CN115159575B - Preparation method and application of molybdenum disulfide with large interlayer spacing - Google Patents
Preparation method and application of molybdenum disulfide with large interlayer spacing Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 74
- 239000011229 interlayer Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 29
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000005642 Oleic acid Substances 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 239000007774 positive electrode material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000010410 layer Substances 0.000 abstract description 9
- 239000002135 nanosheet Substances 0.000 abstract description 8
- 239000003381 stabilizer Substances 0.000 abstract description 5
- -1 OA small molecule Chemical class 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 3
- 239000011733 molybdenum Substances 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002981 blocking agent Substances 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 8
- 238000007796 conventional method Methods 0.000 description 8
- 229910052725 zinc Inorganic materials 0.000 description 8
- 238000003860 storage Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 150000004668 long chain fatty acids Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
Abstract
The invention discloses a preparation method and application of molybdenum disulfide with large interlayer spacing, and MoO is used 3 TAA is respectively used as a molybdenum source and a sulfur source, OA (oleic acid) is used as a blocking agent and a stabilizer, H 2 Control of MoS with O/EtOH (absolute ethanol) as solvent 2 Directional growth of nanoparticles, urea as a weak reductant to decompose CO during the reaction 2 、NH 3 、H 2 O gas molecules, oleic acid as a capping agent covers the surface of the molybdenum disulfide atomic layer, so that the gas molecules are embedded into MoS 2 Interlayer, promote OA small molecule to be inserted between the layers, so as to make MoS 2 (002) The interlayer spacing is obviously enlarged, and the problem of too small interlayer spacing of the positive electrode material of the zinc ion battery is solved. And secondly, oleic acid can adsorb and passivate the surface of molybdenum disulfide crystals, so that the nano-sheets grow in a directional adhesion mode, and the problem that the two-dimensional nano-sheets are easy to agglomerate is solved.
Description
Technical Field
The invention relates to a preparation method of molybdenum disulfide, in particular to a preparation method and application of molybdenum disulfide with large interlayer spacing.
Background
Compared with a lithium ion battery, the water system rechargeable multivalent metal ion battery has the advantages of low cost, convenience in operation, environment friendliness, high safety and the like. Among them, the aqueous zinc ion battery based on two electron transfer mechanism has been paid attention to in recent years due to the characteristics of large zinc reserves, high theoretical capacity (820 mAh/g), low oxidation-reduction potential (-0.76V vs SHE), good stability in water, etc. However, the development of the current aqueous zinc ion battery is still in a starting stage, such as corrosion dendrites of a zinc cathode, and the energy density of the zinc cathode is always limited due to the problems of limited selection of a cathode material, strong interaction with an electrolyte and the like.
Two-dimensional layered materials are the subject of research by researchers in various countries due to their excellent physicochemical properties. A two-dimensional material is a lamellar material having an atomic-scale thickness, typically bound by covalent bonds in the plane, while the layers are bound by weak molecular bonds. Molybdenum disulfide (MoS) 2 ) One kind of commonThe two-dimensional transition metal sulfide, a potential material of a multifunctional electrode capable of being used for energy storage and conversion, plays an important role as a cathode material in lithium ion and sodium ion batteries. In 2019, H.N.Alshareef team first embeds this inactive material into energy to move by regulation 2 The zinc ion battery is converted into a high-efficiency zinc storage carrier, and is a key electrode material for promoting the development of the zinc ion battery. However, in zinc ion batteries, due to MoS 2 Is smaller in interlayer spacing (0.62 nm), is less hydrophilic, and is theoretically Zn 2+ Can not be embedded between layers, limits reversible deintercalation of zinc ions, and basically has no Zn 2+ Storage capacity. Therefore, there is a need for a method of preparing molybdenum disulfide with a large interlayer spacing.
Disclosure of Invention
The invention provides a preparation method of molybdenum disulfide with large interlayer spacing and application of the molybdenum disulfide as a zinc ion positive electrode material, and solves the problems of poor storage capacity and low coulombic efficiency of a zinc ion battery caused by too small interlayer spacing.
The invention adopts the following technical scheme: preparation method of molybdenum disulfide with large interlayer spacing and MoO 3 Thioacetamide (TAA) is respectively used as a molybdenum source and a sulfur source, and a hydrothermal method is adopted to prepare MoS 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the invention, a weak reducing agent urea and a stabilizer blocking agent oleic acid are added into a hydrothermal reaction system, water absolute ethyl alcohol is used as a composite solvent system, and the mixture is reacted for 12-24 hours in a hydrothermal reaction kettle at 200-220 ℃ to obtain molybdenum disulfide with large interlayer spacing. In the process of synthesizing molybdenum disulfide, urea is taken as CO decomposed by weak reducing agent 2 、NH 3 、H 2 O gas molecules, oleic acid as a capping agent covers the surface of the molybdenum disulfide atomic layer, so that the gas molecules are embedded into MoS 2 Interlayer, promote OA small molecule to be inserted between the layers, and make MoS 2 The interlayer spacing is enlarged; secondly, oleic acid is used as a long-chain fatty acid containing double bonds, can adsorb and passivate the surface of molybdenum disulfide crystals, and the nano-sheets grow in a directional adhesion mode to prevent aggregation of the nano-sheets, so that the generated nano-crystals stably exist in a solvent system.
Utilization rate of oleic acid and crystal phase nucleation growth of molybdenum disulfideThe speeds are mutually coordinated, and excessive oleic acid can cause the inhibition of nucleation growth of molybdenum disulfide crystals, so that a uniform molybdenum disulfide crystal phase structure cannot be obtained. Through experiments, the weak reducing agent urea and MoO 3 The mass ratio of the stabilizer oleic acid to the solvent H is 15:2 2 The volume ratio of O is 1:15,1:6 or 4:15.
As the common knowledge in the art, the stabilizer oleic acid is firstly dispersed in absolute ethanol and then added into the hydrothermal reaction system, so that the dispersion effect of oleic acid in the reaction system can be ensured.
Generally, the MoO 3 And the molar ratio of TAA was 5:1.
The invention also provides application of the molybdenum disulfide prepared by the preparation method as a zinc ion battery anode material. Molybdenum disulfide with large interlayer spacing reduces Zn 2+ Is effective in solving MoS 2 As the problems of slow ion diffusion and unstable material structure of the positive electrode of the zinc ion battery in the charge and discharge process, the specific capacity of the zinc ion battery is greatly improved.
In certain embodiments of the present invention, the following steps are employed:
weighing 200-400mg MoO 3 200-400mg of TAA is dissolved in 10-20ml of deionized water, and the solution is recorded as solution A after ultrasonic treatment for 30 min; 2-3g of urea is dissolved in 10-20mL of deionized water, uniformly stirred and recorded as solution B, the solution B is poured into the solution A, 20-35mL of absolute ethyl alcohol and 4-12mL of OA are added after uniformly stirred, and stirring is continued for 1h; placing the mixture into a reaction kettle for reaction for 12-24 hours at 200 ℃; naturally cooling to room temperature, centrifugally washing, and freeze-drying for later use.
Preferably 287.8mg MoO are weighed 3 300.52mg of TAA is dissolved in 20mL of deionized water, and the solution is obtained by ultrasonic treatment for 30 min; 2.16g of urea is dissolved in 10mL of deionized water, the solution B is stirred uniformly, the solution B is poured into the solution A, 35mL of absolute ethyl alcohol and 8mL of OA (oleic acid) are added after the solution B is stirred uniformly, and the stirring is continued for 1h; placing the mixture into a reaction kettle for reaction for 24 hours at 200 ℃; naturally cooling to room temperature, centrifugally washing, and freeze-drying for later use.
Compared with the prior art, the invention has the beneficial effects that:
(1) Oleic acid is used as end capping agent and stabilizer to decompose CO from urea 2 、NH 3 、H 2 O gas molecules are covered on the surface of the molybdenum disulfide atomic layer, so that the gas molecules are embedded into MoS 2 Interlayer, promote OA small molecule to be inserted between the layers, so as to make MoS 2 The interlayer spacing is enlarged toThe above; secondly, oleic acid serving as a long-chain fatty acid containing double bonds can adsorb and passivate the surface of molybdenum disulfide crystals, and the nano-sheets grow in a directional adhesion mode to prevent aggregation of the nano-sheets, so that the generated nano-crystals exist stably.
(2) Greatly improves the specific discharge capacity of the zinc ion battery, and the specific discharge capacity can reach 201.210mAh g under the current density of 0.1A/g -1 。
Drawings
FIG. 1 is a MoS of a large interlayer spacing molybdenum disulfide of the present invention prepared by a method and application of example one 2 Compared with the conventional MoS prepared by the conventional method 2 An XRD contrast pattern of (b);
FIG. 2 is a MoS of a large interlayer spacing molybdenum disulfide of the present invention prepared in accordance with example one of its application 2 Compared with the conventional MoS prepared by the conventional method 2 SEM contrast profile of (a);
FIG. 3 is a MoS of example two of the preparation method and application of the large-layer-spacing molybdenum disulfide of the present invention 2 Compared with the conventional MoS prepared by the conventional method 2 An XRD contrast pattern of (b);
FIG. 4 is a MoS of example two of the preparation method and application of the large-layer-spacing molybdenum disulfide of the present invention 2 Compared with the conventional MoS prepared by the conventional method 2 At 350-450cm -1 Raman spectrum within the range;
FIG. 5 is a MoS of example two of the preparation method and application of the large-layer-spacing molybdenum disulfide of the present invention 2 Compared with the conventional MoS prepared by the conventional method 2 SEM contrast profile of (a);
FIG. 6 is a schematic illustration of a method for preparing and applying a large interlayer spacing molybdenum disulfide of the present inventionMoS prepared in example two 2 Compared with the conventional MoS prepared by the conventional method 2 The rate capability of the assembled full cell;
FIG. 7 is a MoS of example III of the preparation method and application of the large interlayer spacing molybdenum disulfide of the present invention 2 Compared with the conventional MoS prepared by the conventional method 2 An XRD contrast pattern of (b);
FIG. 8 is a MoS prepared in example III of the preparation method and application of the large interlayer spacing molybdenum disulfide of the present invention 2 Compared with the conventional MoS prepared by the conventional method 2 Is provided for the rate capability of the assembled full cell.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description will refer to the specific implementation, structure, characteristics and effects according to the present invention with reference to the accompanying drawings and preferred embodiments.
The preparation method of the large-layer-spacing molybdenum disulfide and an application implementation case thereof are prepared by adopting the following method:
200mg MoO was weighed 3 200mg of TAA is dissolved in 10ml of deionized water, and the solution is recorded as solution A after ultrasonic treatment for 30 min; dissolving 2g of urea in 10mL of deionized water, uniformly stirring and marking as a solution B, pouring the solution B into the solution A, uniformly stirring, adding 20mL of absolute ethyl alcohol and 4mL of OA, and continuously stirring for 1h; placing the mixture into a reaction kettle for reaction for 12 hours at 200 ℃; naturally cooling to room temperature, centrifugally washing, and freeze-drying for later use.
MoS prepared in this example 2 Named O-MoS 2 The comparative sample used was analytically pure MoS manufactured by Shanghai Ala Biochemical technology Co., ltd 2 。
As shown in FIG. 1, O-MoS 2 The characteristic peaks are consistent with pdf card (37-1492), indicating that MoS was successfully produced 2 . Wherein O-MoS 2 (002) The crystal faces are offset by about 3.966 DEG at a small angle, and the corresponding (002) interplanar spacing is calculated according to Bragg diffraction lawEnlarge to +.>
As shown in FIG. 2, the O-MoS obtained 2 All of which are in the shape of typical buds and are composed of ultrathin nano sheets, and after oleic acid is added, O-MoS 2 The sheet is wrinkled, the sheet layer is obviously thinned, the size is smaller, and the efficient zinc storage performance is realized.
Example two
The preparation method of the large-layer-spacing molybdenum disulfide and an application implementation case thereof are prepared by adopting the following method:
287.8mg MoO were weighed out 3 300.52mg of TAA is dissolved in 20mL of deionized water, and the solution is obtained by ultrasonic treatment for 30 min; 2.16g of urea is dissolved in 10mL of deionized water, the solution B is stirred uniformly, the solution B is poured into the solution A, 35mL of absolute ethyl alcohol and 8mL of OA (oleic acid) are added after the solution B is stirred uniformly, and the stirring is continued for 1h; placing the mixture into a reaction kettle for reaction for 24 hours at 200 ℃; naturally cooling to room temperature, centrifugally washing, and freeze-drying for later use.
MoS prepared in this example 2 Named O-MoS 2 The comparative sample used was analytically pure MoS manufactured by Shanghai Ala Biochemical technology Co., ltd 2 。
As shown in FIG. 3, O-MoS 2 The characteristic peaks are consistent with pdf card (37-1492), indicating that MoS was successfully produced 2 . Wherein O-MoS 2 (002) The crystal faces are offset by about 3.63 degrees at a small angle, and their corresponding interplanar spacings are shifted from the bragg diffraction lawEnlarge to +.>
As shown in FIG. 4, O-MoS 2 And sample MoS 2 At 350-450cm -1 Raman spectrum in the range. For synthetic O-MoS 2 Its peak is widened and, at the same time,the mode exhibits a redshift, and the Mo-S bond bonding force is significantly weakened, mainly due to strong out-of-plane vibrations caused by a decrease in van der waals forces after expansion.
As shown in FIG. 5, the obtained O-MoS 2 All of the zinc-rich film has a typical bud shape and is composed of ultrathin nano sheets, and the sheets are wrinkled after oleic acid is added and connected with each other to form a porous net structure, so that the zinc-rich film is favorable for realizing high-efficiency zinc storage performance.
As shown in FIG. 6, O-MoS 2 And sample MoS 2 All assembled and tested under the same conditions. O-MoS 2 The specific discharge capacity can reach 201.210mAh g under the multiplying power of 0.1A/g -1 . When the current density is restored to 0.1A/g, the current density can be restored to 198.993mAh g -1 The capacity retention rate can reach more than 98 percent. In contrast, the sample MoS 2 Shows no zinc ion storage capacity basically, and the maximum specific discharge capacity at 0.1A/g can only reach 16.97508mAh g -1 。
Example III
The preparation method of the large-layer-spacing molybdenum disulfide and an application implementation case thereof are prepared by adopting the following method:
400mg MoO was weighed 3 400mg of TAA was dissolved in 20ml of deionized water and sonicated for 30min, designated solution A;3g of urea is dissolved in 20mL of deionized water, the solution B is stirred uniformly and recorded as solution B, the solution B is poured into the solution A, 35mL of absolute ethyl alcohol and 12mL of OA are added after the solution B is stirred uniformly, and the stirring is continued for 1h; placing the mixture into a reaction kettle for reaction for 24 hours at 200 ℃; naturally cooling to room temperature, centrifugally washing, and freeze-drying for later use.
MoS prepared in this example 2 Named O-MoS 2 The comparative sample used was analytically pure MoS manufactured by Shanghai Ala Biochemical technology Co., ltd 2 。
As shown in FIG. 7, O-MoS 2 The characteristic peaks are consistent with pdf card (37-1492), indicating that MoS was successfully produced 2 . Wherein O-MoS 2 (002) The crystal face is slightly offset by aboutIts corresponding (002) interplanar spacing is from +.>Enlarge to +.>
As shown in FIG. 8, O-MoS 2 And sample MoS 2 All assembled and tested under the same conditions. O-MoS 2 The specific discharge capacity can reach 290.1066mAh g under the multiplying power of 0.1A/g -1 But the rate performance is poor. In contrast, the sample MoS 2 Shows no zinc ion storage capacity basically, and the maximum specific discharge capacity at 0.1A/g can only reach 16.97508mAh g -1 。
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (2)
1. The preparation method of the molybdenum disulfide with large interlayer spacing is characterized by comprising the following steps:
the method comprises the following steps:
200mg MoO was weighed 3 200mg of thioacetamide is dissolved in 10ml of deionized water, and the solution is recorded as solution A after ultrasonic treatment for 30 min; 2g of urea is dissolved in 10ml of deionized water, the solution B is stirred uniformly and recorded as solution B, the solution B is poured into the solution A, 20ml of absolute ethyl alcohol and 4mL oleic acid are added after the solution B is stirred uniformly, and stirring is continued for 1h; placing the mixture in a reaction kettle for reaction at 200 ℃ for 12h; naturally cooling to room temperature, centrifugally washing, freeze drying to obtain interlayerMolybdenum disulfide from 9.96 a;
the second method is as follows:
287.8mg MoO were weighed out 3 300.52mg thioacetamide is dissolved in 20mL of deionized water and is subjected to ultrasonic treatment for 30min to obtain solution A;2.16 Dissolving urea in 10mL deionized water, stirring uniformly to obtain solution B, pouring the solution B into the solution A, stirring uniformly, adding 35mL absolute ethyl alcohol and 8mL oleic acid, and continuing stirring for 1h; placing the mixture in a reaction kettle for reaction at 200 ℃ for 24h; naturally cooling to room temperature, centrifugally washing, and freeze-drying to obtain molybdenum disulfide with an interlayer spacing of 9.85A;
and a third method:
400mg MoO was weighed 3 400mg of thioacetamide is dissolved in 20ml of deionized water, and the solution is recorded as solution A after ultrasonic treatment for 30 min; 3g of urea is dissolved in 20ml of deionized water, the solution B is stirred uniformly and recorded as solution B, the solution B is poured into the solution A, 35ml of absolute ethyl alcohol and 12mL oleic acid are added after the solution B is stirred uniformly, and stirring is continued for 1h; placing the mixture in a reaction kettle for reaction at 200 ℃ for 24h; naturally cooling to room temperature, centrifugally washing, and freeze-drying to obtain the molybdenum disulfide with the interlayer spacing of 10.05A.
2. The application of the molybdenum disulfide prepared by the preparation method of claim 1 as a positive electrode material of a zinc ion battery.
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| CN103915630A (en) * | 2014-04-28 | 2014-07-09 | 华东理工大学 | Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof |
| CN111099658A (en) * | 2020-01-07 | 2020-05-05 | 南开大学 | Preparation method of molybdenum disulfide nano material with different interlayer spacings |
| CN111847514A (en) * | 2020-07-27 | 2020-10-30 | 吉林大学 | Metal phase molybdenum disulfide, self-supporting electrode, preparation method and application |
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| CN103915630A (en) * | 2014-04-28 | 2014-07-09 | 华东理工大学 | Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof |
| CN111099658A (en) * | 2020-01-07 | 2020-05-05 | 南开大学 | Preparation method of molybdenum disulfide nano material with different interlayer spacings |
| CN111847514A (en) * | 2020-07-27 | 2020-10-30 | 吉林大学 | Metal phase molybdenum disulfide, self-supporting electrode, preparation method and application |
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