CN114566621A - Composite anode material for thermal battery based on MXene and transition metal sulfide and synthetic method thereof - Google Patents
Composite anode material for thermal battery based on MXene and transition metal sulfide and synthetic method thereof Download PDFInfo
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Abstract
The invention discloses a composite anode material for a thermal battery based on MXene and transition metal sulfide and a synthesis method thereof, and belongs to the fields of nano materials and thermal batteries. The composite anode material for the thermal battery based on MXene and transition metal sulfide is characterized by consisting of MXene with the surface uniformly deposited with transition metal sulfide, and having a two-dimensional nanostructure, the size of the MXene is about 200-1000nm, the loading amount of the transition metal sulfide is adjusted to be 30-80 wt.%, the transition metal sulfide is nano-particles with the size of about 20-50nm, and the transition metal sulfide comprises at least one or more than two of cobalt sulfide, iron sulfide and nickel sulfide. The anode material for the thermal battery can overcome the basic problem of poor conductivity of the traditional anode material for the thermal battery, plays a role in promoting the development of high-power thermal batteries, and has military value and practical application prospect.
Description
Technical Field
The invention belongs to the field of nano materials and thermal batteries, and relates to a composite anode material for a thermal battery based on MXene and transition metal sulfide and a synthesis method thereof.
Background
Missiles are essential strategic weapons in modern war, and in order to meet the requirements of future spatial, informatization, intellectualization and electronization battlefields, the demand of new-generation missile weapons taking high and new technologies as the core is increasing day by day. In the process of missile flight, a power supply system provides power and electric energy for a guidance system, and the power supply system is a key component for missile operation. The thermal battery is a thermal activation reserve battery which is in a working state and is formed by heating and melting non-conductive solid-state salt electrolyte into an ionic conductor by using a heating system of the battery, and is widely applied to the military fields of missiles, radars, nuclear weapons and the like. The output energy of the thermal battery mainly depends on the electrochemical properties of positive and negative active materials, and the positive material commonly used in the thermal battery at present is FeS2And CoS2Two transition metal sulfides. As the internal resistance of the thermal battery in operation is mainly determined by the anode material, CoS2Has a resistivity (0.002. omega. cm) smaller than FeS2Since the resistivity of (0.036. omega. cm), CoS is a common positive electrode material used in high-power thermal batteries at present2A base composite positive electrode material. Modern weapons and equipment are rapidly developed, more severe requirements are put on the electrochemical performance of a thermal battery, and the existing anode material is difficult to meet the increasing requirements, so that the development of a high-conductivity anode material is one of the keys of the continuous development of the thermal battery.
MXene is a novel two-dimensional crystal of transition metal carbide or nitride with a graphene-like structure. Having the chemical formula Mn+1Xn(n is 1, 2, 3, M is a transition metal element, and X is carbon or nitrogen). MXene has metalloid conductivity, and is expected to couple transition metal sulfide through chemical action to improve the dispersibility and conductivity of the transition metal sulfide, thereby realizing the design and construction of the novel high-conductivity positive electrode material for the thermal battery.
Disclosure of Invention
Aiming at the defect of poor conductivity of the existing transition metal sulfide cathode material, the invention provides a composite cathode material for a thermal battery based on MXene and transition metal sulfide and a synthesis method thereof, and the prepared cathode material consists of MXene with the surface uniformly coated with transition metal sulfide nano particles. The metal sulfide is uniformly distributed on the surface of MXene, so that the problems of poor conductivity of the metal sulfide and performance reduction caused by easy agglomeration in the preparation and reaction processes are solved, the fundamental problem which troubles the performance exertion and application of the metal sulfide cathode material is solved, and the power characteristic of the thermal battery can be improved when the obtained cathode material is applied to the thermal battery. The synthesis method is simple, easy to control and universal, and can be used for large-scale production.
The composite positive electrode material for the thermal battery is characterized by consisting of MXene with transition metal sulfide uniformly deposited on the surface, and having a two-dimensional nanostructure, wherein the size of the MXene is 200-1000nm, the loading amount of the transition metal sulfide is adjusted to be 30-80 wt.%, the transition metal sulfide is nanoparticles with the size of 20-50nm, and the transition metal sulfide comprises at least one or more than two of cobalt sulfide, iron sulfide and nickel sulfide.
The invention also provides a synthesis method of the composite anode material for the thermal battery based on MXene and transition metal sulfide, which is characterized by comprising the following steps of:
1) dispersing MXene, metal salt and polyvinylpyrrolidone PVP-K30 in methanol to obtain suspension A, stirring and centrifuging at normal temperature and pressure, dispersing in appropriate amount of methanol again to obtain suspension B, and making the concentration of MXene in the suspension B be about 4mg mL-1；
2) Adding a methanol solution of metal salt and a methanol solution of dimethyl imidazole with the same volume into the suspension B while stirring, stirring at normal temperature and normal pressure, centrifuging, washing, and freeze-drying to obtain a compound C, wherein the type of the metal salt is the same as that of the metal salt used in the step 1);
3) dispersing the compound C prepared in the step 2) and thioacetamide in methanol, carrying out solvothermal reaction for 1-4h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D;
4) and under the protection of inert gas, placing the compound D prepared in the step 3) into a high-temperature furnace for calcination treatment to obtain the composite anode material for the thermal battery based on MXene and transition metal sulfide, wherein the calcination temperature is 300-400 ℃, and the calcination time is 3-5 h.
Further, the metal salt is at least one or more than two of nitrate and acetate of cobalt, iron and nickel.
Furthermore, the concentration of MXene in the suspension A is 2mg mL-1The concentration of the metal salt is 20mg mL-1PVP concentration 10mg mL-1。
Further, the concentration of the metal salt in the step 2) is 0.02 to 0.08mol L-1The molar ratio of the metal salt to the dimethylimidazole is 1: 8.
Further, the concentration of the complex C in the step 3) is 2mg mL-1The mass ratio of the compound C to thioacetamide is 1: 1-5.
Further, the inert gas is at least one of nitrogen and argon, and the flow rate of the carrier gas is 0.1-1.0L h-1。
Further, the stirring and centrifuging in the step 1) is stirring for 30min, and centrifuging twice; and 2) stirring and then centrifuging, namely stirring for 15min and then centrifuging.
The anode material for the thermal battery can overcome the basic problem of poor conductivity of the traditional anode material for the thermal battery, plays a role in promoting the development of high-power thermal batteries, and has military value and practical application prospect.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has proposed the technical solution of the present invention through long-term research and extensive practice, and further explains the technical solution, the implementation process and the principle, etc. It is to be understood, however, that within the scope of the present invention, each of the above-described features of the present invention and each of the features described in detail below (examples) may be combined with each other to form new or preferred embodiments.
The invention provides a composite anode material for a thermal battery based on MXene and transition metal sulfide and a synthesis method thereof. The composite cathode material for the thermal battery based on MXene and transition metal sulfide can be prepared by the synthesis method.
The composite anode material for the thermal battery based on MXene and transition metal sulfide is composed of MXene with transition metal sulfide uniformly deposited on the surface, and has a two-dimensional nano structure, and the size of the composite anode material is about 200-1000 nm. The loading capacity of the transition metal sulfide loaded on the MXene is adjustable, and the loading capacity is 30-80 wt.%. The size of the transition metal sulfide nano-particles is about 20-50 nm; the transition metal sulfide comprises at least one or more of cobalt sulfide, iron sulfide and nickel sulfide.
The method for synthesizing the composite anode material for the thermal battery based on MXene and transition metal sulfide comprises the following steps:
1) dispersing MXene, metal salt and polyvinylpyrrolidone (PVP K30) in methanol to obtain suspension A, stirring at room temperature under normal pressure for 30min, centrifuging twice, dispersing in appropriate amount of methanol to obtain suspension B, wherein the concentration of MXene in suspension B is about 4mg mL-1. The metal salt can be at least one or more than two of nitrate and acetate of cobalt, iron and nickel. In one embodiment, the concentration of MXene in the suspension A is 2mg mL-1The concentration of the metal salt is 20mg mL-1PVP concentration 10mg mL-1。
2) And adding the same volume of metal salt methanol solution and dimethyl imidazole methanol solution into the suspension B while stirring, stirring for 15min at normal temperature and pressure, centrifuging, washing, and freeze-drying to obtain the compound C. The metal salt is the same as the metal salt used in the step 1). In one embodiment, the metal salt of step 2) has a concentration of 0.02 to 0.08mol L-1The molar ratio of the metal salt to the dimethylimidazole is 1: 8.
3) Dispersing the compound C prepared in the step 2) and thioacetamide in methanol, carrying out solvothermal reaction for 1-4h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D. The concentration of the compound C in the step 3) is 2mg mL-1The mass ratio of the compound C to thioacetamide is 1: 1-5.
4) And under the protection of inert gas, placing the compound D prepared in the step 3) into a high-temperature furnace for calcination treatment to obtain the positive electrode material for the thermal battery based on the MXene and transition metal sulfide composite nano structure, wherein the calcination temperature is 300-400 ℃, and the calcination time is 3-5 h. The inert gas is at least one of nitrogen and argon, and the flow rate of the carrier gas can be 0.1-1.0L h-1。
Examples
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1 based on MXene and CoS2Preparation method of composite nano positive electrode material
1) 100mg of MXene, 1g of cobalt acetate tetrahydrate and 500mg of polyvinylpyrrolidone (PVP K30) were dispersed in 50ml of methanol to obtain a suspension A, stirred at normal temperature and pressure for 30min, centrifuged twice and dispersed in 25ml of methanol to obtain a suspension B.
2) To the suspension B was added 25ml of a methanol solution of cobalt acetate tetrahydrate (0.05mol L) in this order while stirring-1) And 25ml of a solution of dimethylimidazole in methanol (0.4mol L)-1) Stirring for 15min under normal temperature and pressure, centrifuging, washing, and freeze drying to obtain compound C.
3) Dispersing 100mg of the compound C prepared in the step 2) and 200mg of thioacetamide in 50ml of methanol, carrying out solvothermal reaction for 2h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D.
4) Placing the compound D prepared in the step 3) into a high-temperature furnace for calcination treatment under the protection of argon to obtain the composite anode material for the thermal battery based on MXene and transition metal sulfide, wherein the calcination temperature is 350 ℃, the calcination time is 3 hours, and the carrier gas flow rate is 0.5L h-1。
Obtaining products MXene and CoS2The size of the two-dimensional sheet material is about 200-1000nm, CoS2The size is about 20nm, the content is about 46 wt%, and the resistance of the resistivity detection product is 0.00059 omega cm.
Example 2 MXene and Co basedxFe1-xS2Preparation method of composite nano positive electrode material
1) 500mg of MXene, 5g of cobalt nitrate hexahydrate, and iron nitrate nonahydrate (mass ratio of 1: 1) and 2.5g of polyvinylpyrrolidone (PVP K30) in 250ml of methanol to obtain suspension A, stirring at normal temperature and pressure for 30min, centrifuging twice, and dispersing in 125ml of methanol to obtain suspension B.
2) 125ml of a methanol solution (0.08mol L) of cobalt nitrate hexahydrate and iron nitrate nonahydrate were added to the suspension B in this order while stirring-1The molar ratio of Co to Fe is 1: 1) and 125ml of a solution of dimethylimidazole in methanol (0.64mol L)-1) And stirring for 15min at normal temperature and normal pressure, and then centrifuging, washing and freeze-drying to obtain the compound C.
3) Dispersing 100mg of the compound C prepared in the step 2) and 250mg of thioacetamide in 50ml of methanol, carrying out solvothermal reaction for 2.5h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D.
4) Placing the compound D prepared in the step 3) into a high-temperature furnace to be calcined under the protection of argon to obtain the composite anode material for the thermal battery based on MXene and transition metal sulfide, wherein the calcination temperature is 400 ℃, the calcination time is 3 hours, and the carrier gas flow rate is 0.1L h-1。
Obtaining products MXene and CoxFe1-xS2The size of the two-dimensional sheet material is about 200-1000nm, and Co is used as the composite nano anode materialxFe1-xS2The size is about 20-50nm, the content is about 32 wt%, and the resistance of the product is 0.00071 omega cm according to the resistivity detection.
Example 3 MXene and Co basedxNi1-xS2Preparation method of composite nano positive electrode material
1) 400mg of MXene, 4g of cobalt nitrate hexahydrate and iron nitrate hexahydrate (mass ratio of 1: 1) and 2g of polyvinylpyrrolidone (PVP K30) in 200ml of methanol to obtain suspension A, stirring for 30min at normal temperature and pressure, centrifuging twice, and dispersing in 100ml of methanol to obtain suspension B.
2) 100ml of a methanol solution (0.04mol L) of cobalt nitrate hexahydrate and iron nitrate nonahydrate were added to the suspension B in this order while stirring-1The molar ratio of Co to Ni is 3: 1) and 100ml of a solution of dimethylimidazole in methanol (0.32mol L)-1) And stirring for 15min at normal temperature and normal pressure, and then centrifuging, washing and freeze-drying to obtain the compound C.
3) Dispersing 100mg of the compound C prepared in the step 2) and 150mg of thioacetamide in 50ml of methanol, carrying out solvothermal reaction for 4h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D.
4) Placing the compound D prepared in the step 3) into a high-temperature furnace for calcination treatment under the protection of argon to obtain the composite anode material for the thermal battery based on MXene and transition metal sulfide, wherein the calcination temperature is 300 ℃, the calcination time is 5 hours, and the carrier gas flow rate is 0.2L h-1。
Obtaining products MXene and CoxFe1-xS2The size of the two-dimensional sheet material is about 200-1000nm, and Co is used as the composite nano anode materialxFe1-xS2The size is about 30-50nm, the content is about 65 wt%, and the resistance of the product is 0.00085 omega cm according to the resistivity detection.
The anode material prepared by the method consists of MXene with the surface uniformly coated with transition metal sulfide nanoparticles. MXene with surface adsorbed metal cations and PVP and a metal salt solution are subjected to solvothermal reaction, and the obtained product and thioacetamide are subjected to vulcanization reaction and then are calcined at high temperature to obtain the MXene and metal sulfide composite cathode material with controllable structure and components.
The invention solves the problem faced by transition metal sulfide anode material for thermal battery, and the technical effects include:
1) MXene with excellent metalloid conductivity is introduced, so that the resistivity of the transition metal sulfide anode material is obviously reduced, and the power characteristic of the thermal battery is improved.
2) MXene with a two-dimensional layered structure is introduced, and transition metal sulfide with the surface strong coupling size of only tens of nanometers provides a larger chemical reaction activity specific surface area and more abundant chemical reaction active sites for the composite cathode material, so that the composite cathode material is endowed with higher electrochemical reaction activity.
3) The method can realize fine regulation and control of microstructure, chemical composition and the like of the positive electrode material for the thermal battery based on MXene and transition metal sulfide, has simple process and easy control, is beneficial to large-scale production, can be applied to thermal battery technology, and has wide application prospect in energy fields of other batteries, catalysis and the like.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (8)
1. The composite cathode material for the thermal battery based on MXene and transition metal sulfide is characterized by consisting of MXene with the surface uniformly deposited with transition metal sulfide, and the composite cathode material has a two-dimensional nanostructure, the size of 200-1000nm, the loading amount of the transition metal sulfide is adjusted to be 30-80 wt.%, the transition metal sulfide is nano-particles with the size of 20-50nm, and the transition metal sulfide comprises at least one or more than two of cobalt sulfide, iron sulfide and nickel sulfide.
2. The method for synthesizing the composite cathode material for the thermal battery based on MXene and transition metal sulfide as claimed in claim 1, is characterized by comprising the following steps:
1) dispersing MXene, metal salt and polyvinylpyrrolidone PVP-K30 in methanol to obtain suspension A, stirring and centrifuging at normal temperature and pressure, dispersing in appropriate amount of methanol again to obtain suspension B, and making the concentration of MXene in the suspension BAbout 4mg mL-1；
2) Sequentially adding a methanol solution of metal salt and a methanol solution of dimethyl imidazole with the same volume into the suspension B while stirring, stirring at normal temperature and normal pressure, centrifuging, washing, and freeze-drying to obtain a compound C, wherein the type of the metal salt is the same as that of the metal salt used in the step 1);
3) dispersing the compound C prepared in the step 2) and thioacetamide in methanol, carrying out solvothermal reaction for 1-4h at 90 ℃, cooling, centrifuging, washing, and freeze-drying to obtain a compound D;
4) and under the protection of inert gas, placing the compound D prepared in the step 3) into a high-temperature furnace for calcination treatment to obtain the composite anode material for the thermal battery based on MXene and transition metal sulfide, wherein the calcination temperature is 300-400 ℃, and the calcination time is 3-5 h.
3. The method for synthesizing the composite cathode material for the thermal battery based on MXene and the transition metal sulfide as claimed in claim 2, wherein the metal salt is at least one or more of nitrate and acetate of cobalt, iron and nickel.
4. The method for synthesizing the composite cathode material for the thermal battery based on MXene and the transition metal sulfide as claimed in claim 2, wherein the concentration of MXene in the suspension A is 2mg mL-1The concentration of the metal salt is 20mg mL-1PVP concentration 10mg mL-1。
5. The method for synthesizing the composite cathode material for the thermal battery based on MXene and transition metal sulfide as claimed in claim 2, wherein the concentration of the metal salt in step 2) is 0.02-0.08mol L-1The molar ratio of the metal salt to the dimethyl imidazole is 1: 8.
6. The method for synthesizing the composite cathode material for the thermal battery based on MXene and transition metal sulfide as claimed in claim 2, wherein the concentration of the composite C in the step 3) isIs 2mg mL-1The mass ratio of the compound C to thioacetamide is 1: 1-5.
7. The method for synthesizing the composite cathode material for the thermal battery based on MXene and the transition metal sulfide as claimed in claim 2, wherein the inert gas is at least one of nitrogen and argon, and the carrier gas flow rate is 0.1-1.0L h-1。
8. The method for synthesizing the composite cathode material for the thermal battery based on MXene and the transition metal sulfide as claimed in claim 2, wherein the stirring centrifugation in step 1) is stirring for 30min and then centrifuging twice; and 2) stirring and then centrifuging, namely stirring for 15min and then centrifuging.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018195837A1 (en) * | 2017-04-26 | 2018-11-01 | 苏州大学张家港工业技术研究院 | Metal-sulfur battery and preparation method therefor |
| CN111704138A (en) * | 2020-06-03 | 2020-09-25 | 大连理工大学 | Preparation method of two-dimensional nanocomposite material self-assembled layer by layer |
| CN112599769A (en) * | 2020-12-28 | 2021-04-02 | 江苏大学 | Aluminum ion battery and positive electrode material Co thereofxSy@MXene |
| CN113381012A (en) * | 2021-07-02 | 2021-09-10 | 北京化工大学 | MXene-based metal sulfide and preparation method and application thereof |
| CN113764203A (en) * | 2021-08-16 | 2021-12-07 | 中国石油大学(华东) | Cobalt nickel sulfide-MXene electrode material for super capacitor and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018195837A1 (en) * | 2017-04-26 | 2018-11-01 | 苏州大学张家港工业技术研究院 | Metal-sulfur battery and preparation method therefor |
| CN111704138A (en) * | 2020-06-03 | 2020-09-25 | 大连理工大学 | Preparation method of two-dimensional nanocomposite material self-assembled layer by layer |
| CN112599769A (en) * | 2020-12-28 | 2021-04-02 | 江苏大学 | Aluminum ion battery and positive electrode material Co thereofxSy@MXene |
| CN113381012A (en) * | 2021-07-02 | 2021-09-10 | 北京化工大学 | MXene-based metal sulfide and preparation method and application thereof |
| CN113764203A (en) * | 2021-08-16 | 2021-12-07 | 中国石油大学(华东) | Cobalt nickel sulfide-MXene electrode material for super capacitor and preparation method thereof |
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