirring for more than 6h to enable the concentrated hydrochloric acid and the sodium thiosulfate to react to generate elemental sulfur, collecting liquid, and centrifuging to obtain the cathode material.
2. The method according to claim 1, wherein in the step 1), the mass ratio of the aminated column [5] arene to the graphene oxide is 1: 1-2.
3. The method of claim 1, wherein in step 1), the mass ratio of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to N-hydroxysuccinimide is 5: 4.
4. the method according to claim 1, wherein in the step 1), the temperature is raised to 60-90 ℃ and kept constant for 2-3 h.
5. The method according to claim 1, wherein in step 2), the molar ratio of concentrated hydrochloric acid to sodium thiosulfate is 2:1 to 5: 1.
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