CN114464786A - Electrode material of potassium ion battery and preparation method and application thereof - Google Patents
Electrode material of potassium ion battery and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a potassium ion battery electrode material and a preparation method and application thereof, wherein the electrode material has the following structural general formula: Y-S NiS2@ C, wherein C denotes the carbon shell, NiS2Denotes NiS2The compound, Y-S, represents a core-shell structure having a bell shape. The preparation method comprises the following steps: coating NiS with 2-methylimidazolium zinc salt ZIF-82Nanoparticles to give ZIF-8 coated NiS2Composite NiS2@ ZIF-8; etching NiS with tannic acid2@ ZIF-8 to obtain a Bell-shaped complex Y-S NiS with internal voids2@ ZIF-8; in the atmosphere of sulfur vapor, Y-S NiS2@ ZIF-8 annealing carbonization picklingRemoving zinc sulfide to obtain Y-S NiS2The @ C composite material is an electrode material of the potassium ion battery, and the electrode material is used in the potassium ion battery and shows excellent rate performance.
Description
Technical Field
The invention belongs to the field of potassium ion batteries, and particularly relates to a potassium ion battery electrode material, and a preparation method and application thereof.
Background
In potassium ion batteries, nickel-based sulfide NiS2It is widely used in negative electrode materials due to its moderate cost and high theoretical capacity. However, its poor electrical conductivity and large volume change result in poor electrical storage performance. Structure of the deviceNanostructured NiS2And compounded with a highly conductive carbon material (carbon nanotube, graphene, hard carbon, etc.) is an effective method for solving the above problems.
Xu et al reported a 3D flower-like NiS for potassium ion storage2It maintained a high capacity of 433 mA h g-1 after 100 cycles at 0.2A g-1, higher than tubular and spherical NiS2(Energy Storage Materials 34 (2021) 536-) -544. However, during the long-term intercalation and deintercalation of potassium ions, the nano-structured negative electrode material may generate structural collapse due to a large change in volume, thereby resulting in poor cycle stability and rate performance.
Aiming at the problems in the prior art, the invention designs a bell-shaped carbon-based NiS2Composite material, and a novel preparation method is adopted to obtain a bell-shaped structure, and NiS is added2Wrapping the nanospheres in the ZIF-8, corroding the interior of the ZIF-8 by using tannic acid, reserving an outer shell layer, and directly obtaining the composite material with the rattle-shaped structure containing the internal gaps after carbonization. The method is simple in material and convenient to operate, and the size of the internal gap is changed along with the change of the amount of the coated ZIF-8, so that the method is very simple and useful. The material with the bell-shaped structure is used as a secondary battery cathode material, so that the volume change caused by ion embedding and releasing can be buffered, and the battery cycle performance and the rate capability of the material are effectively improved.
Disclosure of Invention
The invention aims to provide a potassium ion battery electrode material, a preparation method and application thereof, aiming at the problems in the prior art.
The technical scheme of the invention is as follows:
a potassium ion battery electrode material, which has the following structural formula: Y-S NiS2@ C, wherein C denotes the carbon shell, NiS2Denotes NiS2The compound, Y-S, represents a core-shell structure having a bell-shape.
The electrode material has a primary microstructure unit and a secondary microstructure feature.
The primary microstructure unit comprises the following characteristics:
the shell layer is a hollow ball carbon shell, and NiS is coated inside the hollow carbon shell2(ii) a The hollow ball carbon shell and NiS2Hollow gaps are reserved between the two.
The NiS2Is nano-particles with the particle size of 100-150 nm;
the volume of the hollow sphere carbon shell layer is NiS2The volume of the nano particles is more than 1.5 times, and more preferably 1.5-3 times;
the shape of the carbon shell layer of the hollow sphere is a hollow sphere-like body, and the hollow sphere-like body comprises one or more of a hollow ellipsoid, a hollow sphere, a hollow ovoid and a hollow olive;
the inner layer and the outer layer of the hollow sphere carbon shell have porous structures;
the hollow sphere carbon shell layer is composed of carbon;
s and N atoms are doped on carbon atoms of the carbon shell layer of the hollow sphere; s, N are uniformly distributed in and on the surface of the carbon shell.
The shape of the nano particles is curved spherical particles.
The secondary microstructure is characterized in that hollow sphere carbon shell layers are gathered in a close-packed mode.
The NiS2The content by mass of the composite material is 30 to 70wt%, and more preferably 52.4 wt%.
The invention provides a potassium ion battery electrode material applied to a potassium ion battery.
The invention provides a secondary battery containing a potassium ion battery electrode material, which comprises a potassium ion battery, wherein the potassium ion battery comprises a positive electrode, a negative electrode and electrolyte; the negative electrode includes: a current collector and a negative electrode material supported on the current collector; wherein the negative electrode material contains the electrode material.
The invention provides a preparation method of a potassium ion battery electrode material, which comprises the following steps: 1. coating NiS with 2-methylimidazolium zinc salt (ZIF-8)2The nanoparticles being ZIF-8 encapsulatedNiS2Compound (NiS)2@ZIF-8)；
2. Partial etching of NiS with tannic acid2@ ZIF-8 gives a Bell-shaped complex (Y-S NiS) having voids inside2@ZIF-8）；
3. In the atmosphere of sulfur vapor, Y-S NiS2@ ZIF-8 annealing carbonization, pickling to remove zinc sulfide to obtain Y-S NiS2The @ C composite material is the electrode material of the potassium ion battery.
Optionally, step 1 comprises: mixing NiS2The dispersion of nanoparticles was homogeneously dispersed to zinc salt Zn (NO)3)2Adding the methanol solution of dimethyl imidazole, fully reacting, filtering, washing and drying to obtain NiS wrapped by ZIF-82Compound (NiS)2@ZIF-8)。
Optionally, said NiS2The particle size of the nano-particles is 100-150nm, and the zinc salt is one or more of zinc nitrate, zinc chloride and zinc sulfate;
optionally, step 2 comprises:
adding aqueous solution of tannic acid to NiS2@ ZIF-8, stirring, centrifuging, washing, precipitating, filtering, and drying to obtain Y-S NiS with internal voids2@ZIF-8。
The NiS2The solvent of the @ ZIF-8 dispersion is a water-alcohol mixed solution phase solvent, preferably a water-ethanol mixed solvent;
optionally, step 3 comprises:
mixing Y-S NiS2Sealing the @ ZIF-8 and sulfur powder in a vacuum quartz tube according to a certain proportion, annealing and carbonizing the whole quartz tube at high temperature, and pickling to remove zinc sulfide to obtain the product Y-S NiS2@ C composite material.
The Y-S NiS2The ratio of @ ZIF-8 to the sulfur powder is that the amount of sulfur element in the sulfur powder is larger than that of Y-S NiS2The amount in @ ZIF-8 is preferably 1:1 by mass; the annealing temperature is 500-800 ℃; the acid for acid washing is an acid solution capable of dissolving zinc sulfide.
The invention has the beneficial effects that:
He-ShiCompared with the prior art, the NiS coated with ZIF-8 of the invention2The preparation method comprises the steps of taking nano particles and tannic acid as initial raw materials, directly mixing and standing the raw materials through a liquid phase to enable the raw materials to completely react, etching ZIF-8 internal substances to obtain pores, and carbonizing the pores to obtain the NiS coated with the carbon in the shape of a bell2Composite material, such structure not only can effectively buffer NiS2The volume expansion of the material in the battery charging and discharging process can keep the structural stability of the material, and higher rate performance is provided. S, N the uniformly co-doped carbon shell layer can effectively increase the capacitance of the active material. The material is used in potassium ion battery at 1A g-1At a current density of 276 mAh g, the capacity after 500 cycles was maintained-1While the charging and discharging current is from 0.1A g-1Increased to 20A g-1The rate capability test is carried out at 20A g-1The capacity of the solution is kept at 260 mAh g-1, and when the solution returns to 0.1A g-1, the capacity is still kept at 550 mAh g-1And excellent rate performance is shown.
The preparation method provided by the invention is simple to operate, short in period and easy to realize large-scale production.
Drawings
FIG. 1 shows NiS of a bell-shaped structure prepared in example 12Transmission electron micrograph of composite, in which: a is NiS2A representative low-resolution image of transmission electron microscope of the composite material, b is NiS2Typical transmission electron microscopy high resolution images of the composites.
FIG. 2 shows NiS of a bell-shaped structure prepared in example 12X-ray diffraction pattern of the composite.
FIG. 3 shows NiS with a bell-shaped structure prepared in example 12The composite material is a battery charge-discharge cycle performance diagram of a potassium ion battery cathode material.
FIG. 4 shows NiS with a bell-shaped structure prepared in example 12The composite material is a battery charge-discharge rate performance diagram of a potassium ion battery cathode material.
FIG. 5 shows NiS with a bell-shaped structure prepared in example 12The nitrogen isothermal adsorption curve a and b of the composite material are shown as pore size distribution curves.
FIG. 6 is a schematic view ofNiS of Bell-shaped Structure prepared in example 12Elemental two-dimensional imaging of composite materials, in which: a is NiS2And (b) a dark field phase transmission electron microscope image of the composite material, wherein b is a distribution diagram of each element.
Fig. 7 is a charge-discharge cycle curve of the potassium ion battery obtained by using the nickel disulfide prepared in step 1) of this embodiment as a negative electrode material of the potassium ion battery.
Fig. 8 is a schematic view of the microstructure of the electrode material of the potassium ion battery.
Detailed Description
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The analysis method in the examples of the present application is as follows:
transmission electron microscopy analysis was performed using a transmission electron microscope (TEM, FEI Inc., USA, Tecnai F20).
Phase analysis of the compounds was performed using an X-ray powder diffractometer (XRD, Rigaku, Miniflex 600).
Specific surface area and pore structure analysis were measured using a fully automated gas physical adsorption apparatus (Autosorb-iQ 2-XR, Congta instruments, USA).
Cyclic voltammetry tests were performed using an electrochemical workstation (shanghai chen hua, CHI 660D).
Thermogravimetric analysis was performed using a simultaneous thermal analyzer (TG/DTA, STA449F3, Netzsch).
The battery performance test was performed using a battery test system (wuhan blue, CT 3001A).
Example 1:
1) dispersing 0.3g PVP (MW:40000) in a mixed solution of 20ml water and 20ml ethylene glycol, stirring to dissolve uniformly, adding 1mmol nickel acetate and 3mmol sodium thiosulfate, stirring to dissolve into a uniform solution, transferring to a 100ml reaction kettle, placing in a water heating box at 180 ℃, preserving heat for 12h, naturally cooling, centrifuging the obtained suspension, washing with water and ethanol, and finally dispersing the washed precipitate in methanol for later use, thus obtaining NiS2A methanol dispersion of nanoparticles.
2) Will obtain 100-150nm sized NiS210mg of the nanoparticle dispersion was added to a solution containing 0.5mmol of Zn (NO)3)2Adding methanol solution containing 1mmol of dimethyl imidazole under stirring, stirring for 1min, standing for 24 hr, filtering, washing with methanol, and drying to obtain 2-methyl imidazole zinc salt (ZIF-8) -coated NiS2Compound (NiS)2@ZIF-8)；
3) Mixing NiS2@ ZIF-8 is dispersed in a mixed solution of 0.4ml of water and 4.6ml of absolute ethyl alcohol, and mixed solution A is obtained by ultrasonic homogenization; dispersing 50mg tannic acid in 5ml water to obtain mixed solution B, adding B into A under stirring, standing for 10min, centrifuging to remove mother liquor, washing precipitate with water and ethanol, filtering, and drying to obtain Y-S NiS with internal void2The structure of @ ZIF-8 and "Y-S" is a core-shell structure having a bell shape.
4) The obtained Y-S NiS2Sealing the tube with the @ ZIF-8 and the sulfur powder according to the mass ratio of 1:1, placing the tube in a muffle furnace at 600 ℃ for 3 hours to obtain a carbonized product, stirring the carbonized product for 8 hours at room temperature by using 1M hydrochloric acid to completely remove zinc sulfide to obtain the Y-S NiS2@ C composite material.
FIG. 1 is the Y-S NiS prepared in example 12A representative Transmission Electron Micrograph (TEM) of the @ C composite is a TEM. As can be seen from FIG. 1, the microstructure of the composite material is represented by a core-shell structure Y-S with a bell shape, the outer shell layer is a hollow sphere carbon shell, and NiS is coated inside the hollow sphere carbon shell2(ii) a Hollow sphere carbon shell and NiS2Hollow gaps are reserved between the two. NiS2Is nano-particles with the particle size of 100-150 nm; the volume size of the carbon shell layer of the hollow ball is NiS21.5-3 times of the nano particles.
FIG. 2 shows the Y-S NiS prepared in this example2X-ray diffraction patterns of @ C composites; the phases of nickel disulfide are shown.
5) The product Y-S NiS of the step 4) is treated2@ C (70 wt%), conductive carbon black (15 wt%) and carboxymethyl cellulose (CMC 15 wt%) were added to an agate mortar for pulverization and grinding, with deionized water as the dispersant. Dry foam ready for pressingNickel and weighed. And smearing the slurry obtained after uniform grinding on a foamed nickel current collector, drying in vacuum at 80 ℃ for 12h, weighing the dried electrode plates, and obtaining the mass of the slurry on each electrode plate according to the mass difference before and after smearing the current collector. After weighing, vacuum drying the electrode plates for 2 hours at 80 ℃, and putting the dried electrode plates into a glove box to be assembled with a button cell;
6) assembling the button cell in a glove box filled with argon, taking a metal potassium sheet as a negative electrode, taking glass fiber as a diaphragm, and taking the manufactured electrode sheet as a positive electrode;
7) the constant-current charge and discharge test mainly inspects the charge and discharge specific capacity, the cycle performance and the multiplying power performance of the potassium ion half-cell under different currents. The potassium ion semi-battery does not have potassium ions in the positive electrode in an initial state, so that the battery is subjected to constant current discharge at first, and the potassium ions in the metal potassium sheet are embedded into the positive electrode material; after the discharge is finished, the anode material is in a potassium-rich state, and the charge test is started, so that the cycle test is carried out. The test voltage of the button cell is 0.05-2.8V, and the charge-discharge current density is set to be 100 mA g-1-20A g-1 according to the experimental conditions.
FIG. 3 shows Y-S NiS prepared by this example2The @ C composite material is a battery charge-discharge cycle performance diagram of a potassium ion battery cathode material. Its capacity after 500 cycles was maintained at 276 mAh g-1 at a current density of 1A g-1;
FIG. 4 shows Y-S NiS prepared in this example2The @ C composite material is a battery charge-discharge rate performance diagram of a potassium ion battery cathode material. The capacity of the battery is 480, 434, 386, 358, 318 and 260 mAh g-1 under the current density of 1, 2, 4, 6, 10 and 20A g-1 when the charge and discharge current is increased from 0.1A g-1 to 20A g-1 and the capacity is still maintained at 550 mAh g-1 when the current density is returned to 0.1A g-1, thereby showing excellent rate performance.
FIG. 5 is Y-S NiS2The graph a and b of the @ C composite nitrogen isothermal adsorption curve is a pore size distribution curve. The specific surface area of the powder is 181 m2Per g, pore volume 0.33 cm3(ii)/g, having a pore size distribution of 0.4nm to 35 nm; wherein the main pore size distribution is concentrated in three intervals: 1-2 nm; 3-6 nm;15-30nm。
fig. 6 shows the bell-shaped structural feature, and S, N element is uniformly distributed on the carbon shell layer, forming S, N co-doped carbon.
Fig. 7 is a charge-discharge cycle curve of the potassium ion battery obtained by using the nickel disulfide prepared in step 1) of this embodiment as a negative electrode material of the potassium ion battery, and it can be seen from the graph that the cycle performance is very poor, and the capacity fading is close to 0 within 50 cycles.
Example 2
This example is different from example 1 in that zinc sulfate is used in place of zinc nitrate in step 2) and Y-S NiS is used in step 4)2@ ZIF-8 and sulfur powder in a mass ratio of 1:2, the annealing temperature is 500-. The product after carbonization is Y-S NiS2@ C composite material.
Claims (10)
1. A preparation method of an electrode material of a potassium ion battery comprises the following steps:
1) coating NiS with 2-methylimidazolium zinc salt ZIF-82Nanoparticles to give ZIF-8 coated NiS2Composite NiS2@ ZIF-8；
2) Etching NiS with tannic acid2@ ZIF-8 to obtain a Bell-shaped complex Y-S NiS with internal voids2@ ZIF-8；
3) In the atmosphere of sulfur vapor, Y-S NiS2@ ZIF-8 annealing, carbonizing, pickling and removing zinc sulfide to obtain Y-S NiS2The @ C composite material is the electrode material of the potassium ion battery.
2. The method of claim 1, wherein step 1) comprises: mixing NiS2Uniformly dispersing the dispersion liquid of the nano particles into a methanol solution of zinc salt, adding a methanol solution of dimethyl imidazole, fully reacting, filtering, washing and drying to obtain NiS wrapped by ZIF-82Compound (NiS)2@ZIF-8)；
The zinc salt is one or more of zinc nitrate, zinc chloride and zinc sulfate.
3. The method of claim 1, wherein step 2) comprises: adding aqueous solution of tannic acid to NiS2@ ZIF-8, stirring, centrifuging, washing, precipitating, filtering, and drying to obtain NiS with internal voids2Compound (Y-S NiS)2@ZIF-8)；
The NiS2The solvent of the @ ZIF-8 dispersion liquid is a water-alcohol mixed solvent;
preferably, NiS2The solvent of the @ ZIF-8 dispersion is a mixed solvent of water and ethanol.
4. The method of claim 1, wherein step 3) comprises: mixing Y-S NiS2Sealing the @ ZIF-8 and sulfur powder in a vacuum quartz tube according to a certain proportion, annealing and carbonizing the whole quartz tube at high temperature, and pickling to remove zinc sulfide to obtain the product Y-S NiS2@ C composite material;
the Y-S NiS2The ratio of @ ZIF-8 to the sulfur powder is that the amount of sulfur element in the sulfur powder is larger than that of Y-S NiS2@ ZIF-8;
the annealing carbonization temperature is 500-800 ℃;
the acid for acid cleaning is an acid solution capable of dissolving zinc sulfide;
preferably, said Y-S NiS2The mass ratio of @ ZIF-8 to sulfur powder is 1: 1.
5. The preparation method of any one of claims 1 to 4, wherein the electrode material for the potassium ion battery is prepared by the following general structural formula: Y-S NiS2@ C, wherein C denotes the carbon shell, NiS2Denotes NiS2A compound, Y-S represents a core-shell structure having a bell shape;
the carbon shell layer is a hollow sphere carbon shell layer, and NiS is coated inside the hollow sphere carbon shell layer2；
The hollow ball carbon shell and NiS2Hollow gaps are reserved between the two.
6. The electrode material for a potassium-ion battery according to claim 5,
the NiS2Is nano-particles with the particle size of 100-150 nm;
the NiS2Accounting for 30-70wt% of the total mass of the electrode material;
preferably, said NiS2The shape of the nano particles is curved spherical particles;
preferably, said NiS2Accounting for 52.4wt percent of the total mass of the electrode material.
7. The electrode material for a potassium-ion battery according to claim 6,
the shape of the carbon shell layer of the hollow sphere is a hollow sphere-like body, and the hollow sphere-like body is selected from one or more of a hollow ellipsoid, a hollow sphere, a hollow ovoid or a hollow olive sphere;
preferably, the carbon shell layer of the hollow sphere has a porous structure;
preferably, the main component of the carbon shell layer of the hollow sphere is carbon;
preferably, the carbon atoms of the carbon shell layer of the hollow sphere are doped with S and N atoms; s, N are uniformly distributed in and on the shell of the hollow sphere carbon shell;
preferably, the volume size of the carbon shell layer of the hollow sphere is NiS21.5 times of the volume of the nano particles;
preferably, the volume size of the carbon shell layer of the hollow sphere is NiS21.5-3 times of the volume of the nano particles.
8. The electrode material for a potassium ion battery according to claim 6, wherein the hollow sphere carbon shell layers are aggregated in a close-packed manner.
9. The electrode material for potassium ion batteries according to any one of claims 5 to 8, which is applied to a potassium ion battery.
10. The potassium ion battery of claim 9, comprising a positive electrode, a negative electrode, and an electrolyte; characterized in that the negative electrode comprises: a current collector and a negative electrode material supported on the current collector; wherein the negative electrode material contains the potassium ion battery electrode material prepared by the preparation method of any one of claims 1 to 4.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115548283A (en) * | 2022-09-01 | 2022-12-30 | 河北工业大学 | NiS 2 Preparation method and application of @ C/HC electrode material |
| CN115548283B (en) * | 2022-09-01 | 2024-04-19 | 河北工业大学 | NiS (nickel-zinc sulfide)2Preparation method and application of @ C/HC electrode material |
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