CN111704173A - Ti-C @ CoMn-LDH composite material and preparation method and application thereof - Google Patents
Ti-C @ CoMn-LDH composite material and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title abstract description 30
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 34
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000013049 sediment Substances 0.000 claims abstract description 13
- 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 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 3
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 19
- 239000006229 carbon black Substances 0.000 claims description 14
- -1 polytetrafluoroethylene Polymers 0.000 claims description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- 239000006260 foam Substances 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000012546 transfer Methods 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 5
- 238000009825 accumulation Methods 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 239000002135 nanosheet Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- 239000011149 active material Substances 0.000 description 20
- 238000002484 cyclic voltammetry Methods 0.000 description 20
- 238000010277 constant-current charging Methods 0.000 description 17
- 238000007599 discharging Methods 0.000 description 17
- 239000010936 titanium Substances 0.000 description 16
- 239000007772 electrode material Substances 0.000 description 14
- 238000005119 centrifugation Methods 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 238000000227 grinding Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 10
- 229910021607 Silver chloride Inorganic materials 0.000 description 10
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 10
- 239000008151 electrolyte solution Substances 0.000 description 10
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 238000002604 ultrasonography Methods 0.000 description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VBNIGYNNILMQRE-UHFFFAOYSA-N O.NN.[Se] Chemical compound O.NN.[Se] VBNIGYNNILMQRE-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- 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 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- 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
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- 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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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- 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
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The invention relates to a preparation method of a Ti-C @ CoMn-LDH material, which comprises the following steps: s1: soaking LiF in HCl solution, then adding Ti gradually3AlC2Stirring the powder at constant temperature, centrifugally washing black sediment by using deionized water until the pH value is 6 to obtain Ti3C2TxPowder; s2: mixing Ti3C2TxPowder is in N2Performing ultrasonic treatment under protection, centrifuging, collecting centrifuged solid particles, and drying to obtain e-Ti3C2(ii) a S3: e-Ti3C2、Co(NO3)2·6H2O、Mn(NO3)3·9H2O、NH4And F, adding the solution into water, uniformly dispersing, gradually adding ammonia water, transferring the solution into a reaction kettle to perform hydrothermal reaction, cooling, washing and drying to obtain the Ti-C @ CoMn-LDH material. Compared with the prior art, the Ti-C @ CoMn-LDH composite material prepared by the invention has a unique layered structure, can effectively inhibit the accumulation of two-dimensional nanosheets, provides effective active sites, and can promote the diffusion of electrolytes and the transfer of electrons due to the high porosity of three-dimensional interconnection morphology.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a Ti-C @ CoMn-LDH composite material and a preparation method and application thereof.
Background
The super capacitor has the advantages of high charge and discharge rate, good stability, wide temperature range, long cycle time, environmental friendliness and the like, and has wide application prospect in the field of energy storage. Electrode materials play an important role in the assembly of high performance supercapacitors. Two-dimensional materials (2D) are ideal for supercapacitor electrodes, including Layered Double Hydroxides (LDHs), transition metal carbide/nitride carbonitrides (MXene), graphene, and the like.
The layered structure provides a unique nanoscale reaction space for chemical reactions. The exfoliated two-dimensional nanoplatelets have a large specific surface area and a large number of active sites. The nano-layered material provides a new strategy for improving the performance of the super capacitor. Such as (Ni, Co) Se2The @ NiCo-LDH hybrid reversible capacitor is a flexible asymmetric supercapacitor. The layered material also has many storage advantages, and the feasibility of improving specific capacitance and rate retention is ensured by larger specific surface area, rapid oxidation-reduction reaction and shorter ion transmission distance. However, two-dimensional materials readily form a pi-piSuperposition of van der waals interactions. (1) Interlayer charge transfer is weak due to a large interlayer spacing. Electron transport barriers are not conducive to increasing power and energy density. (2) Due to the tendency to self-pack, a large number of active sites and channels are covered and blocked.
CN 109402662A discloses a preparation method of a molybdenum selenide two-dimensional layered titanium carbide composite material, which comprises the steps of firstly, mixing and stirring Se powder and hydrazine hydrate to obtain a selenium-hydrazine hydrate dispersion liquid; MXene-Ti3C2Mixing the dispersion liquid with cetyl trimethyl ammonium bromide, and adding sodium molybdate to obtain cetyl trimethyl ammonium bromide solution; thirdly, mixing the selenium-hydrazine hydrate dispersion liquid and a cetyl trimethyl ammonium bromide solution for reaction to obtain a mixed solution; fourthly, cleaning the mixed solution by deionized water and ethanol, centrifuging and drying in vacuum to obtain MoSe2@MXene-Ti3C2A composite material. The molybdenum selenide two-dimensional layered titanium carbide composite material in the technical scheme still cannot overcome the defects caused by pi-pi van der Waals interaction.
Disclosure of Invention
The invention aims to solve the problems and provide a Ti-C @ CoMn-LDH composite material and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the Ti-C @ CoMn-LDH material comprises the following steps:
s1: soaking LiF in HCl solution, then adding Ti gradually3AlC2Stirring the powder at constant temperature, centrifugally washing black sediment by using deionized water until the pH value is 6 to obtain Ti3C2Tx(MXene) powder.
S2: mixing Ti3C2TxPowder is in N2Performing ultrasonic treatment and centrifugation under protectionCollecting the centrifuged solid particles, and drying to obtain e-Ti3C2;
S3: e-Ti3C2、Co(NO3)2·6H2O、Mn(NO3)3·9H2O、NH4Adding F into water, dispersing uniformly, gradually adding ammonia water, transferring into a reaction kettle for hydrothermal reaction, cooling, washing and drying to obtain Ti-C @ CoMn-LDH (namely Ti)3C2@ CoMn-LDH) material.
MXene and LDH involved in the invention are both two-dimensional materials.
MXene has good conductivity and abundant surface groups, and the end group has a large number of-F and-OH surfaces with negative charges, so that the electroactive growth can be promoted. However, when MXene is used alone in the present invention, the electrochemical utilization rate and the specific surface area of the electrolyte are reduced by self-stacking of the nanosheets therein.
The CoMn-LDH has a unique layered structure, a large specific surface area and high electrochemical activity, but if the CoMn-LDH is used alone, the effective surface area of charge storage is reduced due to the heavy pressure tendency, the specific capacitance is limited, the interlayer electron transfer is poor, and the electrochemical performance is poor, because the CoMn-LDH material alone shows obvious hole collapse in the electrochemical reaction. The technical scheme is an effective strategy for solving the inherent accumulation defect of the two-dimensional material by constructing the three-dimensional interconnection form and introducing the spacing material.
The Ti-C @ CoMn-LDH mutually connected 3D structure prepared by the invention can slow down self-rearrangement and accelerate the diffusion of ions and the transfer of electrons. The Ti-C @ CoMn-LDH has a unique structure, the precise design of a pore structure is realized by the preparation method, a larger pore volume is obtained, the three-dimensional pore structure can promote the immersion of an electrode and the precipitation of electrolyte, and the volume change of the electrode in the charge and discharge process is reduced, so that the charge transfer is accelerated in specific application, and high energy and power density are realized.
Further, the mass-to-volume ratio of the LiF to the HCl solution in S1 is (1-3) g/(20-50) mL, and the concentration of the HCl solution is (1-3).
Further, the constant-temperature stirring in the S1 is carried out at the temperature of 35-55 ℃ for 18-24 h.
Further, e-Ti in S33C2、Co(NO3)2·6H2O、Mn(NO3)3·9H2O、NH4The molar feed ratio of F is 1-2:1, (0.5-2) to (4-8).
Further, the concentration of the ammonia water in S3 is 1-2mol/L, and the ammonia water and the e-Ti are3C2The volume molar ratio of (15-18) mL: (1-2) mmol.
Further, the temperature of the hydrothermal reaction in S3 is 120-200 ℃, and the reaction time is 4-10 h.
Further, the drying processes in S2 and S3 are vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
The application process of the Ti-C @ CoMn-LDH material prepared by the method in the invention in the working electrode is as follows: grinding the Ti-C @ CoMn-LDH material, uniformly mixing the ground material with carbon black and polytetrafluoroethylene, and then pressing the mixture on a foamed nickel sheet to obtain the working electrode.
Furthermore, the mass ratio of the Ti-C @ CoMn-LDH material to the carbon black to the polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
Compared with the prior art, the invention has the following advantages:
1. ti prepared by the invention3C2The @ CoMn-LDH composite material has a unique layered structure, can effectively inhibit the accumulation of two-dimensional nanosheets, provides effective active sites, and can promote the diffusion of electrolytes and the transfer of electrons due to the high porosity of three-dimensional interconnected morphology.
2. Ti prepared by the invention3C2The @ CoMn-LDH composite material has MXene with good conductivity and abundant surface groups, meanwhile, the LDH also forms a supercapacitor electrode material with high specific capacitance, high conductivity and better cycling stability due to the unique layered structure, larger specific surface area, higher electrochemical activity and adjustable preparation method, the LDH is designed and realized in the invention to decorate the MXene so as to integrate the advantages of the MXene and the electrode material,the high-performance energy storage is realized, an effective way is provided for preparing a high-performance supercapacitor electrode material, the 3D layered structure can effectively inhibit the accumulation of two-dimensional nanosheets, effective active sites are provided, and the high porosity of the three-dimensional interconnection morphology can promote the diffusion of electrolyte and the transfer of electrons.
3. The raw materials adopted by the preparation method are pollution-free, and the solvent generated in the preparation process is non-toxic, so that large-scale industrial popularization can be realized.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the present invention is not limited thereto in any way.
The raw materials used in the examples are commercially available unless otherwise specified.
Example 1
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-1).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-1 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The specific capacitance and the cyclic stability of the material are detected, and cyclic voltammetry tests show that the material has excellent redox capability. The specific capacitance of the electrode material reaches 551F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 2
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.3g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-2).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-2 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The specific capacitance and the cyclic stability of the material are detected, and cyclic voltammetry tests show that the material has excellent redox capability. The specific capacitance of the electrode material reaches 519F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 3
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 45 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-3).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-3 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The specific capacitance and the cyclic stability of the material are detected, and cyclic voltammetry tests show that the material has excellent redox capability. The specific capacitance of the electrode material reaches 488F/g in 2mol/L KOH solution and at the current density of 1A/g.
Example 4
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.12g e-MXene, 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-4).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-4 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material reaches 416F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 5
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder for 24 hours at the constant temperature of 35 DEG CThe black sediment was washed by centrifugation with deionized water to a pH of 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.16g e-MXene, 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-5).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-5 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material of the invention reaches 493F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 6
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 1mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-6).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-6 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material reaches 474F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 7
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 4mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into an autoclave for hydrothermal reaction at the hydrothermal reaction temperature of 1The hydrothermal time is 8h at 80 ℃, the Ti is obtained after cooling to room temperature, washing with deionized water and ethanol and drying for 12h at 60 DEG C3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-7).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-7 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material reaches 449F/g in a 2mol/L KOH solution and at a current density of 1A/g.
Example 8
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 160 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (note)TCCM-8)。
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-8 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material reaches 437F/g in 2mol/L KOH solution and at a current density of 1A/g.
Example 9
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 200 ℃ for 8h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-9).
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-9 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. In 2mol/L KOH solution and under the current density of 1A/g, the specific capacitance of the electrode material reaches 385F/g.
Example 10
Ti3C2The preparation method and the application of the @ CoMn-LDH composite material comprise the following steps:
s1: 0.1g LiF was soaked in 20mL of 9M HCl solution, followed by gradual addition of Ti3AlC2Stirring the powder at the constant temperature of 35 ℃ for 24h, and then centrifugally washing black sediments by deionized water until the pH value is 6. Obtained Ti3C2TxPowder is in N2The ultrasound was repeated under protection and the exfoliated MXene suspension (e-Ti) was collected by centrifugation3C2)。
S2: mixing 0.08g e-MXene and 2mmol Co (NO)3)2·6H2O、2mmol Mn(NO3)3·9H2O and 5mmol of ammonium fluoride are added into 80mL of deionized water and fully and uniformly stirred. Adding 18mL of 1M ammonia water into the mixed solution dropwise, stirring at room temperature for 2h, transferring the mixture into a high-pressure kettle for hydrothermal reaction at 180 ℃ for 10h, cooling to room temperature, washing with deionized water and ethanol, and drying at 60 ℃ for 12h to obtain Ti3C2@ CoMn-LDH composite material. Grinding the active material, and uniformly mixing the ground active material with carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1 to obtain Ti3C2@ CoMn-LDH working electrode (Note TCCM-10)
The Chenghua CHI760e electrochemical workstation adopts cyclic voltammetry and constant current charging and discharging methods, and adopts a three-electrode system: TCCM-10 foam nickel sheet is used as working electrode, Ag/AgCl electrode is used as reference electrode, Pt electrode is used as counter electrode, and 2mol/L KOH is used as electrolyte solution. The CV characteristic and the specific capacitance of the material are detected by cyclic voltammetry and constant current charging and discharging respectively. The specific capacitance of the electrode material reaches 451F/g in 2mol/L KOH solution and at a current density of 1A/g.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a Ti-C @ CoMn-LDH material is characterized by comprising the following steps:
s1: soaking LiF in HCl solution, then adding Ti gradually3AlC2Stirring the powder at constant temperature, centrifugally washing black sediment by using deionized water until the pH value is 6 to obtain Ti3C2TxPowder;
s2: mixing Ti3C2TxPowder is in N2Performing ultrasonic treatment under protection, centrifuging, collecting centrifuged solid particles, and drying to obtain e-Ti3C2;
S3: e-Ti3C2、Co(NO3)2·6H2O、Mn(NO3)3·9H2O、NH4And F, adding the solution into water, uniformly dispersing, gradually adding ammonia water, transferring the solution into a reaction kettle to perform hydrothermal reaction, cooling, washing and drying to obtain the Ti-C @ CoMn-LDH material.
2. The method for preparing a Ti-C @ CoMn-LDH material as claimed in claim 1, wherein the mass-to-volume ratio of the LiF to the HCl solution in S1 is (1-3) g/(20-50) mL, and the concentration of the HCl solution is 9 mol/L.
3. The method for preparing the Ti-C @ CoMn-LDH material as claimed in claim 1, wherein the constant-temperature stirring in S1 is carried out at 35-55 ℃ for 18-24 h.
4. The method for preparing Ti-C @ CoMn-LDH material according to claim 1Characterized in that e-Ti in S33C2、Co(NO3)2·6H2O、Mn(NO3)3·9H2O、NH4The molar feed ratio of F is 1-2:1, (0.5-2) to (4-8).
5. The method for preparing a Ti-C @ CoMn-LDH material as claimed in claim 1, wherein the concentration of ammonia water in S3 is 1-2mol/L, and the ammonia water and e-Ti are3C2The volume molar ratio of (15-18) mL: (1-2) mmol.
6. The method for preparing the Ti-C @ CoMn-LDH material as claimed in claim 1, wherein the hydrothermal reaction temperature in S3 is 120-200 ℃ and the reaction time is 4-10 h.
7. The method for preparing a Ti-C @ CoMn-LDH material as claimed in claim 1, wherein the drying process in S2 and S3 is vacuum drying, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
8. A Ti-C @ CoMn-LDH material obtained by the preparation process of any one of claims 1 to 7.
9. The use of a Ti-C @ CoMn-LDH material as defined in claim 8 in a working electrode, wherein the Ti-C @ CoMn-LDH material is ground, uniformly mixed with carbon black and polytetrafluoroethylene, and then pressed onto a nickel foam sheet to obtain the working electrode.
10. The use of a Ti-C @ CoMn-LDH material as claimed in claim 9, wherein the mass ratio of Ti-C @ CoMn-LDH material to carbon black to polytetrafluoroethylene is 8 (0.8-1.2) to (0.8-1.2).
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