CN111755262A - CoS/Ti applied to super capacitor3C2Preparation method of (1) - Google Patents
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- 238000000034 method Methods 0.000 title abstract description 8
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 58
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 20
- 238000004108 freeze drying Methods 0.000 claims abstract description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 14
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims abstract description 13
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 11
- 239000003990 capacitor Substances 0.000 claims abstract description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 9
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000010335 hydrothermal treatment Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 239000007772 electrode material Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 15
- 239000012621 metal-organic framework Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012921 cobalt-based metal-organic framework Substances 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- -1 transition metal sulfide Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
- Y02E60/13—Energy storage using capacitors
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- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Materials Engineering (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
CoS/Ti applied to super capacitor3C2The method belongs to the technical field of electrode materials, and accordion-shaped Ti is prepared by the method3C2Dispersing in water, adding cobalt nitrate and polyvinylpyrrolidone, performing ultrasonic treatment, adding methanol solution containing dimethyl imidazole during stirring, reacting, centrifuging, and freeze drying to obtain ZIF-67/Ti3C2. Dispersing the dried product in ethanol water solution for ultrasonic treatment, adding Thioacetamide (TAA) for hydrothermal reaction to obtain CoS/Ti3C2. The preparation method provided by the invention is simple and reliable, and the prepared material has controllable structure and better electrochemistryAnd (4) performance.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to CoS/Ti3C2The preparation method and the application research in the aspect of the super capacitor.
Background
Supercapacitors are a special energy storage system with excellent cycling performance and can combine high energy density with high power density into an ideal energy storage device. The electrode material is used as an important component of the super capacitor, and the performance of the super capacitor is directly determined by the performance of the electrode material. Transition Metal Sulfide (TMS) is introduced into supercapacitors as a common active material to enhance performance because it can provide a large number of redox sites in electrochemical reactions. However, the transition metal sulfide itself is a semiconductor material with poor conductivity, and needs to be compounded with a substrate with strong conductivity to improve the conductivity. Among them, CoS has excellent electrochemical properties and is widely concerned, Wan et al prepare CoS nanorods by hydrothermal method and show higher specific capacity (h.wan et al, Journal of Power sources.2013,06,027.), but CoS particles inevitably agglomerate during long-time charge and discharge and finally cause particle pulverization. The two-dimensional material can provide a large number of active sites in electrochemical reaction, and shortens an electrolyte ion transmission path, thereby improving the electrochemical performance. But two-dimensional CoS is difficult to obtain with precision. The metal organic framework compound (MOFs) is composed of metal clusters and organic ligands, has high specific surface area and porous controllable surface property, and can accurately obtain two-dimensional CoS by properly treating the metal organic framework compound (MOFs) as a precursor, for example, Hu et al use cobalt-based MOFs as a precursor, and the prepared hollow nano-box with the outer layer composed of CoS nano-sheets shows better electrochemical performance (Hu et al, Chem 1, 102-113.). However, two-dimensional CoS still faces poor conductivity during the reaction such that it develops polarization during long cycling and decreases cycling stability. Therefore, compounding with a more conductive substrate can effectively alleviate problems caused by poor conductivity of CoS，Ti3C2Since 2011, the titanium-based metal oxide has been stripped from aluminum-based MAX, the titanium-based metal oxide has attracted much attention due to excellent performance of the aluminum-based MAX3C2The electrode material has the following remarkable advantages: 1) the two-dimensional structure endows the ion/electron transmission path with shorter length; 2) the electron transmission rate is accelerated due to the strong conductivity; 3) abundant surface functional groups, e.g., -O, -F, -OH, to make Ti3C2Has better hydrophilicity, and is easy to disperse in aqueous solution to form a uniform composite structure (Y.F. Dong et al, adv.Funct.Mater.2020, 2000706.). However, MOFs are often combined with other substrates in organic solvent systems, such as Ramachandran et al, in which Co-MOF is directly combined on nickel foam in N, N-Dimethylformamide (DMF) (r. Ramachandran et al, ceramics international.2018.05.055.), while Ti3C2 in pure organic systems cannot exert the advantages of its two-dimensional structure and large surface area rich functional groups due to poor dispersibility. Thus, how to prepare MOF/Ti in aqueous systems3C2And preparing CoS/Ti based thereon3C2Has important practical significance.
Disclosure of Invention
CoS/Ti applied to super capacitor3C2The preparation method is simple and reliable, and the prepared material has good electrochemical performance.
In order to achieve the technical purpose, the invention adopts the technical scheme that:
CoS/Ti applied to super capacitor3C2The method comprises subjecting accordion-like Ti3C2Dispersing in water, adding cobalt nitrate, polyvinylpyrrolidone (PVP) and methanol, performing ultrasonic treatment, adding methanol solution containing dimethyl imidazole during stirring, reacting, centrifuging, and freeze drying to obtain ZIF-67/Ti3C2. Dispersing the dried product in ethanol water solution for ultrasonic treatment, adding Thioacetamide (TAA) for hydrothermal reaction to obtain CoS/Ti3C2. The method comprises the following specific steps:
the first step is as follows: preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 30-40 deg.C for 48-72h, adding deionized water, centrifuging to neutrality, and precipitating to obtain accordion-shaped Ti3C2Filtered and dried.
The second step is that: preparation of ZIF-67/Ti3C2
2.1) mixing polyvinylpyrrolidone (PVP) with accordion-like Ti3C2Dispersing in deionized water according to the mass ratio of 32:1-10:1, wherein 190-608mg of PVP is added in each 30-120mL of deionized water.
2.2) adding cobalt nitrate and methanol solution, wherein, in the step 2.1), 15mL of methanol solution is added into every 30-120mL of deionized water. And (4) after ultrasonic treatment for 40-60min, stirring for 8-24h, and then ultrasonic treatment for 20 min. Wherein, methanol solution containing dimethyl imidazole is added in the stirring process to react for 10-30 min. The mass ratio of the dimethyl imidazole to the cobalt nitrate is 1:1-3: 1; the dimethylimidazole and Ti3C2The mass ratio of (A) to (B) is 26:1-10: 1.
2.3) adding deionized water, centrifuging, and freeze-drying with a freeze dryer to obtain ZIF-67/Ti3C2. The freeze drying time is 12 h.
The third step: preparation of CoS/Ti3C2
Dispersing the product obtained in the second step into ethanol water, adding Thioacetamide (TAA) after ultrasonic treatment, and carrying out hydrothermal treatment at the temperature of 120-150 ℃ for 8-24 h. Obtaining CoS/Ti3C2. The ZIF-67/Ti3C2The mass ratio of the compound to the TAA is 1:1-1: 3; the volume ratio of ethanol to water in the ethanol water solution is 1: 1.
The material prepared by the method is used for manufacturing a negative electrode of a super capacitor.
The invention has the beneficial effects that: 1) the preparation method is simple, and the structure is controllable; 2) using accordion-like Ti3C2The carrier can simplify the preparation process and reduce the energy consumption; 3) ti can be used in combination in an aqueous system3C2The excellent dispersibility in water is beneficial to the uniform composition with MOF; 4) has the advantages ofThe electrochemical performance of (2).
Drawings
FIG. 1 is CoS/Ti of example 13C2SEM image of (d).
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
1) Preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 30 deg.C for 72h, adding deionized water, centrifuging to neutrality, and collecting the precipitate as accordion-shaped Ti3C2Filtered and dried.
2) Preparation of ZIF-67/Ti3C2Taking 19mg of accordion-shaped Ti3C2And 608mg of polyvinylpyrrolidone were dispersed in 120mL of water, and 220mg of cobalt nitrate and 15mL of methanol solution were added. And (4) after ultrasonic treatment for 60min, stirring for 24h, and then ultrasonic treatment for 20 min. While stirring, 15mL of a methanol solution containing 493mg of dimethylimidazole was added, and the reaction was carried out for 10 min.
3) Adding deionized water, centrifuging, and freeze drying with FD-1A-50 freeze dryer to obtain ZIF-67/Ti3C2. The freeze drying time is 12 h.
4) Preparation of CoS/Ti3C2
40mg of the above product was dispersed in a mixed solution of 15mL of ethanol and 15mL of water, sonicated, 80mg of TAA was added, and hydrothermal treatment was carried out at 150 ℃ for 12 hours. Obtaining CoS/Ti3C2。
1Ag in a three electrode test System in 6M KOH solution-1Under the condition of constant current, the specific capacitance is 832F g-1. FIG. 1 is an SEM image of CoS/Ti3C2 of example 1, from which the CoS/Ti produced can be seen3C2Presenting a two-dimensional sheet-like structure.
Example 2
1) Preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 35 deg.C for 48h, adding deionized water, centrifuging to neutrality, and precipitating to obtain accordion-shaped Ti3C2Filtered and dried.
2) Taking 19mg of accordion-shaped Ti3C2And 190mg of polyvinylpyrrolidone in 100mL of water, 190mg of cobalt nitrate and 15mL of methanol solution were added. And after ultrasonic treatment for 40min, stirring for 8h, and then ultrasonic treatment for 20 min. While stirring, 15mL of a methanol solution containing 190mg of dimethylimidazole was added, and the reaction was carried out for 30 min.
3) Adding deionized water, centrifuging, and freeze drying with freeze dryer to obtain ZIF-67/Ti3C2. The freeze drying time is 12 h.
4) 40mg of the above product was dispersed in a mixed solution of 15mL of ethanol and 15mL of water, sonicated, 120mg of TAA was added, and hydrothermal treatment was carried out at 150 ℃ for 8 hours. Obtaining CoS/Ti3C2。
In a three-electrode test system with 6M KOH solution, 1A g-1Under constant current condition, the specific capacitance is 605F g-1。
Example 3
1) Preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 35 deg.C for 54h, adding deionized water, centrifuging to neutrality, and precipitating to obtain accordion-shaped Ti3C2Filtered and dried.
2) Taking 19mg of accordion-shaped Ti3C2And 304mg of polyvinylpyrrolidone in 60mL of water, 95mg of cobalt nitrate and 15mL of methanol solution were added. And (4) after 50min of ultrasonic treatment, stirring for 12h, and then performing ultrasonic treatment for 20 min. While stirring, 15mL of a methanol solution containing 285mg of dimethylimidazole was added, and the reaction was carried out for 20 min.
3) Adding deionized water, centrifuging, and freeze drying with freeze dryer to obtain ZIF-67/Ti3C2. When the freeze-drying is performedFor 12 h.
4) 40mg of the above product was dispersed in a mixed solution of 15mL of ethanol and 15mL of water, and after sonication, 40mg of TAA was added and the mixture was heated at 130 ℃ for 12 hours. Obtaining CoS/Ti3C2。
In a three-electrode test system with 6M KOH solution, 1A g-1Under the condition of constant current, the specific capacitance is 587F g-1。
Example 4
1) Preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 30 deg.C for 72h, adding deionized water, centrifuging to neutrality, and collecting the precipitate as accordion-shaped Ti3C2Filtered and dried.
2) Taking 19mg of accordion-shaped Ti3C2And 380mg of polyvinylpyrrolidone in 30mL of water, 127mg of cobalt nitrate and 15mL of methanol solution were added. And (4) after 50min of ultrasonic treatment, stirring for 12h, and then performing ultrasonic treatment for 20 min. While stirring, 15mL of a methanol solution containing 380mg of dimethylimidazole was added, and the reaction was carried out for 20 min.
3) Adding deionized water, centrifuging, and freeze drying with freeze dryer to obtain ZIF-67/Ti3C2. The freeze drying time is 12 h.
4) 40mg of the above product was dispersed in a mixed solution of 15mL of ethanol and 15mL of water, and after sonication, 40mg of TAA was added and the mixture was heated at 120 ℃ for 16 hours. Obtaining CoS/Ti3C2。
In a three-electrode test system with 6M KOH solution, 1A g-1Under constant current condition, the specific capacitance is 553F g-1。
Example 5
1) Preparation of accordion-like Ti3C2
Mixing Ti3AlC2Slowly add to 9M HCl containing LiF, wherein 1g Ti is added to each 20mL HCl3AlC2And 1g LiF. Stirring at 30 deg.C for 72h, adding deionized water, centrifuging to neutrality, and precipitating to obtain accordionForm Ti3C2Filtered and dried.
2) Taking 19mg of accordion-shaped Ti3C2And 380mg of polyvinylpyrrolidone were dispersed in 120mL of water, and 249mg of cobalt nitrate and 15mL of methanol were added. And (4) after 50min of ultrasonic treatment, stirring for 24h, and then performing ultrasonic treatment for 20 min. While stirring, 15mL of methanol containing 328mg of dimethylimidazole was added and the reaction was carried out for 10 min.
3) Adding deionized water, centrifuging, and freeze drying with freeze dryer to obtain ZIF-67/Ti3C2. The freeze drying time is 12 h.
4) 40mg of the above product was dispersed in a mixed solution of 15mL of ethanol and 15mL of water, sonicated, 80mg of TAA was added, and the mixture was heated at 120 ℃ for 16 hours. Obtaining CoS/Ti3C2。
In a three-electrode test system with 6M KOH solution, 1A g-1Under constant current conditions, the specific capacitance is 790F g-1。
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (4)
1. CoS/Ti applied to super capacitor3C2The preparation method is characterized by comprising the following steps:
the first step is as follows: preparation of accordion-like Ti3C2
The second step is that: preparation of ZIF-67/Ti3C2
2.1) mixing polyvinylpyrrolidone PVP with accordion-like Ti3C2Dispersing in deionized water according to the mass ratio of 32:1-10:1, wherein 190-608mg of PVP is added in every 30-120mL of deionized water;
2.2) adding cobalt nitrate and a methanol solution, wherein in the step 2.1), 15mL of the methanol solution is added into every 30-120mL of deionized water; performing ultrasonic treatment for 40-60min, stirring for 8-24h, and performing ultrasonic treatment for 20 min; wherein, in the stirring processAdding methanol solution containing dimethyl imidazole, and reacting for 10-30 min; the mass ratio of the dimethyl imidazole to the cobalt nitrate is 1:1-3: 1; the dimethylimidazole and Ti3C2The mass ratio of (A) to (B) is 26:1-10: 1;
2.3) adding deionized water, centrifuging, and freeze-drying with a freeze dryer to obtain ZIF-67/Ti3C2；
The third step: preparation of CoS/Ti3C2
Dispersing the product obtained in the second step into ethanol water, adding thioacetamide TAA after ultrasonic treatment, and carrying out hydrothermal treatment at the temperature of 120-150 ℃ for 8-24h to obtain CoS/Ti3C2(ii) a The ZIF-67/Ti3C2The mass ratio of the compound to the TAA is 1:1-1: 3.
2. CoS/Ti applied to supercapacitor according to claim 13C2Characterized in that, in the first step, accordion-like Ti is prepared3C2The preparation process comprises the following steps: mixing Ti3AlC2Adding 9M HCl containing LiF, wherein 1g of Ti is added into each 20mL of HCl3AlC2And 1g LiF; stirring at 30-40 deg.C for 48-72h, adding deionized water, centrifuging to neutrality, and precipitating to obtain accordion-shaped Ti3C2Filtering, and drying to obtain accordion-shaped Ti3C2。
3. CoS/Ti applied to supercapacitor according to claim 13C2The preparation method is characterized in that the volume ratio of ethanol to water in the ethanol aqueous solution in the third step is 1: 1.
4. CoS/Ti applied to super capacitor3C2Characterized in that the CoS/Ti3C2The preparation method is used for preparing the cathode of the super capacitor, and the cathode is prepared by the preparation method of any one of claims 1 to 3.
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Cited By (2)
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| CN115064391A (en) * | 2022-05-25 | 2022-09-16 | 电子科技大学长三角研究院(湖州) | Preparation method of electrode material applied to asymmetric supercapacitor |
| CN115672291A (en) * | 2022-11-04 | 2023-02-03 | 大连佳纯气体净化技术开发有限公司 | Flake NiCo-MOFs/Ti 3 C 2 T x Material, method for the production thereof and use thereof |
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| CN115672291B (en) * | 2022-11-04 | 2023-12-26 | 大连佳纯气体净化技术开发有限公司 | Flake NiCo-MOFs/Ti 3 C 2 T x Material, preparation method and application thereof |
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