CN111180694A - MXene/metal sulfide composite material, negative electrode material, preparation and application - Google Patents
MXene/metal sulfide composite material, negative electrode material, preparation and application Download PDFInfo
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- CN111180694A CN111180694A CN201911409515.6A CN201911409515A CN111180694A CN 111180694 A CN111180694 A CN 111180694A CN 201911409515 A CN201911409515 A CN 201911409515A CN 111180694 A CN111180694 A CN 111180694A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
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- 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
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention belongs to the technical field of high-performance/high-energy-density lithium ion battery cathodes, and particularly relates to an MXene/metal sulfide composite material, a cathode material, preparation and application. Mixing and stirring metal salt of transition metal elements and MXene materials, and carrying out solid-liquid separation and drying to obtain an MXene/metal salt mixture; mixing the MXene/metal salt mixture with a sulfur source under a protective atmosphere and carrying out heat treatment to obtain the MXene/metal sulfide composite material. The invention also provides a sulfur-doped MXene/metal sulfide-based composite battery cathode material, which comprises the MXene/metal sulfide composite material. The cathode material provided by the invention has good long-cycle stability, high energy density and excellent rate capability, and can be applied to various fields.
Description
Technical Field
The invention belongs to the technical field of high-performance/high-energy-density lithium ion battery cathodes, and particularly relates to an MXene/metal sulfide composite material, a cathode material, preparation and application.
Background
During the past decades, lithium ion batteries have received great attention due to their high energy density, light weight and good cycling performance. However, with the development of society, the existing lithium ion battery is difficult to meet the use requirements of some electronic devices, large-scale power grids and electric vehicles. In the face of the ever-increasing demand for higher performance batteries, there is an urgent need to develop a new electrode material to obtain a new lithium ion battery with higher energy density, longer cycle life and fast charge and discharge capability.
The transition metal sulfide has higher theoretical capacity and lower cost, and is a popular material studied in recent years. However, the conductivity of the material is poor, and the volume change of the electrode material is serious in the electrochemical reaction process, so that electrode pulverization is easily caused, and the capacity and the service life of the battery are reduced. Meanwhile, the reaction of the transition metal sulfide material with lithium can generate polysulfide intermediate products which can be dissolved in the electrolyte, and a shuttle effect is formed, so that the capacity is further reduced.
The MXene material is a two-dimensional transition metal carbon/nitride material newly found in 2011, has high specific surface area, excellent conductivity, ultrahigh electronic conductivity, high mechanical strength and excellent electrochemical performance similar to graphene, and has huge application potential on battery electrode materials. The MXene material is doped and modified by sulfur, so that the MXene material has more active sites and can be firmly combined with other materials.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention primarily aims to provide a preparation method of an MXene/metal sulfide composite material.
The invention also aims to provide the MXene/metal sulfide composite material prepared by the preparation method.
The invention further aims to provide application of the MXene/metal sulfide composite material.
The invention also provides a sulfur-doped MXene/metal sulfide-based composite battery anode material, which comprises the MXene/metal sulfide composite material.
The fifth purpose of the invention is to provide the preparation method of the sulfur-doped MXene/metal sulfide-based composite battery negative electrode material, which has the advantages of simple process and environmental protection.
The purpose of the invention is realized by the following technical scheme:
a preparation method of MXene/metal sulfide composite material comprises the following steps:
(1) mixing and stirring metal salt of transition metal element and MXene material with water, then carrying out solid-liquid separation, and drying to obtain MXene/metal salt mixture;
(2) mixing the MXene/metal salt mixture prepared in the step (1) with a sulfur source under a protective atmosphere, heating to 300-900 ℃, and preserving heat for 1-6 hours to obtain an MXene/metal sulfide composite material;
the transition metal element in the step (1) is preferably at least one of tin, antimony, cobalt, iron, titanium, molybdenum and manganese;
the metal salt of the transition metal element in the step (1) is preferably at least one of nitrate, carbonate, sulfate and chloride of the transition metal element;
the MXene material in the step (1) is preferably Ti3C2、Ti2C、V4C3、Ta4C3、Ta2C、Mo2Ta2C3、V2C、Mo4C3、Mo2C、Nb4C3、Nb2C and Cr2At least one of C;
the MXene material is preferably formed by etching by HF; wherein, Mo2Ta2C3Etching off the starting material Mo by HF2Ta2AlC3Al atom in (1) to obtain;
the stirring time in the step (1) is preferably 3-48 h;
the solid-liquid separation mode in the step (1) is preferably suction filtration;
the sulfur source in the step (2) is preferably at least one of thioacetamide, ammonium persulfate, thiourea, sodium sulfide and cysteine;
the protective atmosphere in the step (2) is preferably nitrogen or argon;
the heating rate in the step (2) is preferably 2-20 ℃/min;
the mass ratio of the metal salt of the transition metal element in the step (1), the MXene material and the sulfur source in the step (2) is preferably (1-100): (1-100): (5-400);
an MXene/metal sulfide composite material is prepared by the preparation method;
the MXene/metal sulfide composite material is applied to the field of preparation of battery cathode materials;
a sulfur-doped MXene/metal sulfide-based composite battery negative electrode material comprises the MXene/metal sulfide composite material;
the sulfur-doped MXene/metal sulfide-based composite battery negative electrode material preferably further comprises a conductive agent and a binder;
in the sulfur-doped MXene/metal sulfide-based composite battery negative electrode material, the mass ratio of the MXene/metal sulfide composite material to the conductive agent to the binder is preferably (10-99): (1-20): (1-20);
the conductive agent is preferably at least one of graphene, conductive carbon black, SP and vinyl alkyne;
the binder is preferably at least one of polyvinylidene fluoride (PVDF), sodium carboxymethylcellulose (CMC), polyvinylidene fluoride (HSV), Polytetrafluoroethylene (PTFE), styrene-butadiene rubber (SBR) and polyacrylic acid (PAA);
the preparation method of the sulfur-doped MXene/metal sulfide-based composite battery anode material comprises the following steps:
preparing MXene/metal sulfide composite material, conductive agent and binder into slurry, and coating the slurry on a current collector to obtain MXene/metal sulfide-based composite battery negative electrode material;
the current collector is preferably at least one of copper foil, carbon-coated copper foil, carbon cloth, carbon paper and aluminum foil;
the sulfur-doped MXene/metal sulfide-based composite battery cathode material is applied to the field of lithium ion batteries;
compared with the prior art, the invention has the following advantages and effects:
(1) the invention adopts transition metal sulfide as active substance, and has ultrahigh theoretical capacity and lower cost. The transition metal sulfide is ingeniously loaded on the two-dimensional layered structure of the MXene material, so that the agglomeration of the material is effectively overcome, the collapse of the MXene layer structure is prevented, and the energy density of the composite material is improved.
(2) The invention adopts MXene as a substrate and acts as a three-dimensional conductive network framework, thereby greatly improving the conductivity and mechanical strength of the composite material. By doping the MXene material with sulfur, active sites on the MXene material can be increased, so that the MXene material and the transition metal sulfide are combined more tightly. The large specific surface area of the MXene material can relieve the volume expansion of the transition metal sulfide in the charging and discharging processes, so that the material has good stability. The MXene material has hydrophilicity and affinity to polysulfide, can adsorb polysulfide generated in electrochemical reaction, limits shuttle effect of polysulfide, and improves electrochemical performance and service life of the negative electrode material.
(3) The preparation method is simple and the preparation process is environment-friendly. The sulfur-doped MXene/metal sulfide-based battery cathode material disclosed by the invention has excellent long-cycle stability, high energy density and excellent rate performance, and can be applied to various fields.
Drawings
Fig. 1 is an X-ray diffraction diagram of the MXene material of example 1.
Fig. 2 is a graph showing cycle characteristics of the negative electrode material prepared in example 2.
Fig. 3 is a graph of rate performance of the negative electrode material prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
All materials in the examples are commercially available.
Example 1
(1) 1g of manganese nitrate powder and 1g of Ti were weighed respectively3C2Adding the powder into a beaker, adding 200ml of deionized water for dissolving, mixing and stirring for 5 hours, then carrying out suction filtration and drying to obtain Ti3C2Manganese nitrate mixture;
(2) taking 1g of Ti prepared in the step (1) in a nitrogen atmosphere3C2The manganese nitrate mixture and 1g of thioacetamide are put into a tube furnace, the temperature is raised to 550 ℃ at the heating rate of 2 ℃/min and is kept for 2.5 hours, and Ti is obtained3C2Manganese sulfide composite material;
(3) taking 80g of Ti prepared in the step (2)3C2Mixing the manganese sulfide composite material, 10g of SP, 10g of CMC and water to prepare slurry, and coating the slurry on carbon cloth to obtain the cathode material (Ti) of the sulfur-doped MXene/metal sulfide-based composite battery3C2/MnS)。
FIG. 1 shows MXene material Ti in this example3C2As can be seen from the figure, MXene has a distinct peak of (002) crystal plane, and the surface MXene has a certain interlayer spacing and can be combined with other materials between layers.
Example 2
(1) 1g of cobalt sulfate powder and 0.2g of Ti were weighed out separately2Adding the powder C into a beaker, adding 300ml of deionized water for dissolving, mixing and stirring for 12 hours, then carrying out suction filtration and drying to obtain Ti2A C/cobalt sulfate mixture;
(2) taking 1g of Ti prepared in the step (1) in a nitrogen atmosphere2Placing the C/cobalt sulfate mixture and 3g of ammonium persulfate into a tube furnace, heating to 400 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 4 hours to obtain Ti2C/cobalt sulfide composite material;
(3) taking 75g of Ti prepared in the step (2)2Preparing a slurry from the C/cobalt sulfide composite material, 15g of conductive carbon black, 10g of PAA and water, and coating the slurry on copper foil to obtain the sulfur-doped MXene/metal sulfide-based composite battery negative electrode material (Ti)2C/CoS)。
Assembling the sulfur-doped MXene/metal sulfide-based composite battery cathode material prepared in the step (3) and a lithium sheet into a lithium ion half battery, and testing the electrochemical performance of the lithium ion half battery by charging and discharging at a current of 1A/g within a voltage range of 0-3V.
Fig. 2 is a graph of cycle performance of the sulfur-doped MXene/metal sulfide-based composite battery anode material prepared in the present example. As can be seen from the figure, the cathode material has good cycling stability, still has very high capacity after 1000 cycles of 1A cycling, and has good electrochemical performance.
Example 3
(1) Separately weighing 1g of antimony chloride powder and 0.5g of V4C3Adding the powder into a beaker, adding 300ml of deionized water for dissolving, mixing and stirring for 24 hours, carrying out suction filtration and drying to obtain V4C3Antimony chloride mixture;
(2) under a nitrogen atmosphere, taking 1g of V prepared in the step (1)4C3Putting the antimony chloride mixture and 1g of cysteine into a tubular furnace, heating to 900 ℃ at the heating rate of 20 ℃/min, and keeping the temperature for 6 hours to obtain V4C3Antimony sulfide mixture;
(3) taking 70g of V prepared in the step (2)4C3Mixing antimony sulfide mixture, 20g SP, 10g CMC and water to prepare slurry, coating the slurry on a carbon-coated copper foil to obtain the sulfur-doped MXene/metal sulfide-based composite battery negative electrode material (V)4C3/Sb2S3)。
Assembling the sulfur-doped MXene/metal sulfide-based composite battery cathode material prepared in the step (3) and a lithium sheet into a lithium ion half battery, and testing the electrochemical performance of the lithium ion half battery by charging and discharging at a current of 1A/g within a voltage range of 0-3V. Fig. 3 is a rate performance curve diagram of the sulfur-doped MXene/metal sulfide-based composite battery anode material prepared in the present embodiment. As can be seen from the figure, the negative electrode material has good rate performance, a certain capacity still exists during charging and discharging under high rate, and the capacity does not obviously attenuate after the charging and discharging under high rate and low rate, so that the negative electrode material has good electrochemical performance.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of MXene/metal sulfide composite material is characterized by comprising the following steps:
(1) mixing and stirring metal salt of transition metal element and MXene material with water, then carrying out solid-liquid separation, and drying to obtain MXene/metal salt mixture;
(2) mixing the MXene/metal salt mixture prepared in the step (1) with a sulfur source under a protective atmosphere, heating to 300-900 ℃, and preserving heat for 1-6 hours to obtain the MXene/metal sulfide composite material.
2. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the transition metal element in the step (1) is at least one of tin, antimony, cobalt, iron, titanium, molybdenum and manganese.
3. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the metal salt of the transition metal element in the step (1) is at least one of nitrate, carbonate, sulfate and chloride of the transition metal element.
4. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the MXene material in the step (1) is Ti3C2、Ti2C、V4C3、Ta4C3、Ta2C、Mo2Ta2C3、V2C、Mo4C3、Mo2C、Nb4C3、Nb2C and Cr2C.
5. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the stirring time in the step (1) is 3-48 h.
6. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the sulfur source in the step (2) is at least one of thioacetamide, ammonium persulfate, thiourea, sodium sulfide and cysteine.
7. The method of preparing MXene/metal sulfide composite material according to claim 1, wherein:
the mass ratio of the metal salt of the transition metal element in the step (1), the MXene material and the sulfur source in the step (2) is (1-100): (1-100): (5-400).
8. An MXene/metal sulfide composite material, characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. The use of the MXene/metal sulfide composite material of claim 8 in the field of battery negative electrode material preparation.
10. A sulfur-doped MXene/metal sulfide-based composite battery anode material, comprising the MXene/metal sulfide composite material of claim 8.
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| CN111710862A (en) * | 2020-06-28 | 2020-09-25 | 山东大学 | 3D porous Sb/Ti for high-performance potassium ion battery3C2Preparation method of MXene composite material |
| 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 |
| CN111755262A (en) * | 2020-07-10 | 2020-10-09 | 大连理工大学 | CoS/Ti applied to super capacitor3C2Preparation method of (1) |
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