CN113394387A - Preparation method of novel composite material for positive electrode of lithium-sulfur battery - Google Patents
Preparation method of novel composite material for positive electrode of lithium-sulfur battery Download PDFInfo
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- CN113394387A CN113394387A CN202110645567.4A CN202110645567A CN113394387A CN 113394387 A CN113394387 A CN 113394387A CN 202110645567 A CN202110645567 A CN 202110645567A CN 113394387 A CN113394387 A CN 113394387A
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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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- 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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Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a novel composite material for a lithium-sulfur battery anode. The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery comprises the following steps: (1) preparing Co-LDH; (2) preparing Co-LDH/ZIF-67. The cobalt-based LDH-coated metal-organic framework (MOFs) composite material is prepared by adopting a simple aqueous solution method. The method has the characteristics of low cost, simple preparation process and the like.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a novel composite material for a lithium-sulfur battery anode.
Background
The problems of fossil energy shortage and environmental pollution caused by the high-speed development of global industrialization become important factors for restricting the sustainable development of the current society, so that the search and the sustainability are urgently neededThe development of suitable energy substitutes is continued. Lithium ion batteries are now an energy storage device seen everywhere in daily life, however, the energy density, cycle performance and the like of currently researched lithium ion batteries cannot meet the requirements of large energy storage devices in actual production. At present, energy storage materials with higher energy density, power density and long cycle life are urgently needed, and unlike lithium ion batteries, lithium sulfur batteries taking sulfur as a positive electrode and lithium as a negative electrode have attracted much attention in recent years, and have ultrahigh theoretical specific capacity (1675 mAh. g)-1) And theoretical specific energy (2600Wh kg)-1) (ii) a Meanwhile, the sulfur has the advantages of low production cost, abundant natural reserves, good safety, no toxicity and the like.
However, the technical obstacles that currently hinder the commercial application of lithium-sulfur batteries are specifically as follows: (1) low intrinsic conductivity of sulfur; (2) lithium polysulfide (Li)2SnN is more than or equal to 4 and less than or equal to 8) is easily dissolved in the electrolyte, so polysulfide can shuttle to the surface of the anode and is easy to generate chemical reaction with the lithium anode, and finally irreversible loss of active substances and the ubiquitous phenomenon of shuttle effect are caused, and finally the coulomb efficiency is greatly reduced in the charging and discharging process; (3) from Li during charging2When S is oxidized to S, the volume expansion of the positive electrode is as high as 79%, which may destroy the electrode structure, resulting in a decrease in the cycle performance of the lithium sulfur battery cathode. Among them, limiting the shuttling effect of polysulfides and improving electron conductivity are the first tasks for further development of lithium sulfur batteries.
In order to overcome the above problems, various conductive carbon skeletons having a special morphology are widely introduced into sulfur-based composites. The carbon material not only has good conductivity, but also has large pore volume and high specific surface area, and can improve the conductivity of the sulfur-based material compounded with sulfur. However, during long-term charge/discharge cycles, polar LiPS tends to diffuse out due to its weak affinity to the non-polar carbon host. In view of this, there is a need to develop a new composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a novel composite material for a lithium-sulfur battery anode, aiming at the defects, and the cobalt-based LDH-coated metal-organic frameworks (MOFs) composite material is prepared by adopting a simple aqueous solution method. The method has the characteristics of low cost, simple preparation process and the like.
The technical scheme of the invention is as follows: a preparation method of a novel composite material for a positive electrode of a lithium-sulfur battery comprises the following steps:
(1) preparation of Co-LDH: first Co (NO)3)2Dissolving in deionized water to obtain Co (NO)3)2A solution; dissolving a mixture of 2-methylimidazole and hexadecyl trimethyl ammonium bromide in deionized water to obtain a 2-methylimidazole mixed solution; then Co (NO) is added under the condition of room temperature3)2Pouring the solution into a 2-methylimidazole mixed solution, fully stirring, centrifuging, washing, and drying the obtained product at 60 ℃ for 12 hours in vacuum;
(2) preparation of Co-LDH/ZIF-67: dispersing the Co-LDH obtained in the step (1) in deionized water to obtain a Co-LDH solution; dispersing 2-methylimidazole in deionized water to obtain a 2-methylimidazole solution; and pouring the 2-methylimidazole solution into the Co-LDH solution at room temperature, fully stirring, centrifuging, washing, and performing vacuum drying on the obtained product at 60 ℃ for 12 hours to obtain the Co-LDH/ZIF-67 composite material.
The Co-LDH/ZIF-67 composite material prepared by the preparation method is of a hollow cubic structure, has high monodispersity and has a particle size of 300-400 nm; the structure is characterized in that the ZIF-67 is encapsulated with Co-LDH, and the Co-LDH is an ultrathin nanometer wafer growing on the inner surface of the ZIF-67.
Co (NO) in the step (1)3)2Dissolving the solution in 0.0515-0.103 mmol of deionized water of 8-15 mL; 3.37-6.74 mmol of 2-methylimidazole and 0.00548mmol of hexadecyl trimethyl ammonium bromide, and mixing and dissolving the 2-methylimidazole and the hexadecyl trimethyl ammonium bromide in 8-15 mL of deionized water.
In the step (2), 1.6-3.2 mg of Co-LDH is dispersed in 5-10 mL of deionized water; 1.22-2.44 mmol of 2-methylimidazole is dispersed in 5-10 mL of deionized water.
Stirring for 20 minutes at 25 ℃ in the step (1); washed twice with deionized water and once with ethanol.
Stirring for 6 hours at 25 ℃ in the step (2); washed twice with deionized water and once with ethanol.
The invention has the beneficial effects that: the composite material prepared by the preparation method has the following excellent properties:
(1) the Co-LDH/ZIF-67 composite material has a unique core-shell heterojunction structure, has a large specific surface area and high porosity, improves the specific surface area of the composite material to a great extent, and is beneficial to improving the loading capacity of active substances.
(2) The Co-LDH/ZIF-67 composite material has layered double hydroxide, is an effective LiPSs electrocatalyst, has rich hydrophilic hydroxyl groups, has strong chemical affinity to the LiPSs, promotes the transformation kinetics of the LiPSs through enough sulphur affinity sites, has a large amount of unsaturated coordination sites, and is beneficial to immobilized single atoms by enhancing the interaction between the single atoms and a carrier, thereby being beneficial to improving the adsorption effect of the composite material on polysulfide in the electrochemical reaction process.
(3) The Co-LDH/ZIF-67 composite material has high stability. The composite material has the characteristics of structural stability and phase stability due to the high stability and reversibility of the spinel structure. High sulfur loading can be achieved and volume expansion can be accommodated, helping to mitigate the volume expansion effect of the active species during the reaction.
(4) The Co-LDH/ZIF-67 composite material has high catalytic performance. ZIF-67 is a type of Co-based metal-organic frameworks (MOFs) that has a uniform pore size distribution and an ultra-high surface area, making it a viable option to make electrocatalysts with the structural advantage of large surface area and reasonably distributed pores to improve their catalytic performance. Therefore, the conversion rate of polysulfide can be effectively promoted in the electrochemical reaction process of the lithium-sulfur battery, and the chemical adsorption effect with polysulfide is improved, so that the utilization rate and the cycle performance of active substances of the lithium-sulfur battery are enhanced.
The preparation method has the characteristics of low cost, simple preparation process and the like.
Drawings
FIG. 1 is a plot of the specific electrochemical capacity of a lithium sulfur battery using the Co-LDH/ZIF-67 composite material described in example 1 as the cathode material.
FIG. 2 is a plot of the electrochemical specific capacity of a lithium sulfur battery using the Co-LDH/ZIF-67 composite material described in example 2 as the cathode material.
Detailed Description
The present invention will be described in detail below with reference to examples.
Example 1
The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery comprises the following steps:
(1) preparation of Co-LDH: firstly, 0.0515mmolCo (NO) is added3)2Dissolving in 8mL deionized water to obtain Co (NO)3)2A solution; dissolving a mixture of 3.37mmol of 2-methylimidazole and 0.00548mmol of hexadecyl trimethyl ammonium bromide in 8mL of deionized water to obtain a 2-methylimidazole mixed solution; then adding Co (NO) at 25 deg.C3)2Pouring the solution into a 2-methylimidazole mixed solution, stirring for 20 minutes, centrifuging, washing twice by using deionized water, then washing once by using ethanol, and drying the obtained product at 60 ℃ for 12 hours in vacuum;
(2) preparation of Co-LDH/ZIF-67: dispersing the Co-LDH1.6mg obtained in the step (1) in 5mL of deionized water to obtain a Co-LDH solution; dispersing 1.22mmol 2-methylimidazole in 5mL deionized water to obtain a 2-methylimidazole solution; and pouring the 2-methylimidazole solution into the Co-LDH solution at 25 ℃, stirring for 6 hours, centrifuging, washing twice by using deionized water, washing once by using ethanol, and drying the obtained product in vacuum at 60 ℃ for 12 hours to obtain the Co-LDH/ZIF-67 composite material.
Example 2
The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery comprises the following steps:
(1) preparation of Co-LDH: firstly, 0.0515mmolCo (NO) is added3)2Dissolving in 8mL deionized water to obtain Co (NO)3)2A solution; 3.37mmol of 2-methylimidazole and 0.00548mmol of hexadecylDissolving a mixture of trimethyl ammonium bromide in 8mL of deionized water to obtain a 2-methylimidazole mixed solution; then adding Co (NO) at 25 deg.C3)2Pouring the solution into a 2-methylimidazole mixed solution, stirring for 20 minutes, centrifuging, washing twice by using deionized water, then washing once by using ethanol, and drying the obtained product at 60 ℃ for 12 hours in vacuum;
(2) preparation of Co-LDH/ZIF-67: dispersing the Co-LDH1.6mg obtained in the step (1) in 7mL of deionized water to obtain a Co-LDH solution; dispersing 1.22mmol 2-methylimidazole in 7mL deionized water to obtain a 2-methylimidazole solution; and pouring the 2-methylimidazole solution into the Co-LDH solution at 25 ℃, stirring for 6 hours, centrifuging, washing twice by using deionized water, washing once by using ethanol, and drying the obtained product in vacuum at 60 ℃ for 12 hours to obtain the Co-LDH/ZIF-67 composite material.
Example 3
The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery comprises the following steps:
(1) preparation of Co-LDH: first 0.103mmolCo (NO) is added3)2Dissolving in 15mL deionized water to obtain Co (NO)3)2A solution; dissolving a mixture of 6.74mmol of 2-methylimidazole and 0.00548mmol of hexadecyl trimethyl ammonium bromide in 15mL of deionized water to obtain a 2-methylimidazole mixed solution; then adding Co (NO) at 25 deg.C3)2Pouring the solution into a 2-methylimidazole mixed solution, stirring for 20 minutes, centrifuging, washing twice by using deionized water, then washing once by using ethanol, and drying the obtained product at 60 ℃ for 12 hours in vacuum;
(2) preparation of Co-LDH/ZIF-67: dispersing the Co-LDH3.2mg obtained in the step (1) in 10mL deionized water to obtain a Co-LDH solution; dispersing 2.44mmol 2-methylimidazole in 10mL deionized water to obtain a 2-methylimidazole solution; and pouring the 2-methylimidazole solution into the Co-LDH solution at 25 ℃, stirring for 6 hours, centrifuging, washing twice by using deionized water, washing once by using ethanol, and drying the obtained product in vacuum at 60 ℃ for 12 hours to obtain the Co-LDH/ZIF-67 composite material.
Claims (6)
1. A preparation method of a novel composite material for a positive electrode of a lithium-sulfur battery is characterized by comprising the following steps:
(1) preparation of Co-LDH: first Co (NO)3)2Dissolving in deionized water to obtain Co (NO)3)2A solution; dissolving a mixture of 2-methylimidazole and hexadecyl trimethyl ammonium bromide in deionized water to obtain a 2-methylimidazole mixed solution; then Co (NO) is added under the condition of room temperature3)2Pouring the solution into a 2-methylimidazole mixed solution, fully stirring, centrifuging, washing, and drying the obtained product at 60 ℃ for 12 hours in vacuum;
(2) preparation of Co-LDH/ZIF-67: dispersing the Co-LDH obtained in the step (1) in deionized water to obtain a Co-LDH solution; dispersing 2-methylimidazole in deionized water to obtain a 2-methylimidazole solution; and pouring the 2-methylimidazole solution into the Co-LDH solution at room temperature, fully stirring, centrifuging, washing, and performing vacuum drying on the obtained product at 60 ℃ for 12 hours to obtain the Co-LDH/ZIF-67 composite material.
2. The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery as claimed in claim 1, wherein the Co-LDH/ZIF-67 composite material prepared by the preparation method has a hollow cubic structure and the particle size is 300-400 nm; the structure is characterized in that the ZIF-67 is encapsulated with Co-LDH, and the Co-LDH is an ultrathin nanometer wafer growing on the inner surface of the ZIF-67.
3. The method for preparing a novel composite material for a positive electrode of a lithium-sulfur battery according to claim 1, wherein Co (NO) is used in the step (1)3)2Dissolving the solution in 0.0515-0.103 mmol of deionized water of 8-15 mL; 3.37-6.74 mmol of 2-methylimidazole and 0.00548mmol of hexadecyl trimethyl ammonium bromide, and mixing and dissolving the 2-methylimidazole and the hexadecyl trimethyl ammonium bromide in 8-15 mL of deionized water.
4. The preparation method of the novel composite material for the positive electrode of the lithium-sulfur battery as claimed in claim 1, wherein the Co-LDH in the step (2) is 1.6-3.2 mg, and is dispersed in 5-10 mL of deionized water; 1.22-2.44 mmol of 2-methylimidazole is dispersed in 5-10 mL of deionized water.
5. The method for preparing a novel composite material for a positive electrode of a lithium-sulfur battery according to claim 1, wherein the step (1) is performed by stirring at 25 ℃ for 20 minutes; washed twice with deionized water and once with ethanol.
6. The method for preparing a novel composite material for a positive electrode of a lithium sulfur battery according to claim 1, wherein the step (2) is performed by stirring at 25 ℃ for 6 hours; washed twice with deionized water and once with ethanol.
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| CN111463413A (en) * | 2020-04-09 | 2020-07-28 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Lithium-sulfur battery positive host material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103151524A (en) * | 2013-03-04 | 2013-06-12 | 北京化工大学常州先进材料研究院 | Positive pole material for high-performance lithium-sulfur battery and preparation method thereof |
| CN109103427A (en) * | 2018-08-01 | 2018-12-28 | 北京师范大学 | A kind of composite material, preparation method and its application for lithium-sulphur cell positive electrode |
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Application publication date: 20210914 |