CN114334472B - NiS (nickel-zinc sulfide) 2 /Ti 3 C 2 MXene super capacitor composite material, preparation method and application - Google Patents
NiS (nickel-zinc sulfide) 2 /Ti 3 C 2 MXene super capacitor composite material, preparation method and application Download PDFInfo
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a NiS 2 /Ti 3 C 2 MXene super capacitor composite material, a preparation method and application thereof, and belongs to the technical field of capacitor composite materials. The invention successfully synthesizes the NiS by combining coprecipitation with in-situ vulcanization 2 /Ti 3 C 2 MXene, niS in the resulting composite 2 The nano particles are uniformly distributed in the lamellar Ti 3 C 2 Surface of MXene. In one aspect of the invention, ti of two-dimensional layered structure 3 C 2 MXene can inhibit NiS 2 Aggregation and volume change of the nano particles, and improves the conductivity of the composite material; on the other hand, niS 2 Nanoparticles can also inhibit Ti 3 C 2 The 'self-stacking' of the MXene and the synergistic effect of the two improve the specific capacity and the rate capability of the composite material.
Description
Technical Field
The invention relates to a NiS 2 /Ti 3 C 2 MXene super capacitor composite material, a preparation method and application thereof, and belongs to the technical field of capacitor composite materials.
Background
Along with exhaustion of fossil fuel and aggravation of environmental pollution caused by overuse of people, development of clean energy and efficient energy storage technology have become effective strategies for sustainable development in the current era. Electrochemical energy storage devices are one of the energy storage technologies available to address the global energy crisis, with batteries and supercapacitors being the two main energy storage devices. This limits their development because of the potential safety hazards of batteries that can generate heat and dendrite formation when they are operated at high power. Super capacitor has received extensive attention as an electrochemical energy storage device because of its high power density, fast charge and discharge speed, safe operation and good cycling stability.
Among various electrode materials, transition metal sulfides are promising electrode materials for supercapacitors due to their large theoretical capacity, good conductivity, and low cost. Wherein nickel disulfide (NiS 2 ) The multi-electron transfer can provide rich electrochemical redox sites, and has higher theoretical specific capacity. But adopts NiS 2 The prepared electrode material is easy to expand in volume in the charge and discharge process, so that the cycle stability and the rate capability are poor. NiS is subjected to 2 Compounding with graphene, porous carbon material, conductive polymer and other conductive matrix can effectively inhibit adjacent NiS 2 Aggregation to slow down the volume change in the charge and discharge process and further promote NiS 2 Is used for the electrochemical performance of the battery. Thus, a novel conductive matrix material and NiS are sought 2 Compounding remains a challenge.
MXenes are an emerging class of two-dimensional transition metal carbides, nitrides and carbonitrides, have the characteristics of high conductivity of graphene and hydrophilicity of graphene oxide, and have a unique two-dimensional layered structure, and show great potential in the aspect of application of super capacitor electrode materials as a conductive matrix. However, because of the two-dimensional layered structure of MXene, which is easily "self-stacking", fewer active sites are provided to participate in chemical reactions, resulting in lower mass specific capacity.
Disclosure of Invention
The present invention addresses the above problems by providing a NiS 2 /Ti 3 C 2 MXene super capacitor composite material, and a preparation method and application thereof. The invention successfully synthesizes the NiS by combining coprecipitation with in-situ vulcanization 2 /Ti 3 C 2 MXene, niS in the resulting composite 2 The nano particles are uniformly distributed in the lamellar Ti 3 C 2 Surface of MXene. On the one hand, two-dimensional layersTi of a shape structure 3 C 2 MXene can inhibit NiS 2 Aggregation and volume change of the nano particles, and improves the conductivity of the composite material; on the other hand, niS 2 Nanoparticles can also inhibit Ti 3 C 2 The 'self-stacking' of the MXene and the synergistic effect of the two improve the specific capacity and the rate capability of the composite material.
NiS (nickel-zinc sulfide) 2 /Ti 3 C 2 The preparation method of the MXene super capacitor composite material comprises the following steps:
(1) By titanium carbide (Ti) 3 AlC 2 ) Preparing two-dimensional layered Ti as raw material through etching, washing and centrifuging 3 C 2 An MXene solution;
preferably, ti 3 C 2 The concentration of the MXene solution was 0.25 mg/mL.
(2) Nickel nitrate hexahydrate (Ni (NO 3 ） 2 ·6H 2 O), hexamethylenetetramine (C) 6 H 12 N 4 ) Sodium citrate dihydrate (Na 3 C 6 H 5 O 7 ·2H 2 O) dispersing the Ti obtained in the step (1) 3 C 2 Stirring uniformly in MXene solution, washing, centrifuging, and collecting precipitate;
preferably, the mass ratio of the nickel nitrate hexahydrate to the sodium tetramine to the sodium citrate dihydrate is as follows: 233:140:29; the sodium citrate dihydrate and Ti 3 C 2 The mass volume ratio of the MXene solution is 29:40, mg/mL.
(3) Under the protection of inert gas, placing the mixture prepared in the step (2) and sublimated sulfur into two porcelain boats, respectively placing the porcelain boats at the middle and upstream positions of a high-temperature furnace, and calcining to obtain NiS 2 /Ti 3 C 2 The MXene composite material has a calcination rate of 1 ℃/min, a calcination temperature of 300-500 ℃ and a calcination time of 2-5 h;
preferably, the mass ratio of the mixture prepared in the step (2) to the sublimated sulfur is 1:10; the calcination temperature was 300 ℃ and the calcination time was 3 h.
Further, ti in the step (1) 3 C 2 The preparation method of the MXene solution comprises the following steps:
(1) adding lithium fluoride (LiF) into a polytetrafluoroethylene lining filled with hydrochloric acid solution with the concentration of 6mol/L, and uniformly stirring;
preferably, the mass volume ratio of the lithium fluoride to the hydrochloric acid solution is as follows: 1:20 g/ml, stirring time is 1 h;
(2) slowly adding titanium carbonate into the step (1), putting the mixed solution into a constant-temperature water bath kettle with the temperature of 40 ℃, and stirring for reaction 24 h;
preferably, the mass ratio of the titanium carbon aluminate to the lithium fluoride is 1:2;
(3) centrifuging the solution obtained in the step (2) at 3500 rpm for 10 min, pouring out supernatant, performing ultrasonic treatment for 10 min, repeating the operation for 4-7 times until the pH of the solution is approximately equal to 6, and collecting precipitate; dispersing the precipitate in water, ultrasonic treating under inert gas protection for 1h, centrifuging at 3500 rpm for 1h, and collecting upper layer dark green solution to obtain Ti 3 C 2 MXene solution.
The invention also comprises the NiS obtained by the preparation method 2 /Ti 3 C 2 MXene supercapacitor composite material and NiS 2 /Ti 3 C 2 Application of MXene super capacitor composite material in preparation of super capacitor.
Compared with the prior art, the invention has the following advantages:
1. the composite material and the simple NiS 2 Compared with the super capacitor material, the defect of reduced specific capacity in the charging and discharging process under high current density is overcome.
2. The invention adopts Ti with two-dimensional lamellar structure 3 C 2 MXene has higher conductivity and good hydrophilic property compared with the traditional carbon-based material, and effectively increases the conductivity with NiS 2 Contact area between the two.
3. The invention provides a NiS 2 /Ti 3 C 2 Preparation method of MXene super capacitor composite material, and Ti with two-dimensional layered structure 3 C 2 MXene can inhibit NiS 2 Agglomeration of nanoparticles, and NiS 2 Nanoparticles can also inhibit Ti 3 C 2 The 'self-stacking' of the MXene and the synergistic effect of the two improve the specific capacity and the rate capability of the composite material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is an XRD pattern for example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of example 2 of the present invention;
FIG. 3 is a scanning electron microscope image of example 3 of the present invention;
FIG. 4 is a NiS of example 3 of the present invention 2 Monomer cyclic voltammogram and constant current charge-discharge curve and NiS 2 /Ti 3 C 2 The MXene composite material cyclic voltammetry curve graph and the constant current charge-discharge curve graph;
FIG. 5 is a NiS obtained in example 3 of the present invention 2 /Ti 3 C 2 MXene composite material and NiS 2 Electrochemical performance of the monomers is compared.
Detailed Description
The invention will be further described with reference to specific embodiments, and advantages and features of the invention will become apparent from the description. The embodiments are merely exemplary and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
Example 1: niS (NiS) 2 /Ti 3 C 2 MXene super capacitor composite material and preparation method and application thereof
（1）Ti 3 C 2 Synthesis of MXene
2g of lithium fluoride are added to 10 g of a 40 ml hydrochloric acid solution having a concentration of 6mol/LStir 1h in a 0 ml polytetrafluoroethylene liner. After dissolution, the 1 g carbon titanium aluminate was slowly added thereto, and the mixture was placed in a 40 ℃ thermostatic water bath with stirring for 24 h. Then, the resulting solution was centrifuged at 3500 rpm for 10 min, the supernatant was removed, sonicated for 10 min, and then the operation was repeated 6 times until the solution pH was approximately equal to 6, and the precipitate was collected. Dispersing the precipitate in 80 ml water, ultrasonic treating under inert gas for 1h, centrifuging at 3500 rpm for 1h, and collecting upper layer dark green solution to obtain Ti 3 C 2 MXene solution at a concentration of 0.25 mg/ml.
（2）NiS 2 /Ti 3 C 2 Synthesis of MXene composite
At 90℃to disperse 233 mg of nickel nitrate hexahydrate, 140 mg of hexamethylenetetramine and 29 mg of sodium citrate dihydrate in 40 ml of Ti obtained in step (1) 3 C 2 In the MXene solution, stirring 6 h, then washing for a plurality of times, and centrifuging to obtain a precipitate. In an inert gas N 2 Under the protection, placing the prepared 0.05 g mixture and 0.5 g sublimed sulfur in two porcelain boats, respectively placing the porcelain boats at the middle and upstream positions of a high temperature furnace, heating to 300 ℃ at a calcination rate of 1 ℃/min, preserving heat for 2 hours, and cooling the sample to room temperature to obtain NiS 2 /Ti 3 C 2 MXene composites.
The NiS obtained in this example 2 /Ti 3 C 2 The XRD diffraction pattern of the MXene composite is shown in FIG. 1.
（3）NiS 2 /Ti 3 C 2 Preparation of MXene composite material super capacitor
The NiS obtained in the step (2) is processed 2 /Ti 3 C 2 The MXene composite material comprises the following active substances: acetylene black: mixing polyvinylidene fluoride=8:1:1, adding N-methyl pyrrolidone, stirring to obtain paste, and coating on 1×1.5. 1.5 cm 2 And drying the foam nickel sheet to prepare the supercapacitor electrode. 3 mol/L KOH is used as electrolyte, a mercury-mercury oxide electrode is used as a reference electrode, a platinum sheet is used as a counter electrode, three-electrode electrochemical test is carried out, and test items comprise cyclic voltammogramsTesting, constant current charge and discharge testing and alternating current impedance testing.
Example 2: niS (NiS) 2 /Ti 3 C 2 MXene super capacitor composite material and preparation method and application thereof
（1）Ti 3 C 2 Synthesis of MXene
The procedure is as in example 1.
（2）NiS 2 /Ti 3 C 2 Synthesis of MXene composite
At 90℃to disperse 233 mg of nickel nitrate hexahydrate, 140 mg of hexamethylenetetramine and 29 mg of sodium citrate dihydrate in 40 ml of Ti obtained in step (1) 3 C 2 In the MXene solution, stirring 6 h, then washing for a plurality of times, and centrifuging to obtain a precipitate. In an inert gas N 2 Under the protection, placing the prepared 0.05 g mixture and 0.5 g sublimed sulfur in two porcelain boats, respectively placing the porcelain boats at the middle and upstream positions of a high temperature furnace, heating to 350 ℃ at a calcination rate of 1 ℃/min, preserving heat for 3 hours, and cooling the sample to room temperature to obtain the NiS 2 /Ti 3 C 2 MXene composites.
The NiS obtained in this example 2 /Ti 3 C 2 A transmission electron microscope picture of the MXene composite is shown in fig. 2.
（3）NiS 2 /Ti 3 C 2 Preparation of MXene composite material super capacitor
The NiS obtained in the step (2) is processed 2 /Ti 3 C 2 The MXene composite material comprises the following active substances: acetylene black: mixing polyvinylidene fluoride=8:1:1, adding N-methyl pyrrolidone, stirring to obtain paste, and coating on 1×1.5. 1.5 cm 2 And drying the foam nickel sheet to prepare the supercapacitor electrode. And (3) performing three-electrode electrochemical tests by using 3 mol/L KOH as electrolyte, a mercury-mercury oxide electrode as a reference electrode and a platinum sheet as a counter electrode, wherein the test items comprise cyclic voltammetry curve tests, constant-current charge and discharge tests and alternating-current impedance tests.
Example 3: niS (NiS) 2 /Ti 3 C 2 MXene composite material and preparation method and application thereof
（1）Ti 3 C 2 Synthesis of MXene
The synthesis procedure was as in example 1.
（2）NiS 2 /Ti 3 C 2 Synthesis of MXene composite
At 90℃to disperse 233 mg of nickel nitrate hexahydrate, 140 mg of hexamethylenetetramine and 29 mg of sodium citrate dihydrate in 40 ml of Ti obtained in step (1) 3 C 2 In the MXene solution, stirring 6 h, then washing for a plurality of times, and centrifuging to obtain a precipitate. In an inert gas N 2 Under the protection, placing the prepared 0.05 g mixture and 0.5 g sublimed sulfur in two porcelain boats, respectively placing the porcelain boats at the middle and upstream positions of a high temperature furnace, heating to 400 ℃ at a calcination rate of 1 ℃/min, preserving heat for 3 hours, and cooling the sample to room temperature to obtain the NiS 2 /Ti 3 C 2 MXene composites.
The NiS obtained in this example 2 /Ti 3 C 2 A scanning electron microscope picture of the MXene composite is shown in fig. 3.
（3）NiS 2 /Ti 3 C 2 Preparation of MXene composite material super capacitor
The NiS obtained in the step (2) is processed 2 /Ti 3 C 2 The MXene composite material comprises the following active substances: acetylene black: mixing polyvinylidene fluoride=8:1:1, adding N-methyl pyrrolidone, stirring to obtain paste, and coating on 1×1.5. 1.5 cm 2 And drying the foam nickel sheet to prepare the supercapacitor electrode. And (3) performing three-electrode electrochemical tests by using 3 mol/L KOH as electrolyte, a mercury-mercury oxide electrode as a reference electrode and a platinum sheet as a counter electrode, wherein the test items comprise cyclic voltammetry curve tests, constant-current charge and discharge tests and alternating-current impedance tests.
Test example:
the NiS prepared by the invention 2 /Ti 3 C 2 The MXene composite material is further prepared into a super capacitor, and is subjected to three-electrode electrochemical test, the test results are shown in fig. 4 and 5, and as can be seen from fig. 4a and 5c, along with the increase of the scanning speed, the whole cycle is photovoltaicThe area of the safety curve is increased and the symmetry is good; as can be seen from fig. 4b and d, the symmetry of the charge-discharge plateau of the curve is still good with increasing current density, indicating that the prepared material has higher coulombic efficiency. From FIG. 5a at 5 mV s -1 As can be seen from a comparison of cyclic voltammograms at the scan rate of (C) 2 /Ti 3 C 2 The area of the cyclic voltammogram of the MXene composite material is obviously increased, and the oxidation-reduction peak is more prominent, so that the composite material has larger specific capacitance; from FIG. 5b at 1A g -1 As can be seen from the comparison of the constant current charge and discharge graphs under the current density of (2), niS 2 /Ti 3 C 2 The specific capacity of the MXene composite material is 580C g -1 Whereas NiS 2 Has a specific capacity of 455C g -1 This is because of Ti 3 C 2 MXene tablet loaded NiS 2 After the particles, the active sites of oxidation-reduction reaction are added, so that the electrochemical performance is finally improved; as is evident from the graph of the multiplying power performance of FIG. 5c, the composite material has a higher multiplying power than the specific capacity of the monomer under the same current density, and as is evident from the graph of the alternating current impedance of FIG. 5d, the NiS 2 /Ti 3 C 2 The MXene composite material has a larger linear slope in a low frequency range, which indicates that the ion diffusion is faster, and the NiS is in a high frequency range 2 /Ti 3 C 2 The smaller radius of curvature of the MXene composite indicates that the composite has less resistance to charge transfer, which also demonstrates the improved electrochemical performance of the composite. In conclusion, niS 2 /Ti 3 C 2 The performance of the super capacitor made of the MXene composite material is superior to that of NiS 2 Monomer and has obvious lifting effect.
Claims (9)
1. NiS (nickel-zinc sulfide) 2 /Ti 3 C 2 The preparation method of the MXene super capacitor composite material is characterized in that the preparation method synthesizes the NiS by combining coprecipitation and in-situ vulcanization 2 /Ti 3 C 2 MXene, niS in the resulting composite 2 The nano particles are uniformly distributed in the lamellar Ti 3 C 2 The surface of MXene;
the method comprises the following steps:
(1) By titanium carbide (Ti) 3 AlC 2 ) Preparing two-dimensional layered Ti as raw material through etching, washing and centrifuging 3 C 2 An MXene solution;
(2) Nickel nitrate hexahydrate (Ni (NO 3 ） 2 ·6H 2 O), hexamethylenetetramine (C) 6 H 12 N 4 ) Sodium citrate dihydrate (Na 3 C 6 H 5 O 7 ·2H 2 O) dispersing the Ti obtained in the step (1) 3 C 2 Stirring uniformly in MXene solution, washing, centrifuging, and collecting precipitate;
(3) Under the protection of inert gas, placing the mixture prepared in the step (2) and sublimated sulfur into two porcelain boats, respectively placing the porcelain boats at the middle and upstream positions of a high-temperature furnace, and calcining to obtain NiS 2 /Ti 3 C 2 The calcining speed of the MXene composite material is 1 ℃/min, the calcining temperature is 300-500 ℃, and the calcining time is 2-5 h.
2. The method according to claim 1, wherein Ti in the step (1) 3 C 2 The concentration of the MXene solution was 0.25 mg/mL.
3. The preparation method according to claim 1, wherein the mass ratio of nickel nitrate hexahydrate, hexamethylenetetramine and sodium citrate dihydrate in the step (2) is: 233:140:29; the sodium citrate dihydrate and Ti 3 C 2 The mass volume ratio of the MXene solution is 29:40, mg/mL.
4. The method according to claim 1, wherein the mass ratio of the mixture prepared in the step (2) to the sublimed sulfur in the step (3) is 1:10; the calcination temperature was 300 ℃ and the calcination time was 3 h.
5. According to the weightsThe process according to claim 1, wherein Ti in the step (1) 3 C 2 The preparation method of the MXene solution comprises the following steps:
(1) adding lithium fluoride (LiF) into a polytetrafluoroethylene lining filled with hydrochloric acid solution with the concentration of 6mol/L, and uniformly stirring;
(2) slowly adding titanium carbonate into the step (1), putting the mixed solution into a constant-temperature water bath kettle with the temperature of 40 ℃, and stirring for reaction 24 h;
(3) centrifuging the solution obtained in the step (2) at 3500 rpm for 10 min, pouring out supernatant, performing ultrasonic treatment for 10 min, repeating the operation for 4-7 times until the pH of the solution is approximately equal to 6, and collecting precipitate; dispersing the precipitate in water, performing ultrasonic treatment under inert gas for 1 hr, centrifuging at 3500 rpm for 1h, and collecting upper layer dark green solution to obtain Ti 3 C 2 MXene solution.
6. The method according to claim 5, wherein the mass-to-volume ratio of the lithium fluoride to the hydrochloric acid solution in the step (1) is: 1:20 g/ml, stirring time 1 h.
7. The method according to claim 5, wherein the mass ratio of titanium carbonitride to lithium fluoride in the step (2) is 1:2.
8. NiS obtained by the process of any one of claims 1 to 7 2 /Ti 3 C 2 MXene supercapacitor composites.
9. The NiS as claimed in claim 8 2 /Ti 3 C 2 Application of MXene super capacitor composite material in preparation of super capacitor.
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Citations (4)
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| CN106571244A (en) * | 2016-11-02 | 2017-04-19 | 南京工业大学 | Two-dimensional transition metal carbon (nitrogen) compound and two-dimensional transition metal sulfide nano-composite powder, and preparation and application thereof |
| CN108832097A (en) * | 2018-06-13 | 2018-11-16 | 东华大学 | A kind of curing nickel carbon nano-composite material and its preparation method and application |
| CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
| CN112054199A (en) * | 2020-09-02 | 2020-12-08 | 山东大学 | MoS for high-performance potassium ion battery2/Ti3C2Preparation method of MXene composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106571244A (en) * | 2016-11-02 | 2017-04-19 | 南京工业大学 | Two-dimensional transition metal carbon (nitrogen) compound and two-dimensional transition metal sulfide nano-composite powder, and preparation and application thereof |
| CN108832097A (en) * | 2018-06-13 | 2018-11-16 | 东华大学 | A kind of curing nickel carbon nano-composite material and its preparation method and application |
| CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
| CN112054199A (en) * | 2020-09-02 | 2020-12-08 | 山东大学 | MoS for high-performance potassium ion battery2/Ti3C2Preparation method of MXene composite material |
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