CN114242982A - Graphene-coated two-dimensional metal compound electrode material, preparation method and application thereof - Google Patents
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Abstract
本发明公开了一种石墨烯包覆二维金属化合物电极材料及其制备方法和应用，该方法将金属单质粉末置于真空管式炉中，然后在惰性气体与CX2气体的混合气氛中进行煅烧，煅烧后随炉冷却即得到，其中，所述X选自S、Se、Te中的一种或多种。本发明利用金属单质与CX2型化合物的金属热反应，原位合成了碳包覆二维金属硫化物电极，碳层的存在形式为石墨烯，有效提升了材料的结构稳定性和导电性，从而提高了负极材料的循环稳定性。本发明提供的合成方法仅需一步完成，方法便捷，成本低廉，适合工业化大规模生产使用。
The invention discloses a graphene-coated two-dimensional metal compound electrode material and a preparation method and application thereof. In the method, metal elemental powder is placed in a vacuum tube furnace, and then calcined in a mixed atmosphere of inert gas and CX gas , calcined and then cooled in a furnace, wherein the X is selected from one or more of S, Se, and Te. The present invention utilizes the metal thermal reaction between a metal element and a CX 2 type compound to synthesize a carbon-coated two-dimensional metal sulfide electrode in situ, and the carbon layer exists in the form of graphene, which effectively improves the structural stability and electrical conductivity of the material. Thus, the cycle stability of the negative electrode material is improved. The synthesis method provided by the invention only needs to be completed in one step, the method is convenient, the cost is low, and it is suitable for industrialized large-scale production.
Description
Technical Field
The invention relates to the technical field of lithium ion battery material preparation, in particular to a graphene-coated two-dimensional metal compound electrode material and a preparation method and application thereof.
Background
The lithium ion battery is used as a secondary energy storage device, is widely applied to small-sized portable electronic products and electric vehicles, and has extremely high application prospect. The lithium ion battery is composed of four main raw materials, namely a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the negative electrode material is one of key factors influencing the capacity, the cycle performance and the rate performance of the lithium ion battery. The theoretical capacity of a commercial graphite negative electrode which is mainly applied in the current market is only 372mAh/g, and the research and development of a negative electrode material with higher specific capacity are important tasks in the field of secondary batteries. Wherein the two-dimensional metal compound MX2The unique layered structure and lithium storage characteristics (M ═ Mo/W/Sn, etc., and X ═ S/Se/Te, etc.) make it possible to provide theoretical specific capacity over 600mAh/g, and thus it is a new type of negative electrode material with development prospect. The problems of volume expansion, byproduct dissolution and the like of an independent two-dimensional metal compound generally exist in the battery circulation process, so that the circulation performance is poor, and the problems can be effectively relieved by compounding the metal compound and a carbon material. At present, it has been reported that a hydrothermal method, a chemical vapor deposition method and the like are adopted to successfully synthesize a related two-dimensional metal compound/carbon material composite negative electrode material (such as MoS) with higher specific capacity and more stable cycling performance2、WS2、MoSe2Etc.), however, most of the methods reported at present have the defects of complicated preparation process, low yield, high cost and the like, and are in the laboratory stage.
Chinese patent CN 109671937a discloses an in-situ synthesis method of a transition metal oxide/graphene composite material, which has a process that is approximately: dissolving and mixing soluble ferric salt, soluble transition metal salt and soluble cerium salt in deionized water to obtain a uniform solution, dropwise adding a precipitator into the uniform solution, aging, filtering, washing and drying to obtain a transition metal hydroxide compound precipitate; weighing graphite and potassium permanganate, mixing, adding concentrated sulfuric acid and phosphoric acid mixed acid solution, reacting to obtain a gray green solution, carrying out ice bath treatment, adding a transition metal hydroxide compound for precipitation, then slowly adding hydrogen peroxide, stirring and dispersing to obtain a suspension of transition metal hydroxide/graphene oxide which is coated and grown mutually, and washing, centrifuging, drying and roasting the suspension to obtain the transition metal oxide/graphene composite material. In the patent technology, in the process of in-situ synthesis of graphene oxide, a transition metal hydroxide compound is directly added to obtain a transition metal oxide/graphene composite material with a porous structure, and the specific surface area reaches 100-200 m-2In each case, CeO2The addition of the graphene is beneficial to the generation of the nano-rods, the graphene is uniformly dispersed among gaps of product particles, the structure can buffer the volume expansion effect of the metal oxide in the charge-discharge cycle process, and the electrode reaction dynamic performance is improved. However, the patent technology still has the defects of complicated preparation process, low yield, high cost and the like, and cannot be industrially applied.
Disclosure of Invention
The invention aims to: aiming at the problems, the invention provides a graphene-coated two-dimensional metal compound electrode material and a preparation method and application thereof2The synthesis method provided by the invention is completed in one step, is convenient and fast, has low cost, is suitable for industrial large-scale production and use, and overcomes the defect that the conventional synthesis method for the compound has the defects that the carbon-coated two-dimensional metal sulfide electrode is synthesized in situ, the carbon layer exists in the form of graphene, and the structural stability and the electrical conductivity of the material are effectively improved, so that the cycle stability of the cathode material is improvedThe technology has the defects.
The technical scheme adopted by the invention is as follows: the in-situ synthesis method of the graphene-coated two-dimensional metal compound electrode material comprises the steps of placing metal simple substance powder in a vacuum tube furnace, and then placing inert gas and CX2Calcining in a gas mixed atmosphere, and cooling in a furnace after calcining to obtain the catalyst, wherein X is selected from one or more of S, Se and Te.
Further, the metal simple substance is one or more of Mo, W, Sn, and the like, and is not limited to the first three metal simple substances.
Furthermore, the calcination temperature is 600-1000 ℃, and the calcination time is 4-6 h.
Furthermore, the heating rate is 2-6 ℃/min during the calcination.
Further, the inert gas is argon, argon and CX2Is 100: 1-10. the volume ratio is preferably in this range if CX2If the volume fraction of (A) is too low, the reaction time is longer and the conversion is incomplete, whereas if CX is too low2Too high volume fraction of (C), CS2More waste, high cost and environmental pollution.
Preferably, the metal simple substance is Mo, and the CX is2Is CS2。
The invention further discloses a graphene-coated two-dimensional metal compound electrode material, which is prepared by the method.
Further, the inner layer of the electrode material is a layered metal compound, and the outer layer of the electrode material is graphene.
The invention also comprises a lithium ion battery which comprises a negative electrode material, wherein the negative electrode material is the graphene-coated two-dimensional metal compound electrode material.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the carbon-coated two-dimensional metal compound electrode material, the inner layer is a layered metal compound, the outer layer is graphene, the carbon-coated two-dimensional metal compound electrode material has good structural stability and conductivity, and can provide high specific capacity and good cycling stability when being used as a negative electrode of a secondary ion battery;
2. the invention utilizes metal simple substance and CX2The synthesis method provided by the invention is completed in one step, is convenient and fast, has low cost, is suitable for industrial large-scale production and use, and overcomes the defects in the prior art.
Drawings
FIG. 1 is an SEM image of the original molybdenum powder before reaction in example 1 of the present invention;
FIG. 2 shows the MoS synthesized after the reaction in example 1 of the present invention2SEM topography of @ graphene;
FIG. 3 shows MoS in example 1 of the present invention2TEM images of @ graphene;
FIG. 4 shows MoS in example 1 of the present invention2XRD pattern of @ graphene;
FIG. 5 shows MoS of example 1 of the present invention2@ graphene and comparative example 1 MoS2A cyclic graph of (a);
FIG. 6 is a cycle plot of example 2 SnS @ graphene of the present invention versus comparative example 1 SnS;
FIG. 7 shows WS according to embodiment 3 of the present invention2@ graphene and comparative example 1 WS2The cycle graph of (a).
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Test main detection equipment
X-ray diffraction (XRD) test: x-ray diffractometer, instrument model: rigaku UltimaIV-185, Japan.
Scanning Electron Microscope (SEM) testing: scanning electron microscope, instrument model: FEIQuanta, the netherlands.
Assembling method of CR2025 button battery
The electrode materials (example 1, example 2, example 3), acetylene black, and polyvinylidene fluoride (PVDF) were mixed in a ratio of 7: 2: 1, preparing slurry, coating the slurry on a copper foil, drying, cutting the dried copper foil into small round pieces with the diameter of about 1cm by using a cutting machine, using a metal lithium piece as a counter electrode, using Celgard2500 as a diaphragm, and using EC/DMC/EMC 1: 1: 1(W/W) +1M LiPF6A CR2025 button cell was assembled in an argon atmosphere glove box as an electrolyte.
And (3) electrochemical performance testing:
an LANDCT 2001A tester (blue electronic, Inc., Wuhan city) is adopted to carry out electrochemical performance test on the assembled battery, the test temperature is 30 ℃, the test voltage range is 0.01-3V, and charging and discharging are carried out at 100mAh/g in the test process.
Example 1
Preparation of graphene coated MoS2A method of (M ═ Mo, X ═ S) electrode material, comprising the steps of:
s1, weighing 1g of nano-scale molybdenum powder, placing the nano-scale molybdenum powder in a tube furnace, and then introducing argon and CS2Wherein CS is2The volume ratio of (A) is 8%;
s2, calcining molybdenum powder at a heating speed of 4 ℃ min, heating to 900 ℃, preserving heat for 5 hours, and cooling along with the furnace to obtain graphene-coated MoS2An electrode material.
Coating the obtained graphene-coated MoS2The electrode material is made into a negative pole piece and a button cell is made for performance comparison. Wherein, the negative pole is composed of: composite anode material: conductive additive: binder 70: 20: 10, adopting a Celgard2500 type diaphragm, adopting a lithium metal counter electrode, and adopting an EC/DMC/EMC 1: 1: 1(W/W) +1M LiPF6 is an electrolyte.
Example 2
A method for preparing a graphene coated SnS electrode material comprises the following steps:
s1, weighing 1g of nano-scale tin powder, placing the nano-scale tin powder in a tube furnace, and then introducing argon and CS2Wherein CS is2The volume percentage of (A) is 2%;
s2, calcining tin powder at a heating speed of 5 ℃ min by setting a heating program, heating to 800 ℃, preserving heat for 5 hours, and then cooling along with a furnace to obtain graphene-coated SnS2An electrode material.
SnS obtained in the above embodiment2An electrode sheet was prepared as a negative electrode using a lithium metal sheet as a counter electrode, Celgard2500 as a separator, and a 1M carbonate solution as an electrolyte (wherein the solvent was a mixed solution of ethylene carbonate and dimethyl carbonate at a volume ratio of 1: 1, and the solute was LiPF6) The CR2025 button cell was assembled in a glove box under argon atmosphere. At 100mA · g－1And testing the performance of the battery under the charge and discharge current density.
Example 3
Preparation of graphene coated WS2A method of (M-W, X-S) electrode material, comprising the steps of:
s1, weighing 1g of nano-grade tungsten powder, placing the powder in a tube furnace, and then introducing argon and CS2Wherein CS is2The volume ratio of (A) is 5%;
s2, setting a heating program to be a heating speed of 6 ℃ min, calcining tungsten powder, heating to 700 ℃, preserving heat for 5 hours, and cooling along with a furnace to obtain the graphene coated WS2An electrode material.
WS obtained in the above example2An electrode sheet was prepared as a negative electrode using a lithium metal sheet as a counter electrode, Celgard2500 as a separator, and a 1M carbonate solution as an electrolyte (wherein the solvent was a mixed solution of ethylene carbonate and dimethyl carbonate at a volume ratio of 1: 1, and the solute was LiPF6) The CR2025 button cell was assembled in a glove box under argon atmosphere. At 100mA · g－1And testing the performance of the battery under the charge and discharge current density.
Comparative example 1
For commercial MoS2A sample (Mecline, 99.5% or more and 100nm) is prepared into a negative electrode plate according to the method of the embodiment 1, a button cell is assembled, and the cell test is carried out under the same test conditions as the embodiment 1.
Comparative example 2
A commercially available SnS sample (with a melting material, 99.99%, 325 mesh) was fabricated into a negative electrode tab according to the method described in example 1, assembled into a button cell, and subjected to a battery test under the same test conditions as in example 1.
Comparative example 3
For commercially available WS2Samples (alatin, 99.9%, 2 μm) were fabricated into negative electrode sheets as described in example 1, assembled into coin cells, and subjected to cell testing under the same test conditions as in example 1.
The material obtained in example 1 has a lamellar morphology as shown by SEM tests. TEM tests show that the surface of the sheet of the material obtained in example 1 is coated with the graphene layer. XRD tests show that the main component of the material obtained in example 1 is molybdenum disulfide. The result of the constant-current charge and discharge test of the battery shows that the MoS described in the embodiment 1 is adopted under the condition of 100mA/g current density2The initial specific discharge capacity of the @ graphene negative electrode material is 746.6mAh/g, and the capacity retention rate reaches 77% after 100 times of circulation. SnS as described in example 22The initial discharge specific capacity of the @ graphene negative electrode material is 1194mAh/g, and the capacity retention rate is 42% after 20 times of circulation. WS as described in example 32The initial discharge specific capacity of the @ graphene negative electrode material is 707mAh/g, and the capacity retention rate reaches 88% after 20 times of circulation.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
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| CN118867156A (en) * | 2024-06-12 | 2024-10-29 | 南华大学 | Transition metal and metal-poor sulfur-selenium-tellurium composite materials and their preparation and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118867156A (en) * | 2024-06-12 | 2024-10-29 | 南华大学 | Transition metal and metal-poor sulfur-selenium-tellurium composite materials and their preparation and application |
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