CN111261873A - N-MnO2Preparation and application of/S composite material - Google Patents

N-MnO2Preparation and application of/S composite material Download PDF

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CN111261873A
CN111261873A CN202010088220.XA CN202010088220A CN111261873A CN 111261873 A CN111261873 A CN 111261873A CN 202010088220 A CN202010088220 A CN 202010088220A CN 111261873 A CN111261873 A CN 111261873A
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mno
composite material
nanospheres
prepare
deionized water
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刘守法
何子游
乔勋
何绍元
洪哲
胡希禹
黄箫
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Xijing University
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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/624—Electric conductive fillers
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
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  • Composite Materials (AREA)
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Abstract

N-MnO2The preparation method of the/S composite material comprises the steps of firstly preparing KMnO4Dissolving in deionized water and stirring, then dripping ammonia water and standing, collecting solid precipitate and washing with deionized water for several times to obtain MnO2Nanospheres; then MnO is added2The nanospheres are heated in nitrogen atmosphere and naturally cooled to room temperature to prepare N-doped MnO2Nanospheres; finally, MnO of N doping2Uniformly mixing the nanospheres with pure sulfur, heating in argon atmosphere, and preserving heat to prepare N-MnO2(ii) a/S composite; the application is to use N-MnO2The button cell is assembled by taking the/S composite material as the anode material and tested, and the electrochemical results show that,prepared N-MnO2the/S composite material has small resistance and good conductivity; the circulation stability is good; the specific capacity is large.

Description

N-MnO2Preparation and application of/S composite material
Technical Field
The invention relates to the technical field of lithium-sulfur batteries, in particular to N-MnO2Preparation and application of the/S composite material.
Background
In the past decades, researchers developed energy storage systems including lithium ion batteries, lithium sulfur batteries, lithium metal batteries, and the like, and applied to electric vehicles, unmanned aerial vehicles, and large storage devices, the lithium sulfur batteries have attracted extensive attention of researchers in various countries around the world. It is well known that lithium sulfur batteries have many advantages: the specific capacity is high (1675mAh/g), which is 5 times of that of the traditional anode material; a more excellent energy density (2600 WhK/g); the sulfur has no pollution to the environment, rich reserves and low cost. Therefore, the research on the positive electrode material and the negative electrode protection of the lithium battery is of great significance.
However, to date, lithium sulfur batteries have not been widely used in electronic devices, which is mainly caused by the following disadvantages: firstly, in the process of charging and discharging, the utilization rate of active substances is low due to poor conductivity; secondly, the discharge products are easily dissolved in the electrolyte, thereby creating a shuttling effect. As a result, the prepared lithium-sulfur battery has poor cycle performance and low specific capacity. To solve these problems, many methods have been used, including finding suitable sulfur host materials, developing new anode materials, and designing new functional interlayer materials between the anode material and the separator.
The modified lithium anode can avoid the formation of lithium dendrites and prevent the short circuit of the lithium sulfur battery, and the functional interlayer is favorable for preventing polysulfide from migrating from the anode to the cathode.
The existing sulfur host material has the defects of high resistance and poor conductivity of a composite material; the cycling stability of the composite material is poor; the specific capacity of the composite material is small.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide N-MnO2The preparation and application of the/S composite material are realized, and the prepared composite material is small in resistance and good in conductivity; the circulation stability is good; the specific capacity is large.
In order to achieve the purpose, the invention adopts the technical scheme that:
N-MnO2The preparation method of the/S composite material comprises the following steps:
(1) hydrothermal synthesis of MnO2Nanosphere: 0.8-1.3 g KMnO4Dissolving in 50ml of deionized water, stirring for 30-50 min, then dripping 1-2 ml of ammonia water, standing for 1-3 h, collecting solid precipitate, and washing for 3-5 times by using deionized water to obtain MnO2Nanospheres;
(2) preparation of N-doped MnO2Nanosphere: MnO of2Heating the nanospheres in a nitrogen atmosphere at 190-220 ℃ for 20-40 minutes, and naturally cooling the nanospheres in nitrogen to room temperature to prepare N-doped MnO2Nanospheres;
(3) preparation of N-MnO2The composite material of/S: MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1 (3-5), heating to 150-160 ℃ in an argon atmosphere, and preserving heat for 12-14 hours to prepare N-MnO2a/S composite material.
The N-MnO2Use of/S composite materials with N-MnO2the/S composite material is used as the anode material to assemble the button cell and is tested, and the electrochemical result shows that N-MnO is2The initial specific capacity of the/S composite material at 0.2C is up to 1118 mAh/g; after 500 cycles, N-doped MnO2The capacity of the/S composite material at 1C is kept at 810 mAh/g.
The invention has the advantages that: metal oxides are considered to be the best host material for application to sublimed sulphur. The shuttle effect of lithium-sulfur batteries can be greatly suppressed by using metal oxides as host materials due to the presence of specific chemical bonds between the metal oxides and polysulfides.
The invention successfully prepares the N-doped MnO by a hydrothermal reaction method2Nanospheres, then compounding with sulfur to prepare nitrogen-doped MnO2(N-MnO) composite material2/S) for use in a positive electrode material for a lithium-sulfur battery. Due to the existence of the N-doped nanospheres, the cycling stability and the specific capacity of the lithium-sulfur battery are greatly improved. N-MnO2The initial specific capacity of the/S composite material at 0.2C is up to 1118 mAh/g. After 500 cycles, N-MnO2The capacity of the/S composite material at 1C is kept at 810 mAh/g.
Drawings
FIG. 1 shows N-MnO prepared in example 22SEM microscopic appearance of the/S composite material.
FIG. 2 shows N-MnO prepared in example 22TEM morphology of the/S composite.
FIG. 3 shows N-MnO prepared in example 22Element distribution diagram of the/S composite material.
FIG. 4 shows MnO prepared in example 22、N-MnO2、N-MnO2Comparing XRD patterns of the/S composite material and pure sulfur.
FIG. 5 shows N-MnO prepared in example 22(ii) composite material and MnO2Constant current charge and discharge curve of the/S electrode.
FIG. 6N-MnO prepared in example 22(ii) a/S composite, pure sulphur and MnO2Comparative plot of the rate performance of the/S electrode.
FIG. 7N-MnO prepared in example 22(ii) a/S composite, pure sulphur and MnO2Electrochemical impedance spectrum of the/S electrode.
FIG. 8N-MnO prepared in example 22(ii) a/S composite, pure sulphur and MnO2Long-term cycling performance curve of the/S electrode.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1 an N-MnO2The preparation method of the/S composite material comprises the following steps:
(1)0.8g KMnO4dissolving in 50ml deionized water and stirring for 40min, then dripping 1ml ammonia water and standing for 3h, collecting solid precipitate and washing with deionized water for 5 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 20 minutes in nitrogen atmosphere at 200 ℃, and then naturally cooled to room temperature in nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:3, heating to 150 ℃ in an argon atmosphere, and preserving heat for 13 hours to prepare N-MnO2a/S composite material.
Example 2 an N-MnO2The preparation method of the/S composite material comprises the following steps:
(1)1.3g KMnO4dissolving in 50ml deionized water and stirring for 30min, then dripping 1.5ml ammonia water and standing for 2h, collecting solid precipitate and washing with deionized water for 4 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 40 minutes at 190 ℃ in nitrogen atmosphere, and then naturally cooled to room temperature in nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:5, heating to 160 ℃ in an argon atmosphere, and preserving heat for 14 hours to prepare N-MnO2a/S composite material.
Example 3 an N-MnO2The preparation method of the/S composite material comprises the following steps:
(1)1.0g KMnO4dissolving in 50ml deionized water and stirring for 50min, then dripping 2ml ammonia water and standing for 1h, collecting solid precipitate and washing with deionized water for 3 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 30 minutes in the nitrogen atmosphere at 220 ℃, and then naturally cooled to room temperature in the nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:4, heating to 155 ℃ in an argon atmosphere, and preserving heat for 12 hours to prepare N-MnO2a/S composite material.
For the composite material prepared in the embodiment 2 of the present invention, the scanning electron microscope and the transmission electron microscope are adopted to perform microscopic structure observation, and the results are as follows:
FIG. 1 shows N-MnO prepared in example 22The SEM microscopic appearance of the/S composite material shows that the structure is a spherical structure with the diameter of about 100nm, and the size of the nanospheres is uniform; FIG. 2 shows N-MnO prepared in example 22The TEM appearance of the/S composite material shows that the surfaces of the nanosphere structures with the diameters of about 100nm are rough, which provides conditions for adsorbing polysulfide; FIG. 3 shows N-MnO prepared in example 22The elemental profile of the/S composite material clearly shows that the elements N, Mn, O and S are uniformly dispersed in the composite material.
As shown in FIG. 4, MnO2Typical diffraction peaks appear at 25 °, 38 °, 46 ° and 53 °, corresponding to the (111), (110), (210) and (011) crystal planes, showing relatively pure MnO2The crystal structure of (a); N-MnO prepared in example 22MnO with N-doped-/S composite material2And diffraction peaks of pure sulfur, indicating that elemental sulfur has been incorporated into N-MnO2In nanospheres.
The N-MnO prepared in example 22the/S composite material was used as the positive electrode and assembled into 2032 button cells to test the electrochemical performance of the electrode. With N-MnO as prepared in example 22the/S composite material is used as a positive electrode, the lithium foil is used as a negative electrode, the Clegard2300 polypropylene film is used as a diaphragm, a 2032 type button cell is prepared in an Ar-gas-filled glove box, 1mol/L LiPF6 solution is selected as electrolyte, and the volume ratio of EC to DEC is 1: 1. The discharge and charge curves of the cell were obtained using the novyi electrochemical tester, and the electrochemical impedance spectra of the button cell were obtained using an electrochemical workstation model CHI 660E.
FIG. 5 shows N-MnO prepared in example 22(ii) composite material and MnO2The constant current charge and discharge curve of the/S electrode shows that the N-MnO prepared in example 22The initial specific capacities of the/S composite material electrode at 0.2C, 0.5C, 1C, 2C and 4C are 1118mAh/g, 926mAh/g, 798mAh/g, 625mAh/g and 528mAh/g respectively. For MnO prepared2The initial specific capacity at 0.2C of the/S composite electrode was only 786mAh/g, indicating that the N-MnO prepared in example 2 was2Electrode ratio MnO of/S composite material2Electrode made of/S composite materialHas higher specific capacity.
Referring to FIG. 6, FIG. 6 shows pure sulfur, N-MnO prepared in example 2, respectively2(ii) composite material and MnO2Rate capability of the/S electrode. The results show that the N-MnO prepared in example 22the/S composite material electrode has good rate capability. For pure sulfur and MnO2The capacity of the/S electrode decays rapidly as the current density increases.
Referring to FIG. 7, the impedance spectrum curve of the electrochemical impedance spectrum of the material consists of a high frequency semicircle and a low frequency straight line, and it is apparent that N-MnO prepared in example 22the/S composite electrode showed a smaller conductive resistance than the other electrodes, indicating that the electrode had better conductivity,
referring to FIG. 8, FIG. 8 shows the long cycle performance of the electrode at 1C, and it can be seen that after 500 cycles, the N-MnO prepared in example 22The capacity of the/S composite remained at 810mAh/g after 500 cycles at 1C, however for pure sulfur and MnO2the/S electrode, during electrochemical cycling, suffers from severe capacity fade.

Claims (5)

1. N-MnO2The preparation method of the/S composite material is characterized by comprising the following steps:
(1) hydrothermal synthesis of MnO2Nanosphere: 0.8-1.3 g KMnO4Dissolving in 50ml of deionized water, stirring for 30-50 min, then dripping 1-2 ml of ammonia water, standing for 1-3 h, collecting solid precipitate, and washing for 3-5 times by using deionized water to obtain MnO2Nanospheres;
(2) preparation of N-doped MnO2Nanosphere: MnO of2Heating the nanospheres in a nitrogen atmosphere at 190-220 ℃ for 20-40 minutes, and naturally cooling the nanospheres in nitrogen to room temperature to prepare N-doped MnO2Nanospheres;
(3) preparation of N-MnO2The composite material of/S: MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1 (3-5), heating to 150-160 ℃ in an argon atmosphere, and preserving heat for 12-14 hours to prepare N-MnO2a/S composite material.
2. N-MnO prepared according to the method of claim 12The application of the/S composite material is characterized in that: using N-MnO2the/S composite material is used as the anode material to assemble the button cell and is tested, and the electrochemical result shows that N-MnO is2The initial specific capacity of the/S composite material at 0.2C is up to 1118 mAh/g; after 500 cycles, N-doped MnO2The capacity of the/S composite material at 1C is kept at 810 mAh/g.
3. An N-MnO according to claim 12The preparation method of the/S composite material is characterized by comprising the following steps:
(1)0.8g KMnO4dissolving in 50ml deionized water and stirring for 40min, then dripping 1ml ammonia water and standing for 3h, collecting solid precipitate and washing with deionized water for 5 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 20 minutes in nitrogen atmosphere at 200 ℃, and then naturally cooled to room temperature in nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:3, heating to 150 ℃ in an argon atmosphere, and preserving heat for 13 hours to prepare N-MnO2a/S composite material.
4. An N-MnO according to claim 12The preparation method of the/S composite material is characterized by comprising the following steps:
(1)1.3g KMnO4dissolving in 50ml deionized water and stirring for 30min, then dripping 1.5ml ammonia water and standing for 2h, collecting solid precipitate and washing with deionized water for 4 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 40 minutes at 190 ℃ in nitrogen atmosphere, and then naturally cooled to room temperature in nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:5, and then carrying out argon atmosphereHeating to 160 ℃ in the middle, and preserving the heat for 14h to prepare N-MnO2a/S composite material.
5. An N-MnO according to claim 12The preparation method of the/S composite material is characterized by comprising the following steps:
(1)1.0g KMnO4dissolving in 50ml deionized water and stirring for 50min, then dripping 2ml ammonia water and standing for 1h, collecting solid precipitate and washing with deionized water for 3 times to obtain MnO2Nanospheres;
(2) MnO of2The nanosphere is heated for 30 minutes in the nitrogen atmosphere at 220 ℃, and then naturally cooled to room temperature in the nitrogen to prepare N-doped MnO2Nanospheres;
(3) MnO doping N2Uniformly mixing the nanospheres and the pure sulfur according to the mass ratio of 1:4, heating to 155 ℃ in an argon atmosphere, and preserving heat for 12 hours to prepare N-MnO2a/S composite material.
CN202010088220.XA 2020-02-12 2020-02-12 N-MnO2Preparation and application of/S composite material Pending CN111261873A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657529A (en) * 2020-12-24 2021-04-16 广东工业大学 Nitrogen-doped modified manganese dioxide catalyst and preparation method thereof
CN113937278A (en) * 2021-10-15 2022-01-14 北京化工大学 Sulfur anion doped manganese dioxide material, preparation and application thereof, and zinc ion battery comprising sulfur anion doped manganese dioxide material
CN115337935A (en) * 2022-07-26 2022-11-15 北方民族大学 Cu-MnO with high catalytic activity 2 Nano catalyst, preparation method and application thereof, and printing and dyeing wastewater treatment method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106941161A (en) * 2017-04-05 2017-07-11 深圳市佩成科技有限责任公司 A kind of preparation method of nitrogen-doped graphene/manganese dioxide/hollow sulphur composite
CN106972168A (en) * 2017-05-17 2017-07-21 哈尔滨工业大学 A kind of preparation method and application of the manganese dioxide containing Lacking oxygen/sulphur composite
CN109309216A (en) * 2018-08-20 2019-02-05 中国航发北京航空材料研究院 A kind of preparation method of lithium sulfur battery anode material
CN110165185A (en) * 2019-06-03 2019-08-23 南京邮电大学 A kind of preparation method and application of lithium sulfur battery anode material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106941161A (en) * 2017-04-05 2017-07-11 深圳市佩成科技有限责任公司 A kind of preparation method of nitrogen-doped graphene/manganese dioxide/hollow sulphur composite
CN106972168A (en) * 2017-05-17 2017-07-21 哈尔滨工业大学 A kind of preparation method and application of the manganese dioxide containing Lacking oxygen/sulphur composite
CN109309216A (en) * 2018-08-20 2019-02-05 中国航发北京航空材料研究院 A kind of preparation method of lithium sulfur battery anode material
CN110165185A (en) * 2019-06-03 2019-08-23 南京邮电大学 A kind of preparation method and application of lithium sulfur battery anode material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657529A (en) * 2020-12-24 2021-04-16 广东工业大学 Nitrogen-doped modified manganese dioxide catalyst and preparation method thereof
CN113937278A (en) * 2021-10-15 2022-01-14 北京化工大学 Sulfur anion doped manganese dioxide material, preparation and application thereof, and zinc ion battery comprising sulfur anion doped manganese dioxide material
CN115337935A (en) * 2022-07-26 2022-11-15 北方民族大学 Cu-MnO with high catalytic activity 2 Nano catalyst, preparation method and application thereof, and printing and dyeing wastewater treatment method
CN115337935B (en) * 2022-07-26 2024-01-23 北方民族大学 Cu-MnO with high catalytic activity 2 Nano catalyst, preparation method and application thereof, and printing and dyeing wastewater treatment method

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