CN113964321B - K (K) + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 /N-TG - Google Patents

K (K) + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 /N-TG Download PDF

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CN113964321B
CN113964321B CN202111224763.0A CN202111224763A CN113964321B CN 113964321 B CN113964321 B CN 113964321B CN 202111224763 A CN202111224763 A CN 202111224763A CN 113964321 B CN113964321 B CN 113964321B
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ion battery
magnesium ion
kvs
embedding
reaction
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CN113964321A (en
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李镇江
丁诗琦
田雨欣
戴鑫
孟阿兰
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Qingdao University of Science and Technology
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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
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • 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 a K + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 N-TG, which belongs to the technical field of battery materials. Preparing ammonium metavanadate into an aqueous solution, mixing with an excessive thioacetamide glycol solution, transferring the aqueous solution and a carbon sheet prepared by adopting a vapor deposition method and growing with N-TG into a reaction kettle, and carrying out hydrothermal reaction for 4 hours at 180 ℃; drying the product and then carrying out electrochemical method on the product in K 2 SO 4 K in solution + Pre-embedding to obtain the magnesium ion battery anode material KVS 4 N-TG. The invention is realized by K + The pre-embedded type magnesium ion battery is pre-embedded in an intercalation type positive electrode material, so that multi-electron reaction can be realized, the structural stability of the positive electrode material can be maintained, and the electrochemical performance of the magnesium ion battery is improved. The magnesium ion battery assembled by the method has high specific capacity and excellent cycle stability, and has wide application prospect.

Description

K (K) + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 /N-TG
Technical Field
The invention relates to the technical field of battery materials, in particular to a K + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 /N-TG。
Background
Because of the abundance of multivalent elements, multivalent metal ion-based batteries are considered energy storage devices with potential applications. The magnesium ion battery is used as a novel energy storage system, and has high safety, low cost and high theoretical capacity (3833 mAh cm) –3 ) And the like, and are widely studied. However, the slow charge transfer of divalent magnesium ions causes problems such as low structural stability, slow kinetics and even low specific capacity. To take advantage of the high charge density of divalent magnesium ions, it is desirable to achieve both multiple electron transfer and structural stabilityPositive electrode materials, which are major challenges in developing magnesium ion batteries with high specific capacity and cycling stability.
In recent years, multi-electron reactions in ion batteries have attracted considerable attention from researchers because of the ability of multiple electrons to participate in reactions to increase battery capacity storage. However, the multi-electron reaction mostly occurs in the conventional conversion electrode material, and for the intercalation electrode material, modification of the electrode material is difficult to surpass its reaction mechanism, and is limited to single-electron reaction only (see, documents: naphthalene diimide as a two-electron anolyte for aqueous and neutral pH redox flow batteries, medabalmi et al J. Mater. Chem. A,2020,8,11218-11223). From the perspective of electrode design, vanadium elements exhibit more electrochemical diversity and multiple electron cloud density in different crystal structures. VS (virtual switch) 4 As a typical vanadium-based sulfide, the valence state of the V element is +4, and when the electronic environment is changed, the chemical valence state thereof may be changed from +2 to +5. In addition, VS 4 Has a unique linear chain structure, the distance between adjacent chains is 0.56nm, and the adsorption of magnesium ions is facilitated. Thus VS 4 Is considered as a magnesium ion battery positive electrode material with research significance. However, VS 4 Is a typical intercalation type positive electrode material with single electron transfer, which is verified in the prior report (see literature: morphy-dependent electrochemical performance of VS) 4 for rechargeable magnesium battery and its magnesiation/demagnesiation mechanism, li et al J.Power Sources,2020,451,227815), therefore, by VS without changing the intercalation mechanism 4 And modifying to realize multi-electron reaction and further improve the specific capacity. However, large volume changes are caused during the multi-electron reaction process, which makes it difficult to maintain the structural stability of the host material, which limits the cycle reversibility and stability of the magnesium ion battery (see literature: heter-layed MoS) 2 /C composites enabling ultrafast and durable Na storage,Li et al.Energy Storage Mater.2019,21,115-123)。
The invention realizes K by an electrochemical method + Pre-embedded VS 4 N-TG and studied the KVS 4 N-TG is used as a positive electrode material in the multi-electron reaction process and the electrochemical performance of a magnesium ion battery. The series characterization result shows that K + Pre-embedding induction V 2+ Appear, V 2+ Is present such that V 2+ /V 4+ 、V 4+ /V 5+ The reaction process is carried out to promote the KVS 4 The multi-electron reaction is realized in the positive electrode material of the N-TG magnesium ion battery. The electrochemical properties show that due to K + Pre-embedding induces multiple electron responses and pre-embedded K + KVS as a synergistic effect in maintaining structural stability of the post 4 The specific capacity and the cycle performance of the N-TG are improved. At 0.05A g -1 KVS at current density of (a) 4 N-TG showed 190mAh g -1 Is a high specific capacity of (a). And at 1A g -1 KVS at current density of (a) 4 After 2000 cycles of/N-TG, the capacity retention was approximately 100%.
Disclosure of Invention
The invention aims to provide a magnesium ion battery anode material, in particular to K + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 N-TG. Through K + Pre-embedded modified KVS 4 The N-TG magnesium ion battery anode material realizes multi-electron reaction and maintains the stable structure of the anode material without changing an intercalation reaction mechanism, and has higher specific capacity and better cycle stability.
To achieve the above object, the present invention provides a magnesium ion battery anode material KVS 4 The preparation process of the N-TG is as follows:
1. according to the mass ratio of 9:1, weighing melamine and silicon powder in proportion, fully grinding, putting the melamine and the silicon powder and the carbon sheet with the catalyst dropwise into a vacuum atmosphere furnace for calcination, and obtaining nitrogen doped tubular graphene (N-TG) uniformly growing on the surface of the carbon sheet after the carbon sheet is cooled to normal temperature;
2. ammonium metavanadate is dissolved in deionized water under the condition of stirring at 60 ℃ to obtain a solution A with the concentration of 0.167M;
3. weighing excessive thioacetamide to be dissolved in glycol with the volume equal to that of the solution A, and stirring until the thioacetamide is completely dissolved to obtain a solution B;
4. mixing the solution A and the solution B, and stirring at 60 ℃ until the two solutions are completely mixed;
5. transferring the fully mixed solution and the carbon sheet growing with the N-TG into a 100ml reaction kettle, heating to 180 ℃, reacting for 4 hours, and cooling to room temperature along with a furnace after the reaction is finished;
6. taking out the reacted sample, washing with deionized water and absolute ethyl alcohol for 3 times, respectively, placing the obtained product into a vacuum drying oven, and drying at 60 ℃ for 12h to obtain VS 4 /N-TG。
7. By electrochemical means, as 1M K 2 SO 4 Is a solution with a current density of 20mA cm –2 VS under the condition of 0-1.2V voltage window 4 K-Process with N-TG + Pre-embedding to obtain the magnesium ion battery anode material KVS 4 /N-TG。
The invention also provides a KVS 4 The N-TG is used as a positive electrode material in a magnesium ion battery, and the positive electrode material, a magnesium metal negative electrode, a glass fiber diaphragm and an APC-THF electrolyte are assembled into a button cell. Standing the assembled battery for 24 hours, and then performing 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 and 1Ag -1 。
The invention provides a magnesium ion battery anode material KVS 4 The advantages of N-TG are:
1. the magnesium ion battery anode material KVS prepared by the invention 4 /N-TG，K + Pre-embedding induction V 2+ Production of V 2+ Is present such that V 2+ /V 4+ 、V 4+ /V 5+ The reaction process was carried out in KVS 4 Multiple electron reactions are realized in the positive electrode material of the N-TG magnesium ion battery, so KVS 4 The positive electrode material of the N-TG magnesium ion battery can show higher specific capacity.
2. The magnesium ion battery anode material KVS prepared by the invention 4 N-TG, pre-embedded K + Also acts as a "post" in the structure to maintain the junction by weakening the polarization between the magnesium ions and the positive electrode materialStability of structure, thus KVS 4 The N-TG magnesium ion battery cathode material may exhibit enhanced cycling stability.
3. The magnesium ion battery anode material KVS prepared by the invention 4 N-TG exhibits excellent electrochemical properties: at 0.05Ag -1 KVS at current density of (a) 4 N-TG showed 190mAh g -1 Is a high specific capacity of (a). At 1A g -1 The electrode material showed excellent cycle stability with a capacity retention of approximately 100% after 2000 cycles.
The conception, structure and technical effects of the present invention will be further described with reference to the accompanying drawings.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention. In the drawings:
FIG. 1 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 XRD pattern of N-TG;
FIG. 2 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 XPS profile of N-TG;
FIG. 3 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 V high resolution XPS spectrum of N-TG;
FIG. 4 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 V high resolution XPS spectrum of N-TG under different cut-off voltages;
FIG. 5 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 N-TG at 0.05A g -1 A cycle performance curve at current density;
FIG. 6 is a schematic view of a magnesium ion battery cathode material KVS obtained in example 1 4 N-TG at 1A g -1 Cycling performance curve at current density.
Detailed Description
The present invention is described in further detail below in connection with specific examples, which, however, do not limit the scope of the invention in any way.
Examples
Weighing 12.6g of melamine and 1.4g of silicon powder, fully grinding, then placing the mixture and a carbon sheet dropwise added with a nickel nitrate catalyst into a vertical vacuum atmosphere furnace, reacting at 1250 ℃ for 30min, and cooling the mixture along with the furnace to room temperature to obtain N-TG uniformly growing on the carbon sheet; 0.5814g of ammonium metavanadate is weighed and dissolved in 30ml of deionized water, and stirred at 60 ℃ until the ammonium metavanadate is completely dissolved, so as to obtain a solution A; weighing excessive thioacetamide to be dissolved in 30ml of ethylene glycol, and stirring at normal temperature until the thioacetamide is completely dissolved to obtain a solution B; thoroughly mixing the solution B and the solution A at 60 ℃; transferring the mixed solution and the carbon sheet growing with the N-TG into a 100ml reaction kettle, carrying out hydrothermal reaction for 4 hours at 180 ℃, and cooling to room temperature along with a furnace; taking out the sample, washing with deionized water and absolute ethyl alcohol for 3 times respectively, putting into a vacuum drying oven, and drying at 60 ℃ for 12h to obtain VS 4 N-TG; the obtained VS 4 N-TG as working electrode, saturated calomel electrode and platinum wire electrode as reference electrode and counter electrode, respectively, at 1M concentration of K 2 SO 4 The solution is electrochemically treated at 20mA cm –2 Three-stage circulation is carried out within the range of 0-1.2V voltage window under the current density, after the reaction is finished, the sample is washed 3 times by deionized water, and the magnesium ion battery anode material KVS is obtained by drying 4 /N-TG。
After hydrothermal reaction and electrochemical reaction, K + Successfully embed into VS 4 In the case of N-TG, it can be observed in XRD results (FIG. 1), except for VS 4 And N-TG, no new phase is generated, and VS 4 Low angular shift of diffraction peaks of (2) relative to the standard spectrum, can prove that K + Pre-embedding enlarges VS 4 N-TG strand spacing. K, V, S, C, N element was observed simultaneously in XPS (FIG. 2), further demonstrating K + Pre-embedding into VS 4 In the N-TG lattice. The high resolution XPS spectrum of V (FIG. 3) shows that the V element has V in addition to V 4+ In addition to the peak, V was also shown 2+ The peak of (C) indicates K + Pre-embedding induces V 2+ Is generated. By means of KVS 4 Analysis of the high resolution XPS spectrum of V (FIG. 4) for N-TG at different cut-off voltages gave the following junctionsDuring discharge, V 2+ Gradually disappear, V 5+ Gradually appear and have no V 3+ Is also from V in the valence state of V element during charging 5+ To V 4+ Then from V 4+ Directly change to V 2+ No V in the middle process 3+ Is proved to be KVS 4 V of N-TG positive electrode material 2+ /V 4+ 、V 4+ /V 5+ The reaction process further proves that the multi-electron reaction process occurs in the KVS 4 and/N-TG positive electrode material.
The prepared KVS 4 And (3) taking the N-TG as a magnesium ion battery anode material, taking the polished magnesium foil as a cathode material, taking a glass fiber filter membrane as a diaphragm of the magnesium ion battery, taking 0.4M APC-THF as an electrolyte, and assembling the button cell in a glove box filled with high-purity argon. Standing the assembled magnesium ion battery for 24 hours, and then performing 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 and 1A g -1 。
The obtained magnesium ion battery anode material KVS 4 N-TG at a current density of 0.05A g -1 At the time, 190mAh g was exhibited -1 Is shown (fig. 5). At a current density of 1A g -1 When KVS 4 The positive electrode material of the N-TG magnesium ion battery showed excellent cycle stability after 2000 cycles with a capacity retention of nearly 100% (FIG. 6).

Claims (3)

1. K (K) + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 N-TG, characterized by the following preparation process:
ammonium metavanadate is dissolved in water under magnetic stirring at 60 ℃ to prepare an aqueous solution with the concentration of 0.167M; weighing excessive thioacetamide and dissolving in glycol with the volume equal to that of the aqueous solution; the two solutions are completely mixed and then transferred to a reaction kettle together with a carbon sheet growing with N-TG, the reaction is carried out for 4 hours at 180 ℃, after the reaction is finished, deionized water and absolute ethyl alcohol are respectively used for cleaning the carbon sheet for 3 times, and the carbon sheet is dried in vacuum; electrochemical method is adopted at 20mA cm –2 Is of the current density of (1)Degree, in the voltage range of 0 to 1.2V, K with concentration of 1M 2 SO 4 K in solution + Pre-embedding, washing the sample with deionized water for 3 times after the reaction, and vacuum drying to obtain K + Pre-embedded magnesium ion battery anode material KVS 4 /N-TG；
The obtained magnesium ion battery anode material KVS 4 The N-TG is assembled into a button magnesium ion battery, the voltage window of the electrochemical performance test is 0.2-2.1V, and the current density is 0.05 and 1A g -1 。
2. A K according to claim 1 + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 N-TG characterized by K + The pre-embedding can not only play a role of a 'pillar' to maintain structural stability, but also induce multiple electron reactions.
3. A K according to claim 1 + Magnesium ion battery anode material KVS capable of inducing multi-electron reaction through pre-embedding 4 N-TG, characterized in that when the obtained material is used as the positive electrode of a magnesium ion battery, the current density is 0.05A g -1 When the specific capacity is stabilized at 190mAh g -1 Left and right; at 1A g -1 KVS at current density 4 After 2000 cycles of/N-TG, the capacity retention was approximately 100%.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111029172A (en) * 2019-12-31 2020-04-17 青岛科技大学 Two-dimensional layered supercapacitor electrode material Ti3C2Interlayer structure regulation and control method of MXene
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111029172A (en) * 2019-12-31 2020-04-17 青岛科技大学 Two-dimensional layered supercapacitor electrode material Ti3C2Interlayer structure regulation and control method of MXene
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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Alkali ions pre-intercalated layered vanadium oxide nanowires for stable magnesium ions storage;Han Tang;《Nano Energy》;20190116;第347-354页 *

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