CN113937285B - PVP (polyvinyl pyrrolidone) induced VS (voltage VS) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 - Google Patents
PVP (polyvinyl pyrrolidone) induced VS (voltage VS) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 Download PDFInfo
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- CN113937285B CN113937285B CN202111159109.6A CN202111159109A CN113937285B CN 113937285 B CN113937285 B CN 113937285B CN 202111159109 A CN202111159109 A CN 202111159109A CN 113937285 B CN113937285 B CN 113937285B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/604—Polymers containing aliphatic main chain polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses PVP induced VS 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 Belonging to the technical field of battery materials. Firstly, preparing an aqueous solution with the concentration of 0.167M from ammonium metavanadate and polyvinylpyrrolidone according to the proportion of 1; then respectively washing the anode material for 3 times by using deionized water and ethanol, and drying to obtain the positive electrode material PVP-VS of the magnesium ion battery 4 . The invention realizes the embedding of PVP into VS by a one-step hydrothermal method 4 Interchain, PVP-VS was induced 4 Chain pitch enlargement, V 3+ Self-doping, sulfur-rich vacancy formation and high-index crystal face exposure, and realizes Mg 2+ With MgCl + The co-embedding of ions exposes more active sites, improves the ion diffusion speed, enhances the reaction kinetics and the structural stability, and further improves the electrochemical performance of the magnesium ion battery. The magnesium ion battery assembled by the composite material has high specific capacity, excellent cycling stability and rate performance, and wide application prospect.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to PVP (polyvinyl pyrrolidone) induced VS (voltage VS) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 。
Background
The development of low-cost renewable energy storage technology is undoubtedly an effective approach to solve the energy and environmental crisis faced by the present society. Magnesium ion battery with high volume specific capacity (3833 mAh cm) -3 ) Low cost, high safety, and little environmental impact, and is receiving wide attention (see literature: cu (copper) 2 MoS 4 hollow nanocages with fast and stable Mg 2+ Storage performance, zhang et al chem.eng.j.,2020,387, 124125). Despite the magnesiumIon batteries have many advantages, but still have some problems, such as: the magnesium ion battery has poor cycle stability, low specific capacity, slow diffusion kinetics and the like (see the literature: precipitation-purification TiO) 2 (B) nanowies with proto-ns charge compression for regulating a reversible magnesium store, luo et al. On the other hand, in a standard chlorine-based electrolyte, mgCl + As the main electro-active species, mg-Cl bond is hardly destroyed to release Mg 2+ Participate in the reaction. Therefore, there is still a great challenge to properly modify the cathode material, and the microstructure of the cathode material is controlled to maximize the ion transport channel, improve the structural stability and ensure Mg 2+ And MgCl + Co-insertion and rapid diffusion are of crucial importance.
An interlayer control method by introducing organic molecules is one of effective approaches to solve the above problems. The organic molecules can realize the expansion of the interlayer spacing of the anode material through the bonding action between the organic molecules and the anode material, weaken the electrostatic interaction between the organic molecules and the anode material when working ions are rapidly diffused, and relieve the stress change caused in the embedding/removing process of the working ions (see the literature: PVP incorporated MoS) 2 as a Mg ion host with enhanced capacity and purity, wu et al.J. mater. Chem.A,2019,7, 4426-4430). Further, if the interlayer spacing of the positive electrode material is expanded sufficiently, it is possible to realize Mg 2+ And MgCl + Co-intercalation, which will achieve high reversible capacity, excellent cycling stability and good rate performance of magnesium ion batteries (see literature: interchain-expanded vanadium tetrasulf iotade with fast kinetics for rechargeable magnesium batteries, pei et al, acs appl. Mater. Inter.,2019,11, 31954-31961). Polyvinylpyrrolidone (PVP) is used as a nonionic polymer, has high-efficiency coordination force, contains a lactam ring, and can interact with other compounds to expand the interlayer spacing of the positive electrode material and keep the structure stable, so that the regulated positive electrode material has higher magnesium storage performance.
Self-doping in addition to interlayer organic molecular regulationIs a promising strategy for improving the electrochemical performance of the magnesium-ion battery. Since the difference between the ionic radii of the autodoping material and the host material is small, the lattice distortion caused by the autodoping material is small, and the structural stability of the active material can be maintained. In addition, autodoping can also increase the carrier transport rate to achieve excellent cycling stability and significant rate performance. In addition to autodoping, the formation of abundant vacancies can also serve as electrochemically active sites to adsorb more Mg 2+ Promoting Mg 2+ The storage of (2), enhancing charge transfer kinetics. In addition, the exposed high-index crystal face has high surface energy, an open surface structure and abundant unsaturated coordination, is beneficial to enhancing interface charge transfer and adsorbing more magnesium ions, provides a more effective diffusion path for ion diffusion, and improves the specific capacity and rate capability of the magnesium ion battery. Among the numerous magnesium ion battery positive electrode materials, VS 4 Is considered to be a typical linear chain-like structure host material with two S' S between the V centers 2 2- In which V is 4+ (S 2 2- ) 2 The chains are bound by weak van der waals forces, a special linear chain structure and weak van der waals forces that facilitate rapid diffusion and transport of ions/electrons. However, VS 4 The magnesium-ion battery is still required to be modified by the method so as to enhance the magnesium storage performance of the magnesium-ion battery and be applied to the magnesium-ion battery.
The invention prepares PVP interchain embedded VS by a one-step hydrothermal method 4 (PVP-VS 4 ) As a magnesium ion battery cathode material, the electrochemical performance of the magnesium ion battery cathode material applied to a magnesium ion battery is studied. Electrochemical performance test results show that VS is embedded between PVP chains 4 Induced chain spacing expansion, V 3+ The synergistic effect of the series of microstructure changes such as self-doping, sulfur-rich vacancy formation and high-index crystal face exposure enables PVP-VS 4 The specific capacity, the cycle life and the rate capability of the material are all improved. At 0.05Ag -1 At current density of (2), PVP-VS 4 The specific capacity of the alloy is maintained to be 145mAh g -1 Left and right. And at a current density of from 0.05Ag -1 Increased to 5Ag -1 The specific capacity of the electrode material is 151mAh g -1 Change to 45mAhg -1 When the current density is restored to 0.05ag -1 The specific capacity is recovered to 138mAh g -1 And the high-power-factor performance is shown. Furthermore, at 5ag -1 At current density of (2), PVP-VS 4 After 1500 cycles, the capacity retention rate reaches 80%. The invention provides an innovative feasible way for obtaining the microstructure regulation of the electrode material of the ion battery with high electrochemical performance.
Disclosure of Invention
The invention aims to provide a magnesium ion battery positive electrode material, in particular to a PVP (polyvinyl pyrrolidone) -induced VS (positive electrode material) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 . PVP at VS 4 Induces an enlargement of the strand spacing, V 3+ The PVP-VS is caused by the microstructural changes of self doping, the formation of sulfur-rich vacancy, the exposure of high-index crystal face and the like 4 And the material has the characteristics of high specific capacity, excellent cycling stability, high rate capability and the like.
In order to achieve the aim, the invention provides a positive electrode material PVP-VS of a magnesium ion battery 4 The preparation process of (A) is as follows: 1. respectively weighing polyvinylpyrrolidone (PVP) and ammonium metavanadate according to the mass ratio of 1;
2. weighing excessive thioacetamide, dissolving in glycol with the same volume as the solution A, and magnetically stirring at normal temperature until the thioacetamide is completely dissolved to obtain a solution B;
3. mixing the solution B and the solution A, and magnetically stirring at a constant temperature of 60 ℃ until the two solutions are completely mixed;
4. transferring the fully mixed solution into a 100ml reaction kettle, heating to 200 ℃, reacting for 4 hours, and cooling to room temperature along with the furnace after the reaction is finished;
5. washing with deionized water and anhydrous ethanol for 3 times, centrifuging, collecting precipitate, vacuum drying at 60 deg.C for 12 hr to obtain positive electrode material PVP-VS 4 。
The invention also providesSupplied with PVP-VS 4 The composite material is used as a positive electrode material in a magnesium ion battery, and is assembled with a metal magnesium negative electrode, a glass fiber diaphragm and an APC-THF electrolyte to form a button battery. Standing the assembled battery for 24h, and then carrying out electrochemical performance test on a CT2001A battery program-controlled tester, wherein the test voltage window is 0.2-2.1V, and the current density is 50-5000 mA g -1 。
The positive electrode material PVP-VS of the magnesium ion battery provided by the invention 4 Has the advantages that:
1. the positive electrode material PVP-VS of the magnesium ion battery synthesized by the invention 4 Due to PVP embedding into VS 4 Interchain, enlarged PVP-VS 4 Not only increase PVP-VS 4 The contact area with the electrolyte exposes more active sites, and Mg can be realized 2+ And MgCl + Co-embedding and attenuating the same in PVP-VS 4 The polarization in the structure enhances the diffusion dynamics and improves the specific capacity and the rate capability of the magnesium ion battery;
2. the positive electrode material PVP-VS of the magnesium ion battery prepared by the invention 4 Due to PVP embedding in VS 4 Between chains, induce V 3+ Self-doping, formation of sulfur-rich vacancy, exposure of high-index crystal face and other series of microstructure changes. Wherein, V 3+ The self-doping can improve the conductivity of the anode material and accelerate the reaction kinetics; sulfur-rich vacancy formation can increase active sites and can mitigate PVP-VS induction during cycling 4 Maintaining structural stability; the exposure of the high-index crystal face is beneficial to increasing the active sites and accelerating the diffusion speed of ions; the specific capacity, the cycle life and the rate capability of the magnesium ion battery are improved under the synergistic effect of the microstructure changes.
3. The positive electrode material PVP-VS of the magnesium ion battery prepared by the invention 4 Shows excellent electrochemical performance: at 0.05A g -1 The specific capacity is maintained at 145mAh g under the current density -1 Left and right. And at a current density of from 0.05ag -1 Increased to 5ag -1 The specific capacity of the electrode material is 151mAh g -1 Change to 45mAh g -1 When current density is highThen returns to 0.05A g -1 The specific capacity is recovered to 138mAh g -1 And the high-power-factor performance is shown. In addition, at 5Ag -1 The capacity retention rate reached 80% after 1500 cycles at the current density of (1).
The concept, shape, structure and technical effects of the present invention will be further described with reference to the accompanying drawings.
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 principles of the invention and not to limit the invention. In the drawings:
FIG. 1 shows the positive electrode material PVP-VS of the magnesium-ion battery obtained in example 1 4 XRD pattern of (a);
FIG. 2 shows the positive electrode material PVP-VS of the magnesium ion battery obtained in example 1 4 XPS spectra of (1);
FIG. 3 shows the positive electrode material PVP-VS of the magnesium ion battery obtained in example 1 4 V high resolution XPS spectra of (a);
FIG. 4 shows the positive electrode material PVP-VS of the magnesium ion battery obtained in example 1 4 An EPR map of (a);
FIG. 5 shows the positive electrode material PVP-VS of the magnesium-ion battery obtained in example 1 4 HRTEM picture of (020) crystal face;
FIG. 6 shows the positive electrode material PVP-VS of the magnesium-ion battery obtained in example 1 4 The electrochemical performance curve of (a);
FIG. 7 shows the positive electrode material PVP-VS of the magnesium-ion battery obtained in example 1 4 At 5A g -1 Cycling performance curve at current density.
Detailed Description
The present invention will be described in further detail with reference to specific examples, which, however, should not be construed as limiting the scope of the present invention in any way.
Examples
Weighing 0.58g of ammonium metavanadate and 0.0058g of polyvinylpyrrolidone, dissolving in 30ml of deionized water, and magnetically stirring at a constant temperature of 60 ℃ until the ammonium metavanadate and the polyvinylpyrrolidone are completely dissolved to obtain a solution A; at the same time, the excess of thio groups is weighedDissolving acetamide in 30ml of glycol, and magnetically stirring at normal temperature until the acetamide is completely dissolved to obtain a solution B; the solution A and the solution B are fully mixed under constant temperature magnetic stirring at 60 ℃. Then, transferring the mixed solution into a 100ml reaction kettle, reacting for 4 hours at 200 ℃, and cooling to room temperature along with the furnace; washing the precipitate with deionized water and anhydrous ethanol for 3 times, respectively, placing into a vacuum drying oven, and drying at 60 deg.C for 12 hr to obtain positive electrode material PVP-VS of magnesium ion battery 4 。
After hydrothermal reaction, PVP is embedded into VS 4 Interchain, and enlarging PVP-VS 4 The results are shown in XRD (FIG. 1), as can be seen in FIG. 1, except for VS 4 Is not formed, and PVP-VS 4 The diffraction peak of (A) is shifted to a low angle relative to the standard pattern, indicating that PVP is embedded in VS 4 The chain space is enlarged among chains. From PVP-VS 4 VS was also observed in the XPS survey (FIG. 2) 4 V and S elements in PVP and C, N and O elements in PVP prove that PVP-VS is adopted 4 The synthesis of (2). The high resolution XPS spectrum of V shows that V has both +3 and +4 valency states (FIG. 3), indicating that PVP-VS 4 In has V 3+ Self-doping of (3). PVP-VS 4 The EPR profile of (fig. 4) shows PVP-VS at g =1.953 4 Has a significantly higher VS 4 Peak of (D) in PVP-VS 4 Rich sulfur vacancies exist in the alloy. The HRTEM image in FIG. 5 clearly shows that several layers of PVP-VS with the same orientation and the lattice spacing of 0.52nm are all observed 4 Nanosheets, corresponding to the (020) crystal plane, indicated that the high index crystal plane was exposed.
The prepared PVP-VS 4 And (3) as a positive electrode material of the magnesium ion battery, respectively using the polished magnesium foil and the glass fiber filter membrane as a negative electrode and a diaphragm of the magnesium ion battery, using 0.4M APC-THF as an electrolyte, and assembling the magnesium foil and the glass fiber filter membrane into a button battery in a glove box filled with argon. Standing the assembled magnesium ion battery for 24 hours, and then carrying out electrochemical performance test on a CT2001A battery program-controlled tester, wherein the test voltage window is 0.2-2.1V, and the current density is 0.05-5 Ag -1 。
The obtained positive electrode material PVP-VS of the magnesium ion battery 4 Rate capability ofAnd cycling behavior as shown in FIG. 6 at current densities from 0.05ag -1 Is lifted to 5Ag -1 In the process, the specific capacity is 151mAh g -1 Change to 45mAh g -1 And when the current density is reduced to 0.05ag -1 When the specific capacity is recovered to 134mAh g -1 And excellent rate performance is shown. The cycling behavior is shown in FIG. 6 at a current density of 0.05ag -1 The specific capacity is stabilized at 145mAh g -1 Left and right. 5A g -1 The cycle performance under the current density is shown in fig. 7, and it can be seen that after 1500 cycles, the capacity can still keep about 80% of the initial capacity value, and good cycle stability performance is shown.
Claims (3)
1. PVP induced VS 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 The preparation method is characterized by comprising the following preparation processes:
respectively weighing polyvinylpyrrolidone and ammonium metavanadate according to the mass ratio of 1; then weighing excessive thioacetamide and dissolving the thioacetamide in glycol with the same volume as the aqueous solution; completely mixing the two solutions, transferring the mixture into a reaction kettle, reacting for 4 hours at 200 ℃, after the reaction is finished, respectively washing precipitates for 3 times by using deionized water and absolute ethyl alcohol, and drying in vacuum to obtain the positive electrode material PVP-VS of the magnesium ion battery 4 ；
The obtained positive electrode material PVP-VS of the magnesium ion battery 4 The button magnesium ion battery is assembled, the voltage window for electrochemical performance test is 0.2-2.1V, and the current density is 0.05-5 Ag -1 。
2. A PVP-induced VS according to claim 1 4 Microstructure-regulated magnesium ion battery positive electrode material PVP-VS 4 Characterized in that PVP is embedded in VS 4 Interchain, PVP-VS was induced 4 Enlargement of chain spacing, V 3+ Self-doping, formation of sulfur-rich vacancies, and exposed series microstructural changes of high index crystal planes.
3. The PVP induced VS of claim 1 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 Characterized in that when the prepared material is used as the anode of the magnesium ion battery, the current density is 0.05Ag -1 The specific capacity is stabilized at 145mAh g -1 Left and right; at 5Ag -1 Under the current density, after 1500 cycles, the capacity retention rate reaches 80%, and the high-power-factor performance is achieved.
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| CN202111159109.6A CN113937285B (en) | 2021-09-30 | 2021-09-30 | PVP (polyvinyl pyrrolidone) induced VS (voltage VS) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 |
| ZA2022/00085A ZA202200085B (en) | 2021-09-30 | 2022-01-03 | Magnesium ions battery cathode material pvp-vs4 acquired by pvp inducing microstructure modulation of vs4 and application thereof |
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| CN202111159109.6A CN113937285B (en) | 2021-09-30 | 2021-09-30 | PVP (polyvinyl pyrrolidone) induced VS (voltage VS) 4 Microstructure-regulated positive electrode material PVP-VS of magnesium ion battery 4 |
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| CN112242526A (en) * | 2020-10-20 | 2021-01-19 | 青岛科技大学 | Mo-doped VS4Magnesium ion battery positive electrode material and application thereof |
| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
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| CN112259733A (en) * | 2020-10-21 | 2021-01-22 | 湘潭大学 | Nanotube-shaped magnesium ion battery positive electrode material and preparation method thereof |
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| CN112242526A (en) * | 2020-10-20 | 2021-01-19 | 青岛科技大学 | Mo-doped VS4Magnesium ion battery positive electrode material and application thereof |
| CN112490438A (en) * | 2020-11-27 | 2021-03-12 | 青岛科技大学 | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof |
Non-Patent Citations (1)
| Title |
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| PVP incorporated MoS2 as a Mg ion host with enhanced capacity and durability;Han Tang;《Journal Materials Chemistry A》;20190731;第4426-4430页 * |
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