CN114999836A - Sandwich-like CoNi 2 S 4 /Ti 3 C 2 Preparation method and application of MXene heterojunction composite material - Google Patents
Sandwich-like CoNi 2 S 4 /Ti 3 C 2 Preparation method and application of MXene heterojunction composite material Download PDFInfo
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- 239000002994 raw material Substances 0.000 claims abstract description 5
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- 239000000843 powder Substances 0.000 claims description 7
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
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- 229910052979 sodium sulfide Inorganic materials 0.000 claims 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
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- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 229940048181 sodium sulfide nonahydrate Drugs 0.000 description 1
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 150000003623 transition metal compounds Chemical class 0.000 description 1
- -1 transition metal sulfide Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
Abstract
The invention discloses sandwich-like CoNi 2 S 4 /Ti 3 C 2 A preparation method and application of an MXene heterojunction composite material belong to the field of nano materials and super capacitors. The invention adopts a simple one-step hydrothermal method, takes cobalt salt, nickel salt, sulfur salt and the like as raw materials, takes water as a solvent, reacts in a high-pressure kettle at a temperature of between 180 and 220 ℃ for 10 to 14 hours, and prepares the CoNi successfully after washing and drying 2 S 4 The nano-sheet grows on Ti uniformly 3 C 2 MXene surface and interlaminar composite. Interlayer CoNi is inhibited by the layered structure of MXene 2 S 4 The overgrowth of the nanosheets makes the nanosheets very small in size, which not only shortens the electron transfer and ion diffusion paths, but also enables CoNi 2 S 4 The volume change of the nano-sheet in the electrochemical process is minimized, and the cycle of the nano-sheet is improvedRing stability. And thanks to the special configuration of the sandwich, CoNi 2 S 4 The volume expansion in the electrochemical cycle is effectively alleviated. Furthermore, CoNi 2 S 4 With Ti 3 C 2 MXene not only improves single CoNi through stronger interface combination and good electronic coupling effect 2 S 4 Is also optimized for OH ‑ The stability and the adsorptivity on the surface of the electrode greatly improve the activity of electrochemical reaction. The heterojunction composite material shows excellent electrochemical performance when used as a supercapacitor electrode, and the maximum specific mass capacity of the heterojunction composite material can reach 2398F g –1 The recycling time can reach 4 thousands of times, and the application prospect is very good.
Description
Technical Field
The invention relates to sandwich-like CoNi 2 S 4 /Ti 3 C 2 A preparation method and application of an MXene heterojunction composite material belong to the field of nano materials and super capacitors.
Background
In recent years, with the development of science and technology and society, fossil fuels such as coal and petroleum are continuously consumed and become in short supply, and the environmental pollution caused by the combustion of the fossil fuels is more and more serious. Energy shortage and environmental pollution become major problems in human survival and development today. The development and research of renewable green energy is the key to solving the problem, and the related efficient, safe and reliable energy storage device is unprecedentedly developed. Among them, the super capacitor can collect energy in a very short time and then release energy as required, and has a very long cycle life and a wide range of use temperature, and is more and more favored by researchers. The super capacitor is developed to present day, the biggest challenge is to lower energy density, and the electrode material is the core component of the super capacitor and is the key factor for determining the electrochemical performance of the super capacitor, so that the search for the electrode material with excellent electrochemical performance is very important.
At present, electrode materials of the battery type, e.g. CoNi 2 O 4 ，NiCo 2 O 4 ，CoMoO 4 ，CoNi 2 S 4 And the multi-element transition metal compounds are widely concerned due to abundant active sites and high theoretical specific capacity. Among these compounds, the transition metal sulfide CoNi 2 S 4 Due to its lower optical forbidden band gap, higher conductivity and moreThe redox active sites thus achieve higher specific capacitance and are becoming more and more appreciated by researchers. However, the single sulfide is easy to agglomerate when in use, so that the effective specific surface area and the active sites for electrochemical reaction are reduced, and higher specific capacity is difficult to achieve; in addition, although the multi-transition metal sulfide is highly conductive among many metal compounds, it is still lower than the carbon-based material, which also reduces its reactivity. To solve this problem, various regulation and optimization strategies have been proposed in succession, such as designing unique nanostructures or doping heterogeneous elements. These methods do play a certain role in improving electrochemical performance, but the requirements of actual production and life cannot be met no matter the capacity or the cycling stability is compared. Particularly, the cycle life of the capacitor is generally less than 10000 cycles at present.
The heterojunction is constructed, particularly the sandwich-like two-dimensional heterojunction can overcome the defects of a single material, combines the advantages of two or more materials, and develops the advantages and avoids the disadvantages, so that the electrode material with excellent electrochemical performance is obtained. Research shows that after the heterostructure is constructed, atoms at the interface can interact to cause the change of an interface electronic structure, so that the electronic structure is regulated, and the electrochemical reaction activity of the electrode material is activated or optimized. In addition, the sandwich-type heterogeneous layered structure can reduce the ionic movement resistance and accelerate diffusion by increasing the distance between layers, thereby obtaining higher energy density. More importantly, by using a two-dimensional heterostructure expansion and contraction of the electrode material can be minimized or eliminated, thereby improving cycle life. So far, many common CoNi 2 S 4 Base heterojunctions such as CoNi 2 S 4 Graphene (J.alloys Compd.845(2020)156164), NiCo 2 S 4 [ CoNi-LDH (chem. Eng. J.383(2020)123206) and CoNi 2 S 4 /Co 3 O 4 (Electrochimica Acta 412(2022)140139) and the like have been successfully synthesized and applied to supercapacitors for improving their energy storage capacity. However, based on CoNi 2 S 4 The sandwich type two-dimensional heterojunction of (2) is rarely reported. This is mainly due to the lack of effectivenessAssembly strategies, not all materials can be easily assembled together. Recently, the accordion-like MXene material has shown outstanding advantages in constructing two-dimensional heterojunction. The structure has a layered structure, and the interlayer spacing is adjustable, so that a space is provided for the growth of heterogeneous active materials. In addition, the MXene surface has abundant surface functional groups and good hydrophilicity, and can provide attachment sites for the growth of nano materials. It also has excellent electrical conductivity and good mechanical properties. Importantly, many electrode materials expand in volume upon ionic intercalation, whereas Ti 3 C 2 T x The MXene electrode undergoes volume shrinkage during ion intercalation, which provides possibility for designing electrode materials with volume expansion close to zero. Therefore, the two materials are compounded to construct the sandwich type two-dimensional heterojunction, and the electrode material with comprehensive excellent electrochemical performance can be obtained.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the single electrode material in the prior art and provide sandwich-like CoNi 2 S 4 /Ti 3 C 2 Preparation method of MXene heterojunction composite material by using CoNi 2 S 4 Can be dispersedly grown on the surface and the interlayer of MXene, improves the integral electrochemical performance of the composite material and is applied to a super capacitor.
The technical scheme adopted by the invention is as follows:
(1) selecting nickel nitrate hexahydrate and cobalt nitrate hexahydrate as reaction raw materials, weighing and dispersing the raw materials in 75mL of deionized water according to a molar ratio of 2:1, adding hexamethylenetetramine, performing magnetic stirring until a transparent light pink solution is formed, and then adding Ti 3 C 2 MXene powder and a sulfur source form a black suspension;
(2) transferring the suspension into a reaction kettle, putting the reaction kettle into an oven, heating to 220 ℃ at 180 ℃, and preserving heat for 10-14 h. Naturally cooling to room temperature after the reaction is finished, washing and drying to obtain CoNi 2 S 4 /Ti 3 C 2 MXene composite material.
The invention has the advantages and beneficial effects that:
1. the invention adopts a one-step hydrothermal method to prepare CoNi 2 S 4 /Ti 3 C 2 The MXene heterojunction composite material has the advantages of simple operation, high yield, low cost and no pollution.
2. CoNi prepared by the invention 2 S 4 /Ti 3 C 2 In the MXene heterojunction composite material, CoNi 2 S 4 The nano-sheet is uniformly dispersed and grown on the MXene surface and among the MXene layers, has a unique sandwich structure, is not separately separated from the MXene surface and the MXene layers, and has CoNi 2 S 4 The nanoplatelets also did not significantly agglomerate. In addition, the layered structure of MXene suppresses interlayer CoNi 2 S 4 The overgrowth of the nanosheets makes the nanosheets very small in size, which not only shortens the electron transfer and ion diffusion paths, but also makes the CoNi 2 S 4 The volume change of the nano-sheet in the electrochemical process reaches the minimum, and the cycling stability of the nano-sheet is improved.
3. CoNi prepared by the invention 2 S 4 /Ti 3 C 2 In the MXene heterojunction composite material, CoNi 2 S 4 With Ti 3 C 2 MXene has stronger interface bonding force and good electronic coupling effect, which not only improves single CoNi 2 S 4 Is also optimized for OH - The stability and the adsorptivity on the surface of the electrode greatly improve the activity of electrochemical reaction.
4. CoNi prepared by the invention 2 S 4 /Ti 3 C 2 When the MXene heterojunction composite material is used as a super capacitor electrode material, the MXene heterojunction composite material has ultrahigh specific capacity and excellent cycling stability. When the current density is 1A/g, the specific capacity can reach 2398F/g; when the current is increased to 25A/g, the specific capacity can still reach 1042F/g; after 40000 times of charging and discharging cycles at a current density of 25A/g, the specific capacitance can be maintained to be more than 80% of the initial specific capacitance of the electrode material.
The invention is further described with reference to the following figures and examples.
Drawings
FIG. 1 is CoNi prepared 2 S 4 /Ti 3 C 2 X-ray diffraction (XRD) patterns of MXene heterojunction composite materials as well as single materials;
FIG. 2 is CoNi produced 2 S 4 /Ti 3 C 2 Scanning Electron Microscope (SEM) photographs of MXene heterojunction composites;
FIG. 3 is CoNi prepared 2 S 4 /Ti 3 C 2 Constant current charge and discharge data of the MXene heterojunction composite material. The left panel is sequentially 1A g at current density -1 ，2A g -1 ，3A g -1 ，5A g -1 ，10A g -1 ，15A g -1 ，20A g -1 ，25A g -1 Under the condition, measuring a charge-discharge curve, wherein Time/s is charge-discharge Time, and Potential (V vs. Hg/HgO) is the voltage corresponding to the charge-discharge of the reference electrode Hg/HgO; the right graph shows the capacitance at different current densities calculated from the charge and discharge curves.
FIG. 4 shows CoNi prepared 2 S 4 /Ti 3 C 2 And (3) constant-current charge-discharge long-Cycle test data of the MXene heterojunction composite material, wherein Cycle number is Cycle number, and Specific capacitance is Specific capacity.
Detailed Description
Example 1
(1) 2g of Ti 3 AlC 2 The block was added to 30mL of hydrofluoric acid stock solution and reacted until no bubbles were generated. Then the obtained Ti 3 C 2 The powder was washed with deionized water and filtered with suction until the pH of the solution obtained by suction filtration was about 6. Cleaning the filtered Ti 3 C 2 Drying the powder at 60 ℃.
(2) 0.5671g of nickel nitrate hexahydrate, 0.2838g of cobalt nitrate hexahydrate and 0.1682g of hexamethylenetetramine are weighed and dispersed in 75mL of deionized water for magnetic stirring until a transparent light pink solution is formed; then adding 200mg of the multilayer Ti obtained in the step (1) 3 C 2 MXene powder, stirring to form dispersion liquid; 1.8014g of sodium sulfide nonahydrate are added into the dispersion liquid, and a black suspension is formed by stirring; the suspension was transferred to a 100mL stainless steel reaction kettle, placed in an oven and heated to 200 ℃ and held for 12 h. Knot to be reactedThen naturally cooling to room temperature, washing and drying to obtain CoNi 2 S 4 /Ti 3 C 2 MXene composite material.
(3) CoNi obtained as above 2 S 4 /Ti 3 C 2 The MXene composite material is subjected to XRD characterization. The results showed (FIG. 1) that the diffraction peaks of XRD were all derived from Ti 3 C 2 MXene and CoNi 2 S 4 In which Ti 3 C 2 The small angle deviation of the (0002) peak position of MXene shows that the interlayer distance is large, which shows that CoNi is introduced into MXene interlayer 2 S 4 . SEM characterization results showed (FIG. 2), at Ti 3 C 2 MXene surface and interlayer uniformly grow CoNi 2 S 4 Nanosheets, no apparent individual agglomerated CoNi was found 2 S 4 And (3) a block body. The composite material is used for a supercapacitor electrode material to carry out constant current charge-discharge test, and the result shows that when the current density is 1A/g, the specific capacity can reach 2398F/g; when the current is increased to 25A/g, the specific capacity can still reach 1042F/g (figure 3). After 40000 cycles of charge and discharge at a current density of 25A/g, the specific capacitance remained 80% or more of the initial specific capacitance of the electrode material (FIG. 4).
Example 2:
this embodiment is different from embodiment 1 in that,
and (3) adjusting the heat preservation time to 10h when the water is heated at the temperature of 200 ℃ in the step (2). The obtained product is used for a constant current charge-discharge test of the electrode material of the super capacitor, and the result shows that when the current density is 2A/g, the specific capacity can reach 1708F/g; when the current is increased to 25A/g, the specific capacity can still reach 640F/g.
Claims (7)
1. Sandwich-like CoNi 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized by comprising the following steps of:
(1) selecting nickel nitrate hexahydrate and cobalt nitrate hexahydrate as reaction raw materials, weighing and dispersing the raw materials in 75mL of deionized water according to a molar ratio of 2:1, adding hexamethylenetetramine, and performing magnetic stirringStirring until a transparent light pink solution is formed, and then adding Ti 3 C 2 MXene powder and a sulfur source form a black suspension;
(2) and transferring the suspension into a reaction kettle, putting the reaction kettle into an oven, heating to a certain temperature, and keeping the temperature for a certain time. Naturally cooling to room temperature after the reaction is finished, washing and drying to obtain CoNi 2 S 4 /Ti 3 C 2 MXene heterojunction composite materials.
2. Sandwich-like CoNi according to claim 1 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized in that the nickel nitrate hexahydrate and Ti in the step (1) 3 C 2 The mass ratio of MXene powder is 2-3.5: 1.
3. sandwich-like CoNi according to claim 1 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized in that the Ti in the step (1) 3 C 2 Etching Ti from MXene powder by HF 3 AlC 2 Preparation, HCl/LiF etch of Ti 3 AlC 2 Preparation or high-temperature molten-salt etching of Ti 3 AlC 2 The preparation can be carried out.
4. Sandwich-like CoNi according to claim 1 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized in that the sulfur source in the step (1) is one or more of sodium sulfide, thiourea and other sulfur-containing substances.
5. Sandwich-like CoNi according to claim 1 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized in that in the step (2), an oven is adopted for hydrothermal treatment, and the hydrothermal treatment temperature is 180-220 ℃.
6. Sandwich-like CoNi according to claim 1 2 S 4 /Ti 3 C 2 The preparation method of the MXene heterojunction composite material is characterized in that in the step (2), a drying oven is adopted for hydrothermal treatment, and the hydrothermal treatment time is 10-14 h.
7. CoNi obtained by the preparation method of claim 1 2 S 4 /Ti 3 C 2 Use of an MXene heterojunction composite in a supercapacitor.
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| CN115888780B (en) * | 2022-09-30 | 2024-04-26 | 扬州大学 | CuFeS2MXene composite nano material and preparation method thereof |
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