CN116889884A - Preparation method and application of CS-CSS/NHC heterogeneous nanocube - Google Patents
Preparation method and application of CS-CSS/NHC heterogeneous nanocube Download PDFInfo
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- CN116889884A CN116889884A CN202310798845.9A CN202310798845A CN116889884A CN 116889884 A CN116889884 A CN 116889884A CN 202310798845 A CN202310798845 A CN 202310798845A CN 116889884 A CN116889884 A CN 116889884A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 19
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 7
- 239000011593 sulfur Substances 0.000 claims abstract description 7
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 5
- 239000011669 selenium Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000000975 co-precipitation Methods 0.000 claims abstract description 4
- 239000013384 organic framework Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 101100289192 Pseudomonas fragi lips gene Proteins 0.000 description 9
- 210000000088 lip Anatomy 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229920001021 polysulfide Polymers 0.000 description 4
- 239000005077 polysulfide Substances 0.000 description 4
- 150000008117 polysulfides Polymers 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- -1 Transition metal sulfides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002078 nanoshell Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- 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
-
- 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
- H01M2004/028—Positive electrodes
Abstract
The invention discloses a preparation method of a CS-CSS/NHC heterogeneous nanocube, which specifically uses 2-methylimidazole as an organic framework, cobalt nitrate hexahydrate as a cobalt source and water as a solvent, and synthesizes a ZIF-67 precursor by a room temperature coprecipitation method; then selenium powder/sulfur powder is used as a selenium source and a sulfur source, and finally the preparation of the CS-CSS/NHC heterogeneous nanocubes is realized by a one-step method; the method disclosed by the invention is simple in synthesis path and operation, does not need large equipment or harsh reaction conditions, and also discloses the application of the prepared CS-CSS/NHC heterogeneous nanocube in the fields of lithium-sulfur battery positive hosts and photo/electro catalysis.
Description
Technical Field
The invention belongs to the technical field of MOFs-derived N-doped carbon anchored metal selenide/metal sulfide nanocubes, and relates to a preparation method of a CS-CSS/NHC heterogeneous nanocubes.
The invention also relates to the application of the CS-CSS/NHC heterogeneous nanocubes.
Background
Transition metal sulfides have polar surfaces and significant adsorption to soluble LiPSs, have been used as functional catalysts for LSBs. For example, seo (Seunglook Seo, dongjoo Park, et al advanced Functional materials.2019,29 (38), 1903712) et al propose in situ growth of N-doped graphitic carbon nanoshell (NGCNs) matrices and embedded CoS 2 The nanoparticles act as an effective sulfur host and exhibit excellent electrochemical properties. They demonstrated a polar CoS 2 Shows strong adsorption effect on LiPSs and promotes the conversion of LiPSs. However, the inherently low conductivity of electronegative S atoms greatly limits electron delocalization in transition metals; in addition to the polarity of the catalyst, the conductivity of the polar surface plays a particularly important role as the primary active site for the LiPSs redox reaction. Transition metal selenides generally exhibit high electrical conductivity and high catalytic activity towards LiPSs due to their inherent metallic character. Therefore, the design of the difunctional synergic catalyst has important significance for realizing the strong chemical adsorption and the high-efficiency catalytic conversion of LiPSs; here, coSe having excellent adsorption ability and high catalytic activity was designed 2 -CoSe 0.25 S 1.75 Hetero-interface structure to achieve tandem catalytic effect on LiPSs "adsorption-diffusion-conversion" in LSBs, coSe 0.25 S 1.75 Captured LiPSs are CoSe 2 Further catalysis, the conversion of LiPSs is effectively promoted, so that high utilization rate of sulfur is realized, and the electrochemical performance of LSBs is further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a CS-CSS/NHC heterogeneous nanocube, which has the characteristics of simple reaction process, low temperature, easiness in control, no need of large-scale equipment and severe reaction conditions.
The technical scheme adopted by the invention is that the preparation method of the CS-CSS/NHC heterogeneous nanocube specifically takes 2-methylimidazole as an organic framework, cobalt nitrate hexahydrate as a cobalt source and water as a solvent, and a ZIF-67 precursor is synthesized by a room temperature coprecipitation method; and then selenium powder/sulfur powder is used as a selenium source and a sulfur source, and finally the preparation of the CS-CSS/NHC heterogeneous nanocubes is realized by a one-step method.
The invention is also characterized in that:
the preparation method of the CS-CSS/NHC heterogeneous nanocubes comprises the following steps:
step 1, weighing 2-methylimidazole, and then adding the 2-methylimidazole into deionized water for magnetic stirring to obtain a uniformly dispersed transparent solution A;
step 2, weighing cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into deionized water, and magnetically stirring to obtain uniformly dispersed red solution B;
step 3, rapidly mixing the two solutions under the condition of stirring to form a purple mixed solution, magnetically stirring, and then aging at room temperature to obtain a mixed solution with purple precipitate;
step 4, after the room-temperature aging is finished, obtaining a purple product through centrifugation, then cleaning and collecting the product, and then drying to obtain a ZIF-67 precursor;
step 5, weighing a certain amount of precursors ZIF-67, selenium powder and sulfur powder, placing the precursors ZIF-67, selenium powder and sulfur powder in a tube furnace filled with inert atmosphere for reaction, and cooling to room temperature to obtain a CS-CSS/NHC heterogeneous nanocube;
wherein the step 1 specifically comprises the following steps: weighing 7.3-14.7 g of 2-methylimidazole, adding the 2-methylimidazole into 13-26 ml of deionized water, and magnetically stirring for 2-10 min;
the step 2 specifically comprises the following steps: weighing 0.6-1.2 g of cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into 4-8 ml of deionized water, and magnetically stirring for 2-10 min;
wherein in the step 3, the magnetic stirring is carried out for 10-30 min, the aging is carried out for 24h, and when the two solutions are mixed, the solution B is rapidly poured into the solution A;
in the step 4, the product is collected through 2-3 times of water/methanol alternate cleaning, and the drying process is that the product is dried for 12-24 hours at the temperature of 60-80 ℃ in a vacuum drying oven;
wherein in the step 5, the mass ratio of the precursor ZIF-67 to the selenium powder to the sulfur powder is 1: (1-2): (1-2);
wherein the reaction conditions in the tube furnace in the step 5 are as follows: preserving heat for 2h at the temperature of 300-450 ℃ at the heating rate of 2 ℃/min;
and (5) removing air in the quartz glass tube before the temperature of the tube furnace begins to rise in the step (5), preventing the sample from being oxidized by the left air, mixing and grinding the precursor ZIF-67 and selenium powder, placing the precursor ZIF-67 and the selenium powder in the downstream of the tube furnace, and placing the sulfur powder in the upstream of the tube furnace.
The CS-CSS/NHC heterogeneous nanocube prepared by the preparation method of the CS-CSS/NHC heterogeneous nanocube is applied to the field of lithium-sulfur battery positive hosts or photocatalysis/electrocatalysis.
The beneficial effects of the invention are as follows:
(1) The invention synthesizes the final nanocube structure through the synchronous selenizing/vulcanizing process, and the synthesis path is simple, the operation is simple, and large-scale equipment and harsh reaction conditions are not needed;
(2) The cobalt source used in the invention is cobalt nitrate hexahydrate, the organic compound is 2-methylimidazole, the commercial selenium powder/sulfur powder is selenium source/sulfur source, the solvent is water, the needed raw and auxiliary materials are few in variety and easy to obtain, and the raw and auxiliary materials are supplied in sufficient quantity, so that the whole reaction yield is high, the environment is friendly, the product does not need subsequent treatment, and the method is suitable for large-scale production;
(3) When the invention is applied to the positive electrode material of the lithium-sulfur battery, the CoSe with strong polarity 0.25 S 1.75 Can realize strong chemical adsorption to polysulfide, high conductivity and high catalytic activity of metal CoSe 2 Exhibits high catalytic activity for polysulfide conversion, coSe 2 And CoSe 0.25 S 1.75 The built-in electric field formed by interface coupling can accelerate the transportation of polysulfide, thereby inhibiting the shuttle effect of polysulfide, improving the utilization rate of active substances and finally showing excellent multiplying power performance and cycle stability.
Drawings
FIG. 1 is an XRD pattern of the product of example 1 of the invention;
FIG. 2 is a low power scanning electron microscope image of the product prepared in example 1 of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention provides a preparation method of a CS-CSS/NHC heterogeneous nanocube, namely a ZIF-67-derived nitrogen-doped carbon-anchored CoSe with low cost and mild process conditions 2 -CoSe 0.25 S 1.75 A method for preparing heterogeneous nanocubes (CS-CSS/NHC); specifically, 2-methylimidazole is taken as an organic framework, cobalt nitrate hexahydrate is taken as a cobalt source, water is taken as a solvent, and a ZIF-67 precursor is synthesized by a room temperature coprecipitation method; then taking commercial selenium powder/sulfur powder as a selenium source and a sulfur source, and controlling parameters such as the ratio of a precursor ZIF-67 to the selenium powder/sulfur powder, the reaction temperature, the reaction time and the like to prepare the CS-CSS/NHC heterogeneous nanocubes by a one-step method, wherein the method has the advantages of simple reaction process, low temperature, easy control, no need of large-scale equipment and severe reaction conditions, and can realize the uniform dispersion of CoSe on nitrogen-doped carbon with hierarchical porous structure characteristics under relatively mild conditions 2 -CoSe 0.25 S 1.75 Heterogeneous nanoparticles; when the above product is applied as a positive host material for lithium-sulfur batteries, it can exhibit excellent electrochemical and catalytic properties.
Example 1
Step 1, weighing 11g of 2-methylimidazole, adding the 2-methylimidazole into 20ml of deionized water, and magnetically stirring for 10min to obtain a uniformly dispersed transparent solution A;
step 2, weighing 0.9g of cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into 6ml of deionized water, and magnetically stirring the mixture for 10 minutes to obtain uniformly dispersed red solution B;
step 3, rapidly mixing the two solutions under the condition of stirring to form a purple mixed solution, magnetically stirring for 10min, and then aging for 24h at room temperature to obtain a mixed solution with purple precipitation;
step 4, after the room temperature aging is finished, obtaining a purple product through centrifugation, alternately cleaning and collecting the product through water/methanol for 2-3 times, and then drying the product for 24 hours at the temperature of 60 ℃ in a vacuum drying oven to obtain a ZIF-67 precursor;
and 5, weighing 500mg of precursor ZIF-67, 1000mg of selenium powder and 500mg of sulfur powder, placing in a tube furnace filled with inert atmosphere, preserving heat for 2 hours at 450 ℃ at a heating rate of 2 ℃/min, and cooling to room temperature to obtain the CS-CSS/NHC heterogeneous nanocube.
As shown in fig. 1 and 2, the heterogeneous nanocubes are ZIF-67-derived N-doped carbon anchored CoSe 2 –CoSe 0.25 S 1.75 Heterogeneous polyhedral particles of CoSe 2 And CoSe 0.25 S 1.75 The heterogeneous interface of atomic level contact has a polyhedron size of about 300nm, a rough surface and a hierarchical porous structure, and is composed of a large number of small primary spherical particles.
Example 2
Step 1, weighing 11g of 2-methylimidazole, adding the 2-methylimidazole into 20ml of deionized water, and magnetically stirring for 10min to obtain a uniformly dispersed transparent solution A;
step 2, weighing 0.9g of cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into 6ml of deionized water, and magnetically stirring the mixture for 10 minutes to obtain uniformly dispersed red solution B;
step 3, rapidly mixing the two solutions under the condition of stirring to form a purple mixed solution, magnetically stirring for 10min, and then aging for 24h at room temperature to obtain a mixed solution with purple precipitation;
step 4, after the room temperature aging is finished, obtaining a purple product through centrifugation, alternately cleaning and collecting the product through water/methanol for 2-3 times, and then drying the product for 24 hours at the temperature of 60 ℃ in a vacuum drying oven to obtain a ZIF-67 precursor;
and 5, weighing 500mg of precursor ZIF-67, 1000mg of selenium powder and 1000mg of sulfur powder, placing in a tube furnace filled with inert atmosphere, preserving heat for 2 hours at 450 ℃ at a heating rate of 2 ℃/min, and cooling to room temperature to obtain the CS-CSS/NHC heterogeneous nanocube.
Example 3
Step 1, weighing 11g of 2-methylimidazole, adding the 2-methylimidazole into 20ml of deionized water, and magnetically stirring for 10min to obtain a uniformly dispersed transparent solution A;
step 2, weighing 0.9g of cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into 6ml of deionized water, and magnetically stirring the mixture for 10 minutes to obtain uniformly dispersed red solution B;
step 3, rapidly mixing the two solutions under the condition of stirring to form a purple mixed solution, magnetically stirring for 10min, and then aging for 24h at room temperature to obtain a mixed solution with purple precipitation;
step 4, after the room temperature aging is finished, obtaining a purple product through centrifugation, alternately cleaning and collecting the product through water/methanol for 2-3 times, and then drying the product for 24 hours at the temperature of 60 ℃ in a vacuum drying oven to obtain a ZIF-67 precursor;
and 5, weighing 500mg of precursor ZIF-67, 500mg of selenium powder and 500mg of sulfur powder, placing in a tube furnace filled with inert atmosphere, preserving heat for 2 hours at 450 ℃ at a heating rate of 2 ℃/min, and cooling to room temperature to obtain the CS-CSS/NHC heterogeneous nanocube.
Claims (10)
- The preparation method of the CS-CSS/NHC heterogeneous nanocube is characterized by comprising the steps of specifically taking 2-methylimidazole as an organic framework, cobalt nitrate hexahydrate as a cobalt source, water as a solvent, and synthesizing a ZIF-67 precursor by a room temperature coprecipitation method; and then selenium powder/sulfur powder is used as a selenium source and a sulfur source, and finally the preparation of the CS-CSS/NHC heterogeneous nanocubes is realized by a one-step method.
- 2. The method for preparing the CS-CSS/NHC heterogeneous nanocube according to claim 1, which is characterized by comprising the following steps:step 1, weighing 2-methylimidazole, and then adding the 2-methylimidazole into deionized water for magnetic stirring to obtain a uniformly dispersed transparent solution A;step 2, weighing cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into deionized water, and magnetically stirring to obtain uniformly dispersed red solution B;step 3, rapidly mixing the two solutions under the condition of stirring to form a purple mixed solution, magnetically stirring, and then aging at room temperature to obtain a mixed solution with purple precipitate;step 4, after the room-temperature aging is finished, obtaining a purple product through centrifugation, then cleaning and collecting the product, and then drying to obtain a ZIF-67 precursor;and 5, weighing a certain amount of precursors ZIF-67, selenium powder and sulfur powder, placing the precursors ZIF-67, selenium powder and sulfur powder in a tube furnace filled with inert atmosphere for reaction, and cooling to room temperature to obtain the CS-CSS/NHC heterogeneous nanocubes.
- 3. The method for preparing a CS-CSs/NHC heterogeneous nanocube according to claim 2, wherein step 1 specifically comprises: 7.3 to 14.7g of 2-methylimidazole is weighed and added into 13 to 26ml of deionized water, and the magnetic stirring time is 2 to 10 minutes.
- 4. The method for preparing a CS-CSs/NHC heterogeneous nanocube according to claim 2, wherein step 2 specifically comprises: weighing 0.6-1.2 g of cobalt nitrate hexahydrate, adding the cobalt nitrate hexahydrate into 4-8 ml of deionized water, and magnetically stirring for 2-10 min.
- 5. The method for preparing the CS-CSS/NHC heterogeneous nanocube according to claim 2, wherein in the step 3, the magnetic stirring is performed for 10-30 min, and the aging is performed for 24h.
- 6. The method for preparing the CS-CSs/NHC heterogeneous nanocubes according to claim 2, wherein in step 4, the washing process is to collect the product by 2-3 times of water/methanol alternate washing, and the drying process is to dry for 12-24 hours at 60-80 ℃ in a vacuum drying oven.
- 7. The preparation method of the CS-CSS/NHC heterogeneous nanocube according to claim 2, wherein the mass ratio of the precursors ZIF-67, selenium powder and sulfur powder in the step 5 is 1: (1-2): (1-2).
- 8. The method for preparing the CS-CSs/NHC heterogeneous nanocubes according to claim 2, wherein the reaction conditions in the tube furnace in step 5 are: the temperature is kept for 2 hours at the temperature of 300-450 ℃ at the heating rate of 2 ℃/min.
- 9. The method for preparing the CS-CSS/NHC heterogeneous nanocube according to claim 2, wherein in step 5, air in a quartz glass tube is removed before the tube furnace starts to heat up, the precursor ZIF-67 and selenium powder are mixed and ground and placed at the downstream of the tube furnace, and sulfur powder is placed at the upstream of the tube furnace.
- Application of CS-CSS/NHC heterogeneous nanocubes in the field of lithium-sulfur battery anode hosts or photo/electrocatalysis.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117486264A (en) * | 2023-12-29 | 2024-02-02 | 洛阳理工学院 | Carbon nano-sheet loaded cobalt-based heterojunction material and preparation method and application thereof |
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| CN117486264A (en) * | 2023-12-29 | 2024-02-02 | 洛阳理工学院 | Carbon nano-sheet loaded cobalt-based heterojunction material and preparation method and application thereof |
| CN117486264B (en) * | 2023-12-29 | 2024-04-02 | 洛阳理工学院 | Carbon nano-sheet loaded cobalt-based heterojunction material and preparation method and application thereof |
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