LU500737B1 - Preparation method of ordered mesoporous Co/CMK composite nano anode material - Google Patents
Preparation method of ordered mesoporous Co/CMK composite nano anode material Download PDFInfo
- Publication number
- LU500737B1 LU500737B1 LU500737A LU500737A LU500737B1 LU 500737 B1 LU500737 B1 LU 500737B1 LU 500737 A LU500737 A LU 500737A LU 500737 A LU500737 A LU 500737A LU 500737 B1 LU500737 B1 LU 500737B1
- Authority
- LU
- Luxembourg
- Prior art keywords
- cmk
- ordered mesoporous
- certain amount
- distilled water
- hours
- Prior art date
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000010405 anode material Substances 0.000 title description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 36
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 17
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 16
- 229930006000 Sucrose Natural products 0.000 claims abstract description 16
- 239000005720 sucrose Substances 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 9
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- 239000012153 distilled water Substances 0.000 claims description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007772 electrode material Substances 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 7
- 238000010000 carbonizing Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 abstract description 8
- 239000010941 cobalt Substances 0.000 abstract description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003575 carbonaceous material Substances 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 239000007773 negative electrode material Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 229920001577 copolymer Polymers 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 239000010406 cathode material Substances 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 238000000527 sonication Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
-
- 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
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A method for preparing an ordered mesoporous Co/CMK composite nano negative electrode material, which belongs to the technical field of nano materials and chemical power sources. The method includes first using the copolymer P123 as a template and tetraethylorthosilicate as a silicon source to synthesize SBA-15 by hydrothermal method, and then use this as a hard template and sucrose as a carbon source to synthesize ordered mesoporous carbon material CMK-3; then, the ordered mesoporous Co/CMK-3 composite nanomaterial was obtained in the CoCl2 6H2O solution through reduced pressure ultrasound, and finally the ordered mesoporous Co/CMK composite nanomaterial was reduced by hydrothermal method with hydrazine hydrate. The ordered mesoporous Co/CMK composite nano material prepared by this method can relieve the volume expansion/shrinkage during charging and discharging, and at the same time, the cobalt metal component increases the conductivity of the material. The cycle performance and coulombic efficiency of the battery are improved.
Description
DESCRIPTION 10500737 Preparation method of ordered mesoporous Co/CMK composite nano anode material
TECHNICAL FIELD The invention belongs to the technical field of nano materials and chemical power sources, and relates to a method for preparing an ordered mesoporous Co/CMK composite nano negative electrode material, and in particular to a hydrothermal method for preparing CMK -3 and an ultrasonic method for preparing a cobalt-loaded CMK-3 mixture.
BACKGROUND With the development of the world economy, while people's living standards are improving, energy crisis and environmental pollution have increasingly become unavoidable problems in today's society. With the gradual depletion of resources, the acquisition and storage of renewable energy has gained extensive attention and research in the world. Lithium-ion batteries have many advantages, such as high energy density, long service life, environmental friendliness, and no memory effect. In recent years, lithium-ion batteries have been widely used in portable electronic equipment, transportation and other fields, and have also been greatly promoted and applied in aerospace and military fields. With the rapid development of transportation industry and electronic communication, the service life and energy density of lithium ion batteries are required to be higher. As the main body of lithium storage, the cathode materials of lithium batteries play a decisive role in the performance of lithium batteries. However, most of the cathode materials of commercial lithium batteries are carbon materials with low specific capacity, which can no longer meet people's demand for high energy density.
Ordered mesoporous carbon materials have high specific surface area and high porosity. The aperture size can be adjusted within a certain range; mesopores have various shapes and adjustable pore wall composition, structure and properties. High thermal stability and hydrothermal stability can be obtained by optimizing synthesis conditions. The synthesis is simple, easy to operate, and has no physiological toxicity. The interconnected carbon walls give it excellent electrical conductivity. However, when mesoporous carbon materials are directly applied to lithium battery cathode materials, the first coulombic efficiency can only reach about 34%, which makes it impossible to be used in commercial batteries. Through the combination of mesoporous carbon with metal and its oxide, the specific surface area of 10500737 mesoporous carbon is reduced, and the activation point is reduced, thus reducing the irreversible capacity. Meanwhile, the three-dimensional network structure of mesoporous carbon provides a good channel for lithium ion transmission, which is beneficial to the mutual reaction between electrolyte, lithium ion and electrode materials, thus facilitating the charge-discharge contact between lithium ion and active substances, improving its coulombic efficiency and improving its cycle performance.
Cobalt is a simple metal. As the cathode material of lithium battery, although it can not react directly with lithium ions, it can catalyze the electrochemical reaction in the battery. Combining the advantages of cobalt and mesoporous carbon, we made cobalt nanoparticles nano-sized, and the cobalt nanoparticles were uniformly diffused in the internal pore channels of mesoporous carbon by ultrasound, which was conducive to the direct contact between active materials and electrolyte, which not only improved the lithium storage performance of negative electrode materials, but also improved the discharge capacity and cycle stability of batteries.
In the prior art, there is an urgent need for a method for preparing an ordered mesoporous Co/CMK composite nano-electrode material.
SUMMARY The purpose of the present invention is to overcome the defects of the above technology, and provide a preparation method of ordered mesoporous Co/CMK composite nano negative electrode material, which is required to improve cycle performance and initial capacity. At the same time, the method has low processing cost, simple production method, energy saving and environmental protection, and is convenient for large-scale investment and production.
According to the technical scheme of the invention, copolymer P123 is used as a template agent, tetraethyl orthosilicate (TEOS) is used as a silicon source, mesoporous molecular sieve SBA-15 is hydrothermally synthesized, and then ordered mesoporous carbon material CMK-3 is synthesized by using SBA-15 as a template and sucrose as a carbon source. Then, the Co/CMK nano-composite cathode material was prepared by combining the precursor of cobalt with ultrasonic under reduced pressure, and finally reducing it with hydrazine hydrate through hydrothermal reaction.
In order to achieve the above technical purpose, the technical scheme of the invention is 10500737 as follows: the method for preparing the ordered mesoporous Co/CMK composite nano cathode material comprises the following steps: (1) weighing a certain amount of template P123, dissolving it in 2mol/L hydrochloric acid solution at 35°C, adding a certain amount of tetraethylorthosilicate TEOS and distilled water, and continuously stirring for 5-12h; transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15; (2) weighing a certain amount of SBA-15 prepared in step (1) and add it into a solution containing a certain amount of sucrose, concentrated sulfuric acid and distilled water, and heat it at 100°C and 160°C for 6h respectively. After cooling, add a certain amount of sucrose, concentrated sulfuric acid and distilled water, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C under N2 protection. After the carbonization is finished, the template is removed with 5% HF solution, washed with distilled water, and dried at 120°C. Finally, add the dried sample to a 1mol/L concentrated sulfuric acid solution and reflux, place it at 80°C for 3 hours, and then wash and dry it to obtain ordered mesoporous carbon CMK-3; (3) weighing a certain amount of CMK-3 prepared in step (2), a certain amount of CoCl::6H:0 and cetyltrimethylammonium bromide CTAB into distilled water, ultrasonic under circulating water, adding a certain amount of hydrazine hydrate after ultrasonic, continuously stirring for 1-2h, transferring the solution to a reaction kettle, performing hydrothermal reaction, washing with water, and drying in vacuum for 1-2h to obtain the Co/CMK composite nano negative electrode material.
Further, in the step (3), the ultrasonic time is 1-2h, and the ultrasonic power is 60-100w.
Furthermore, the temperature of the hydrothermal reaction in step (3) is 180°C, the hydrothermal reaction time is 5 h, and the heating rate in the hydrothermal reaction process is 2°C/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the ordered mesoporous Co/CMK composite nano cathode material of the present 10500737 invention combines the excellent catalytic performance of metallic cobalt with the advantages of high conductivity and high specific surface area of mesoporous carbon to form complementary advantages, make up for the defects of single mesoporous carbon material, improve the cycle stability and initial capacity of lithium batteries, and open up new ideas for the application of mesoporous materials.
(2) The ordered mesoporous Co/CMK composite nano cathode material has simple preparation process, low cost and environmental friendliness.
BRIEF DESCRIPTION OF THE FIGURES Figure 1 is a transmission electron microscope image of an ordered mesoporous Co/CMK nanocomposite; Figure 2 is a graph of the cycle performance of ordered mesoporous Co/CMK nanocomposites.
DESCRIPTION OF THE INVENTION In order to make the technical means, creative features, objectives and effects of the present invention easy to understand, the present invention will be further described in conjunction with the accompanying drawings and specific embodiments below.
Embodiment 1 (1) Weighing 2g of template agent P123, dissolve it in 60mL of 2mol/L hydrochloric acid solution at 35°C, then add 4.4mL of tetraethylorthosilicate (TEOS) and 15mL of distilled water, and continue to stir for 5-12h, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15.
(2) Adding 1g SBA-15 into the solution containing 1.25g sucrose, 0.14g concentrated sulfuric acid and SmL distilled water, heat it at 100°C and 160°C for 6h respectively, add 0.8g sucrose, 0.09g concentrated sulfuric acid and Sg distilled water after cooling, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C for 6h under N2 protection. After carbonization and grinding, the template was removed with 5% HF solution, washed repeatedly with distilled water and dried at 120°C. And finally, adding the dried sample into 1mol/L concentrated sulfuric acid solution for refluxing, standing at 80°C for 3h, 10500737 and then washing and drying to obtain the ordered mesoporous carbon CMK-3.
(3) Weighing 0.1g of CMK-3, 0.476g of CoCl,:6H:0, 0.360g into 40mL of distilled water, sonicate under circulating water for 2h, the ultrasonic power is 60W, adding 45ml of hydrazine hydrate after sonication, and continue to stir for 2h. Then the solution was transferred to the reaction kettle, hydrothermally reacted at 180°C for 6 hours, washed with water, and dried under vacuum at 50°C for 12 hours to obtain an ordered mesoporous Co/CMK composite nano-electrode material.
Embodiment 2 (1) Weighing 2g of template agent P123, dissolve it in 60mL of 2mol/L hydrochloric acid solution at 35°C, then add 4.4mL of tetraethylorthosilicate (TEOS) and 15mL of distilled water, and continue to stir for 5-12h, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15.
(2) Adding 1g SBA-15 into the solution containing 1.25g sucrose, 0.14g concentrated sulfuric acid and SmL distilled water, heat it at 100°C and 160°C for 6h respectively, add 0.8g sucrose, 0.09g concentrated sulfuric acid and Sg distilled water after cooling, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C for 6h under N2 protection. After carbonization and grinding, the template was removed with 5% HF solution, washed repeatedly with distilled water and dried at 120°C. And finally, adding the dried sample into Imol/L concentrated sulfuric acid solution for refluxing, standing at 80°C for 3h, and then washing and drying to obtain the ordered mesoporous carbon CMK-3.
(3) Weighing 0.1g of CMK-3, 0.532g of CoCl;-6H,O, 0.391g into 40mL of distilled water, sonicate under circulating water for 2h, the ultrasonic power is 70W, adding 50ml of hydrazine hydrate after sonication, and continue to stir for 2h. Then the solution was transferred to the reaction kettle, hydrothermally reacted at 180°C for 6 hours, washed with water, and dried under vacuum at 60°C for 12 hours to obtain an ordered mesoporous Co/CMK composite nano-electrode material.
Embodiment 3
(1) Weighing 2g of template agent P123, dissolve it in 60mL of 2mol/L hydrochloric acid 10500737 solution at 35°C, then add 4.4mL of tetraethylorthosilicate (TEOS) and 15mL of distilled water, and continue to stir for 5-12h, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15.
(2) Adding 1g SBA-15 into the solution containing 1.25g sucrose, 0.14g concentrated sulfuric acid and SmL distilled water, heat it at 100°C and 160°C for 6h respectively, add 0.8g sucrose, 0.09g concentrated sulfuric acid and Sg distilled water after cooling, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C for 6h under N2 protection. After carbonization and grinding, the template was removed with 5% HF solution, washed repeatedly with distilled water and dried at 120°C. And finally, adding the dried sample into Imol/L concentrated sulfuric acid solution for refluxing, standing at 80°C for 3h, and then washing and drying to obtain the ordered mesoporous carbon CMK-3.
(3) Weighing 0.1g of CMK-3, 0.621g of CoCl;-6H,0O, 0.450g into 60mL of distilled water, sonicate under circulating water for 2h, the ultrasonic power is 80W, adding 55ml of hydrazine hydrate after sonication, and continue to stir for 2h. Then the solution was transferred to the reaction kettle, hydrothermally reacted at 180°C for 5 hours, washed with water, and dried under vacuum at 70°C for 12 hours to obtain an ordered mesoporous Co/CMK composite nano-electrode material.
Embodiment 4 (1) Weighing 2g of template agent P123, dissolve it in 60mL of 2mol/L hydrochloric acid solution at 35°C, then add 4.4mL of tetraethylorthosilicate (TEOS) and 15mL of distilled water, and continue to stir for 5-12h, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15.
(2) Adding 1g SBA-15 into the solution containing 1.25g sucrose, 0.14g concentrated sulfuric acid and SmL distilled water, heat it at 100°C and 160°C for 6h respectively, add 0.8g sucrose, 0.09g concentrated sulfuric acid and Sg distilled water after cooling, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C for 6h under N2 10500737 protection. After carbonization and grinding, the template was removed with 5% HF solution, washed repeatedly with distilled water and dried at 120°C. And finally, adding the dried sample into Imol/L concentrated sulfuric acid solution for refluxing, standing at 80°C for 3h, and then washing and drying to obtain the ordered mesoporous carbon CMK-3.
(3) Weighing 0.1g of CMK-3, 0.476g of CoCl,:6H:0, 0.360g into 40mL of distilled water, sonicate under circulating water for 2h, the ultrasonic power is 60W, adding 45ml of hydrazine hydrate after sonication, and continue to stir for 2h. Then the solution was transferred to the reaction kettle, hydrothermally reacted at 180°C for 6 hours, washed with water, and dried under vacuum at 50°C for 12 hours to obtain an ordered mesoporous Co/CMK composite nano-electrode material.
Embodiment 5 (1) Weighing 2g of template agent P123, dissolve it in 60mL of 2mol/L hydrochloric acid solution at 35°C, then add 4.4mL of tetraethylorthosilicate (TEOS) and 15mL of distilled water, and continue to stir for 5-12h, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15.
(2) Adding 1g SBA-15 into the solution containing 1.25g sucrose, 0.14g concentrated sulfuric acid and SmL distilled water, heat it at 100°C and 160°C for 6h respectively, add 0.8g sucrose, 0.09g concentrated sulfuric acid and Sg distilled water after cooling, continue heating at 100°C and 160°C for 6h respectively, and then carbonize it at 877°C for 6h under N2 protection. After carbonization and grinding, the template was removed with 5% HF solution, washed repeatedly with distilled water and dried at 120°C. And finally, adding the dried sample into Imol/L concentrated sulfuric acid solution for refluxing, standing at 80°C for 3h, and then washing and drying to obtain the ordered mesoporous carbon CMK-3.
(3) Weighing 0.1g of CMK-3, 0.476g of CoCl;-6H,O, 0.360g into 40mL of distilled water, sonicate under circulating water for 2h, the ultrasonic power is 60W, adding 45ml of hydrazine hydrate after sonication, and continue to stir for 2h. Then the solution was transferred to the reaction kettle, hydrothermally reacted at 180°C for 6 hours, washed with water, and dried under vacuum at 50°C for 12 hours to obtain an ordered mesoporous 17500787 Co/CMK composite nano-electrode material.
The above is only the best mode of the present invention, and any simple change or equivalent replacement of the technical scheme that can be obviously obtained by any person familiar with the technical field within the technical scope disclosed by the present invention falls within the protection scope of the present invention.
Claims (3)
1. A preparation method of ordered mesoporous Co/CMK composite nano-electrode material, characterized in that it comprises the following steps: (1) weighing a certain amount of template agent P123 and dissolving it in a 2mol/L hydrochloric acid solution at 35°C, then adding a certain amount of tetraethylorthosilicate TEOS and distilled water, and continuing to stir for 5-12 hours, transferring the solution to a reaction kettle, hydrothermal aging at 120°C for 24h, washing with water, filtering, drying, carbonizing under the protection of N2, heating from room temperature to 550°C, keeping the temperature for Sh, and naturally cooling to room temperature after calcination to obtain SBA-15; (2) weighing a certain amount of SBA-15 prepared in step (1) and adding it to a solution containing a certain amount of sucrose, concentrated sulfuric acid, and distilled water, and heating it at 100°C and 160°C for 6 hours, respectively, after cooling, adding a certain amount of sucrose, concentrated sulfuric acid and distilled water, continue to heat at 100°C and 160°C for 6 hours respectively, and then carbonize at 877°C under the protection of N2; after carbonization and grinding, the template was removed with 5% HF solution, washed with distilled water and dried at 120°C, finally, adding the dried sample to a 1mol/L concentrated sulfuric acid solution and reflux, placing it at 80°C for 3 hours, and then washing and drying it to obtain ordered mesoporous carbon CMK-3; (3) weighing a certain amount of CMK-3 prepared in step (2), a certain amount of CoCl,'6H,O and cetyltrimethylammonium bromide CTAB into distilled water, after circulating underwater ultrasound, a certain amount of hydrazine hydrate is added, stirring is continued for 1-2h, the solution is transferred to a reaction kettle for hydrothermal reaction, after washing with water and drying for 12 hours in a vacuum environment, a Co/CMK composite nano-electrode material is obtained.
2. A method for preparing an ordered mesoporous Co/CMK composite nano-electrode material according to claim 1, wherein the ultrasound in step (3) has a duration of 1 to 2 hours and an ultrasound power of 60 to 100W.
3. A method for preparing an ordered mesoporous Co/CMK composite nano-electrode material according to claim 1, the temperature of the hydrothermal reaction in step (3) is
. . . . . LU500737 180°C, the hydrothermal reaction time is 5 hours, and the temperature rise rate during the hydrothermal reaction is 2°C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU500737A LU500737B1 (en) | 2021-10-15 | 2021-10-15 | Preparation method of ordered mesoporous Co/CMK composite nano anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU500737A LU500737B1 (en) | 2021-10-15 | 2021-10-15 | Preparation method of ordered mesoporous Co/CMK composite nano anode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| LU500737B1 true LU500737B1 (en) | 2022-04-15 |
Family
ID=81127815
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| LU500737A LU500737B1 (en) | 2021-10-15 | 2021-10-15 | Preparation method of ordered mesoporous Co/CMK composite nano anode material |
Country Status (1)
| Country | Link |
|---|---|
| LU (1) | LU500737B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161641A (en) * | 2022-11-02 | 2023-05-26 | 南开大学 | A method for preparing ordered mesoporous carbon from sugar-derived humic acid without cross-linking agent |
-
2021
- 2021-10-15 LU LU500737A patent/LU500737B1/en active IP Right Grant
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161641A (en) * | 2022-11-02 | 2023-05-26 | 南开大学 | A method for preparing ordered mesoporous carbon from sugar-derived humic acid without cross-linking agent |
| CN116161641B (en) * | 2022-11-02 | 2024-05-31 | 南开大学 | A method for preparing ordered mesoporous carbon using saccharide-derived humic acid without crosslinking agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110467182B (en) | Reaction template-based hierarchical porous carbon-based material and preparation method and application thereof | |
| CN104518209A (en) | Lithium ion battery silicon composite material and preparation method thereof | |
| CN107482218A (en) | A three-dimensional hollow material and its preparation method and application in electrochemical energy storage devices | |
| CN110729480A (en) | Nitrogen-doped porous hollow carbon sphere and preparation method and application thereof | |
| CN107919461A (en) | Preparation method and application of nitrogen-doped porous carbon negative electrode material | |
| CN112421044B (en) | Core-shell structure sulfur positive electrode material, preparation method and application in lithium-sulfur battery | |
| CN106159222A (en) | The lithium ion battery preparation method of Co/CMK-3 composite Nano negative material | |
| CN109950487A (en) | A kind of lithium sulfur battery anode material and preparation method thereof | |
| CN116621156B (en) | Nitrogen-doped porous carbon material and preparation method and application thereof | |
| CN112886029A (en) | Bifunctional oxygen electrocatalyst with hollow carbon nanotube as carrier, preparation and application | |
| CN111313012A (en) | Multiwalled carbon nanotube graphite lithium ion battery negative electrode material and preparation method thereof | |
| CN109301194B (en) | Phosphorus quantum dot composite porous hard carbon material, preparation method and application thereof | |
| CN116395670A (en) | A kind of preparation method of hard carbon negative electrode material of sodium ion battery | |
| CN114804039A (en) | Carbon matrix composite vanadium nitride nano array and preparation method and application thereof | |
| CN108232158A (en) | A kind of preparation method of order mesoporous Co/CMK composite Nanos negative material | |
| CN104843800B (en) | A kind of solvothermal preparation method of carbon coated ferriferrous oxide negative material | |
| CN114074936B (en) | A kind of nitrogen-doped carbon nanosphere and its preparation method and application | |
| LU500737B1 (en) | Preparation method of ordered mesoporous Co/CMK composite nano anode material | |
| CN109360961B (en) | Hollow composite microsphere for lithium-sulfur battery positive electrode material and preparation method thereof | |
| CN110061236A (en) | A kind of preparation method of the three-dimensional porous carbon negative pole material of self-supporting | |
| CN111740083B (en) | Carbon-coated porous Co3O4Microsphere lithium ion battery cathode material and preparation method thereof | |
| CN109802093A (en) | Modified non-carbon anode of lithium-air battery and preparation method thereof and lithium-air battery | |
| CN111192762B (en) | A kind of Cu-Co-P composite material and its preparation method and application | |
| CN110416512B (en) | Based on Bi4Ti3O12Preparation method of @ C/S composite material, composite material and application | |
| CN116282202B (en) | Oxygen-vacancy-rich petal-shaped lithium battery negative electrode material, preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FG | Patent granted |
Effective date: 20220415 |