A method for controlling lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers and its preparation

CN116581233BActive Publication Date: 2026-08-21YANTAI UNIV
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Patent Information

Application Number
CN202310597286.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-23
Publication Date
2026-08-21
Estimated Expiration
2043-05-23

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Technical Problem

[0004]尽管有关硒化钼作为锂电池负极材料一系列研究已经取得较大进展,但目前包括上述提及的文献和专利在内的大部分研究还存在制备工艺较为复杂,材料制备成本较高,量产难度较大等问题,因此限制了硒化钼在商业化中的进一步应用

Benefits of technology

[0028](1)制备方法简单、可量产、可控性强,经多次试验验证,该方法制备的电极材料形貌与电化学性能具有良好的重复性,且循环性能、倍率性能等电化学性能优异。

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Abstract

A kind of 1T / 2H MoSe2 nanoflower regulated lithium ion battery negative material and preparation method, configuration contains molybdenum base and selenium precursor solution, and join reducing agent, mix stirring to completely dissolved, the solution is transferred to autoclave and heated, obtain precursor solution;The liquid centrifugation of precursor, remove the upper solution, after washing repeatedly, centrifugal drying, prepared 2H MoSe2 nanoflower (MS);The obtained precursor powder is ultrasonically treated, again transferred to autoclave and heated, obtain 1T / 2H MoSe2 nanoflower regulated lithium ion battery negative material.The present application can significantly improve the conductivity, realize phase and defect synergistic optimization to improve the conductivity of material, and relieve the volume change of MoSe2 in the process of charge and discharge, improve the cycle stability of material.The present application has the characteristics of low preparation cost, simple process, mass production, and stable cycle performance, excellent rate performance.
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Description

Technical Field

[0001] This invention belongs to the field of lithium-ion battery technology, and specifically relates to a method for controlling lithium-ion battery anode materials using 1T / 2HMoSe2 nanoflowers. Background Technology

[0002] Among numerous lithium-ion battery anode materials, transition metal dihalogen compounds have been extensively studied due to their complex and varied phase and electronic structures, abundant elemental reserves, and excellent photoelectric properties. With the increasingly tense global energy situation, the research on lithium-ion battery anode materials with high specific capacity and high power density is becoming increasingly urgent, providing broad development space for the research of transition metal dihalogen compounds. Among various transition metal dihalogen compounds, molybdenum selenide (MoSe2) stands out due to its high theoretical specific capacity (422 mAh g / g). -1 Molybdenum dioxide (MoO2), a transition metal dihalogen compound, possesses excellent electronic conductivity, superior ion transport properties, and high catalytic activity, making it a highly promising anode material for lithium-ion batteries. However, MoO2 still has some limitations. During charge and discharge, significant volume changes lead to particle pulverization or agglomeration, causing mechanical breakage of the battery and consequently affecting its electrochemical performance. These shortcomings will hinder the commercial application of MoO2 as a lithium-ion battery anode material.

[0003] Numerous studies have shown that nanostructuring MoSe2 particles and combining them with conductive materials such as graphene, carbon nanotubes, and biomass carbon can significantly improve the electrochemical performance of MoSe2 as a negative electrode material for lithium-ion batteries. For example, Vikraman et al. (Dhanasekaran Vikraman, Sajjad Hussain, K. Prasanna, K. Karuppasamy, Jongwan Jung, Hyun-Seok Kim, Facile method to synthesis hybrid phase 1T@2H MoSe2 nanostructures for rechargeable lithium ion batteries[J]. Journal of Electroanalytical Chemistry 2019, 833, 333-339.) designed a simple and economical one-step method to synthesize a nanoparticle honeycomb structure (1T@2H MoSe2) at 0.1 A g. -1 At a current density, the capacity remains at 843 mAh g after 100 cycles. -1Hyeongi et al. from Gachon University (Hyeongi Kima, Quoc Hai Nguyen, Tae Kim, Jaehyun Hur, Scalable synthesis of high-performance molybdenum diselenide-graphite nanocomposite anodes for lithium-ion batteries[J]. Applied Surface Science 2021, 481, 1196-1205.) prepared a MoSe2-graphite nanocomposite material as a new high-performance lithium-ion battery anode through high-energy mechanical milling. At 100 mA g -1 It can maintain 909mAh g after 100 cycles at current density. -1 It has a high specific capacity and also exhibits ultra-long cycling performance, namely at 3.0 A g. -1 It can maintain 611 mAh g after cycling at current density -1 Specific capacity.

[0004] Although significant progress has been made in a series of studies on molybdenum selenide as a negative electrode material for lithium batteries, most of the current research, including the aforementioned literature and patents, still faces challenges such as complex preparation processes, high material preparation costs, and difficulties in mass production. These limitations restrict the further commercial application of molybdenum selenide. Summary of the Invention

[0005] In order to overcome the problems existing in the prior art, the purpose of this invention is to provide a method for controlling lithium-ion battery anode materials using 1T / 2HMoSe2 nanoflowers, which has the characteristics of low preparation cost, simple process, mass production capability, stable cycle performance and excellent rate performance.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0007] A lithium-ion battery anode material is developed using 1T / 2H MoSe2 nanoflowers. The material exhibits a circular nanoflower-like structure composed of nanosheets ranging from 380nm to 400nm. This layered flower-like structure possesses multidimensional channels, and the layered nanoflower-like structure is doped with MoSe2 in a specific 1T / 2H phase ratio. This significantly promotes rapid electron diffusion and increases the number of catalytic active centers, providing ample space for storing discharge products. This also helps mitigate the volume changes caused by lithium-ion insertion / extraction, improving the material's cycle stability. The mixed structure of the 1T and 2H phases synergistically enhances the catalytic activity for redox reactions and greatly improves the mobility of interfacial charges, resulting in significantly enhanced conductivity and a substantial increase in the material's theoretical specific capacity. The synergistic effect of the nanoflower-like structure, the 1T phase, and the 2H phase contributes to stable cycle performance and excellent rate performance in the final product.

[0008] The electrode material is used at a current density of 0.1 A g. -1 After 100 cycles, the specific capacity reached 886.1 mAh g. -1 The coulombic efficiency remains at 98%; and / or the current density is 1.0 A g. -1 After 1105 cycles, the highest specific capacity reached 1272.0 mAh g. -1 Coulomb efficiency remains above 99%.

[0009] A method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers includes the following steps;

[0010] (1) Prepare a molybdenum-based and selenium-based precursor solution, add a reducing agent, mix and stir until completely dissolved, transfer the solution to an autoclave and heat to obtain the precursor solution;

[0011] (2) The precursor liquid was centrifuged to remove the supernatant solution. After washing several times, it was centrifuged and dried to obtain 2H MoSe2 nanoflowers (MS).

[0012] (3) After ultrasonic treatment of the precursor powder obtained in step (2), it is transferred to a high-pressure autoclave for heating again to obtain 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material.

[0013] Furthermore, in step (1), when preparing the solution, the solvent is high-purity water or deionized water, and the volume is 28 ml.

[0014] Furthermore, in step (1), the molybdenum-based precursor is sodium molybdate, but it is not limited to sodium molybdate; other molybdenum salts can also be used to prepare the precursor.

[0015] Furthermore, in step (1), the selenium-containing precursor is selenium dioxide, but it is not limited to selenium dioxide. Selenite, selenite acid, selenium-enriched yeast and other selenium-containing precursors can also be used.

[0016] Furthermore, in step (1), the mass ratio of ammonium molybdate providing molybdenum and selenium dioxide providing selenium is 1:1.

[0017] Furthermore, in step (1), the magnetic stirring speed is 2000-9000 rpm, and the stirring time is 15-20 minutes.

[0018] Furthermore, in step (1), the high-pressure vessel is a 50ml high-pressure reactor, and the heating temperature is 180-220℃, preferably 190-210℃, and more preferably 200℃;

[0019] Furthermore, in step (1), the heating time is 24-40 hours, preferably 30-38 hours, and more preferably 36 hours.

[0020] Furthermore, in step (2), the prepared MS precursor is centrifuged and separated using a centrifuge, and then washed with deionized water and alcohol. The centrifugation speed is 8000-9000 rpm.

[0021] Furthermore, in step (2), the drying temperature is 60°C and the drying time is 12 hours.

[0022] Furthermore, in step (3), the precursor powder is sonicated in anhydrous ethanol for 20 minutes.

[0023] Furthermore, in step (3), the high-pressure vessel is a 50ml high-pressure reactor, and the heating temperature is 200-240℃, preferably 220℃;

[0024] Furthermore, in step (3), the heating time is 3-20 hours, preferably 5-15 hours.

[0025] Furthermore, the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material is used to prepare lithium-ion batteries.

[0026] The beneficial effects of the present invention.

[0027] This invention utilizes a one-step hydrothermal synthesis strategy to prepare partially crystalline 2H-MoSe2 nanosheets. Excess hydrazine hydrate is used as a reducing agent, and the electron injection effect of hydrazine hydrate on MoSe2 during the hydrothermal reaction induces the formation of a 1T phase MoSe2. Simultaneously, by adjusting the temperature of the secondary hydrothermal reaction, the degree of defects in the 1T / 2H MoSe2 nanoflowers is effectively controlled, achieving synergistic optimization of phase and defects to improve the material's conductivity. Combined with centrifugal drying and subsequent hydrothermal processes, a 1T / 2HMoSe2 nanoflower-controlled lithium-ion battery anode material is prepared. Compared with traditional materials, this material's layered nanoflower structure provides more ion transport channels, mitigating the volume change of MoSe2 during charge and discharge, and improving the material's cycle stability. Due to its unique two-phase doped structure, it exhibits excellent electrochemical performance. Compared with existing research, the advantages of electrode materials prepared using hydrothermal methods and centrifugal drying are:

[0028] (1) The preparation method is simple, mass-producible and highly controllable. After multiple experiments, the electrode material prepared by this method has good repeatability in terms of morphology and electrochemical performance, and excellent electrochemical performance such as cycle performance and rate performance.

[0029] (2) MoSe2 nanoflowers with different 1T / 2H ratios were prepared to control the anode material of lithium-ion batteries by simply adjusting the temperature.

[0030] (3) The 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention has low material cost and low industrialization cost in the process of preparing finished batteries. At the same time, the process is simple and suitable for large-scale production. Attached image description:

[0031] Figure 1 This is a SEM image of the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention.

[0032] Figure 2 This is a TEM image of the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention.

[0033] Figure 3 The XRD test results are for the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention.

[0034] Figure 4 These are the XPS test results of the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention.

[0035] Figure 5This is a rate performance diagram of the 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material prepared by the method of this invention.

[0036] Figure 6 0.1A g of the composite electrode material of this invention -1 Current density cyclic graph. Detailed Implementation

[0037] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0038] Example 1

[0039] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0040] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0041] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0042] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0043] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0044] (5) After heating at 220℃ for 5 hours, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS-5.

[0045] Figure 1 SEM images of 1T / 2H MoSe2 nanoflower-modulated lithium-ion battery anode materials, obtained by... Figure 1 The MoSe2 material synthesized by this invention was found to have a layered nanoflower-like structure; Figure 2 The TEM image of the lithium-ion battery anode material controlled by 1T / 2H MoSe2 nanoflowers shows that there are two different crystal structures, representing the presence of the 1T phase and the 2H phase, respectively. Figure 3 The XRD pattern of the lithium-ion battery anode material regulated by 1T / 2H MoSe2 nanoflowers is shown. Comparison with the standard card shows that the phase of the obtained product is MoSe2. Figure 4 XPS test results of 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials prepared at different temperatures by the method of the present invention demonstrate that the 1T / 2H phase ratio in the material can be effectively changed by altering the secondary hydrothermal temperature.

[0046] The lithium-ion battery anode material regulated by the 1T / 2H MoSe2 nanoflowers obtained in Specific Implementation Case 1 was used to fabricate an electrode according to the following method:

[0047] Weigh 1T / 2HMoSe2 nanoflower-modified lithium-ion battery anode material, Super P, and tetrafluoroethylene in a mass ratio of 7:2:1. After mixing evenly, add 10-15 drops of N-methylpyrrolidone and continue grinding for 1-2 hours. Coat the mixture evenly onto copper foil with a spatula to form an electrode, and dry it. Use lithium metal sheet as the positive electrode and 1 mol L⁻¹ electrolyte. -1 The LiPF6 / EC-DMC, with a polypropylene microporous membrane as the separator, is assembled into a 2032 half-cell. Figure 5 Rate performance of a half-cell; Figure 6 The half-cell was tested at a current density of 0.1 A g. -1 The present invention utilizes 1T / 2HMoSe2 nanoflowers to regulate the cycling performance of lithium-ion battery anode materials in the range of 0.1-20 A g. -1 It exhibits excellent rate performance within the current density range; at a current density of 0.1 A g -1 After 100 cycles, the specific capacity reaches 886.1 mAh g. -1 The coulombic efficiency remains at 98%; at a current density of 1.0 A g -1 After 1105 cycles, the highest specific capacity reached 1272.0 mAh g. -1 Coulomb efficiency remains above 99%.

[0048] Example 2

[0049] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0050] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0051] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0052] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0053] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0054] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS-10.

[0055] Example 3

[0056] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0057] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0058] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0059] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0060] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0061] (5) After heating at 220℃ for 15h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS-15.

[0062] Example 4

[0063] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0064] (1) Dissolve 0.1332gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0065] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0066] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0067] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0068] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS'-10.

[0069] Example 5

[0070] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0071] (1) Dissolve 0.1554gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0072] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0073] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0074] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0075] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS'-10.

[0076] Example 6

[0077] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0078] (1) Dissolve 0.111gSeO2 and 0.1272gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0079] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0080] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0081] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0082] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS'-10.

[0083] Example 7

[0084] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0085] (1) Dissolve 0.111gSeO2 and 0.1484gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0086] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 200°C for 36 hours.

[0087] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0088] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0089] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS'-10.

[0090] Example 8

[0091] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0092] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0093] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 180°C for 36 h.

[0094] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0095] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0096] (5) After heating at 220℃ for 5 hours, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS”-5.

[0097] Example 9

[0098] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0099] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0100] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 180°C for 36 h.

[0101] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0102] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0103] (5) After heating at 220℃ for 10h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS”-10.

[0104] Example 10

[0105] The preparation steps for 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode materials are as follows:

[0106] (1) Dissolve 0.111gSeO2 and 0.106gNa2MoO4·2H2O in 28ml of deionized water under vigorous stirring;

[0107] (2) Add 1.5 ml of hydrazine hydrate solution to the solution obtained in step (1) and continue stirring for 15 minutes. After stirring, transfer the solution to a 50 ml autoclave lined with polytetrafluoroethylene and keep it at 180°C for 36 h.

[0108] (3) After heating, the solution was placed in a centrifuge tube and centrifuged to get the black precipitate. The precipitate was washed three times with ethanol and deionized water and then dried at 60°C for 12 hours to obtain the MS black powder precursor.

[0109] (4) Weigh 60mg MS and sonicate it in 30ml alcohol for 20min, then transfer it to a 50ml autoclave lined with polytetrafluoroethylene.

[0110] (5) After heating at 220℃ for 15h, 1T / 2H MoSe2 nanoflowers were obtained and labeled as MS”-15.

Claims

1. A method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers, characterized in that, Includes the following steps; (1) Prepare a molybdenum-based and selenium-based precursor solution, add a reducing agent, mix and stir until completely dissolved, transfer the solution to an autoclave and heat to obtain the precursor solution; (2) The precursor liquid was centrifuged to remove the supernatant solution. After washing several times, it was centrifuged and dried to obtain 2H MoSe2 nanoflower MS. (3) After ultrasonic treatment of the precursor powder obtained in step (2), it is transferred to the autoclave again for heating to obtain 1T / 2HMoSe2 nanoflower-regulated lithium-ion battery anode material. A lithium-ion battery anode material is controlled by 1T / 2H MoSe2 nanoflowers. The material presents a circular nanoflower structure composed of nanosheets. The layered flower structure has multidimensional channels, and 1T / 2H MoSe2 is doped on the layered nanoflower structure. The negative electrode material operates at a current density of 0.1 A·g -1 After 100 cycles, the specific capacity reached 886.1 mAh·g. -1 The coulombic efficiency remains at 98%; and / or the current density is 1.0 A·g. -1 After 1105 cycles, the highest specific capacity reached 1272.0 mAh·g. -1 Coulomb efficiency remains above 99%.

2. The method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers according to claim 1, characterized in that, In step (1), when preparing the solution, the solvent is high-purity water or deionized water, and the volume is 28 ml.

3. The method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers according to claim 1, characterized in that, In step (1), the molybdenum-based precursor is sodium molybdate; In step (1), the selenium-containing precursor is selenium dioxide, selenite, selenite acid, or selenium-enriched yeast.

4. The method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers according to claim 1, characterized in that, In step (1), the stirring rate is 2000~9000 rpm and the stirring time is 15-20 minutes; In step (1), the high-pressure vessel is a 50ml high-pressure reactor with a heating temperature of 180-220℃; In step (1), the heating time is 24-40 hours.

5. The method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers according to claim 1, characterized in that, In step (2), the prepared MS precursor is centrifuged and separated using a centrifuge, and then washed with deionized water and alcohol. The centrifugation speed is 8000-9000 rpm. In step (2), the drying temperature is 60°C and the drying time is 12 hours.

6. The method for preparing lithium-ion battery anode materials using 1T / 2H MoSe2 nanoflowers according to claim 1, characterized in that, In step (3), the precursor powder is sonicated in anhydrous ethanol for 20 minutes. In step (3), the high-pressure vessel is a 50ml high-pressure reactor with a heating temperature of 200-240℃; In step (3), the heating time is 3-20 hours.

7. The lithium-ion battery anode material prepared by the method according to any one of claims 1-6, characterized in that, The 1T / 2H MoSe2 nanoflower-regulated lithium-ion battery anode material is used to prepare lithium-ion batteries.