CN111333119A - Two-dimensional carbide crystal MXene-based iron oxide negative electrode material and preparation method and application thereof - Google Patents
Two-dimensional carbide crystal MXene-based iron oxide negative electrode material and preparation method and application thereof Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000013078 crystal Substances 0.000 title claims abstract description 50
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 16
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 15
- 150000002505 iron Chemical class 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims 7
- 239000010406 cathode material Substances 0.000 abstract description 18
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
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- 229910052742 iron Inorganic materials 0.000 abstract 1
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000007385 chemical modification Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
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- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention relates to a two-dimensional carbide crystal MXene-based ferric oxide cathode material and a preparation method and application thereof, and the method comprises the steps of dissolving ferric salt in deionized water to obtain ferric salt solution, adding MXene aqueous solution into the ferric salt solution, carrying out magnetic stirring and ultrasonic treatment, carrying out hydrothermal reaction for 10-14 hours at the temperature of 70-90 ℃, obtaining a product after reaction, repeatedly washing by deionized water, and finally carrying out vacuum drying to obtain the two-dimensional carbide crystal MXene-based ferric oxide cathode materialAn iron negative electrode material. Compared with the prior art, the MXene-based iron oxide cathode material of the two-dimensional carbide crystal prepared by the invention has the concentration of 100 mA.g‑1The capacity of the battery can reach 800 mAh.g under the charge-discharge current‑1And the initial capacity can be stably recovered after 4000 cycles, so that the lithium ion battery has high reversible capacity, very good cycle stability, greenness and sustainability, and has wide application prospect in the field of lithium ion batteries.
Description
Technical Field
The invention belongs to the technical field of material science and electrochemistry, and particularly relates to a two-dimensional carbide crystal MXene-based iron oxide cathode material as well as a preparation method and application thereof.
Background
With the development and progress of the automobile industry, the continuous development problem of human beings faces huge challenges. The combustion of non-renewable fuels can release various exhaust gases, leading to various problems. Therefore, it is important to find renewable and sustainable energy storage devices. The rechargeable battery is economical, environment-friendly, high in power and long in service life, and compared with non-renewable energy, the rechargeable battery realizes continuous utilization of energy. Particularly, lithium ion batteries are one of the most important rechargeable and dischargeable batteries because of their advantages such as high energy density, no memory effect, and small self-discharge effect.
The lithium ion battery is composed of four most important parts, namely positive and negative electrode materials, electrolyte, a diaphragm and the like. The lithium ion battery cathode material is a main body of lithium storage of the lithium ion battery and has the advantages of large capacity, low potential, high charge-discharge reaction reversibility and the like. Graphite is currently the most widely used negative electrode material, but has much room for improvement because the specific energy density of the negative electrode is still lower than that of the positive electrode. For example, when graphene is used as a negative electrode material, although the lithium storage capacity of the lithium ion battery can be improved, the requirements of the power battery cannot be met due to the defects of insufficient specific capacity, slightly low stability of the layered structure, excessively low charge and discharge platform and the like. In recent years, research has focused on the research of high specific capacity negative electrode materials.
The two-dimensional carbide crystal (MXene) which can be used as a negative electrode material is a novel two-dimensional material, belongs to transition metal carbon/nitride, and the precursor of the two-dimensional carbide crystal is MAX-phase. The MAX-phase is a general term of a series of ternary layered compounds, wherein M represents a transition group metal element, A is a main group element, X is carbon and/or nitrogen in the MAX phase, X atoms are filled into an octahedral structure formed by close stacking of M atoms, and A atoms are positioned between MX layers. In 2011 scientists found that the appearance of MXene is very sandwich-like, and as a new class of two-dimensional materials, MXene, which is a two-dimensional carbide crystal nano material composed of oxide, carbon and metal filler, has good hydrophilicity imparted to MXene by functional groups generated in the MAX-phase etching process, and the conductivity of MXene is not significantly influenced. Therefore, due to the intrinsic two-dimensional nano-layered structure, good hydrophilicity, excellent conductivity and mechanical property of MXene, the Mxene-based material is widely applied to compounding of electrode materials in the fields of energy storage and conversion, and has wide application prospects in various fields such as lithium ion electrodes, super capacitors, photo (electro) catalyst electrodes and the like.
Iron oxide is the main component of rust. The main cause of rust is that iron metal reacts with moisture and oxygen in the environment in the presence of carbon as an impurity, and then rust is generated. Used for coloring paints, rubbers, plastics, buildings, etc., are inorganic pigments, and are used as rust-preventive pigments in the coating industry. Used as a colorant for rubber, artificial marble, and floor terrazzo, a colorant and filler for plastics, asbestos, artificial leather, leather slurry, etc., a polishing agent for precision instruments and optical glass, and a raw material for manufacturing ferrite elements which are magnetic materials, etc. Iron oxide has been increasingly emphasized in environmental regulations due to its stable chemical properties, high specific surface area and fine particle structure. However, the iron oxide has disadvantages that firstly, the final product is the rod-shaped nano iron oxide, the size of the nano iron oxide is smaller, and the rod-shaped appearance of the iron oxide makes the nano iron oxide more easily agglomerated, so that the nano iron oxide is not very beneficial to being used for adsorbing and decomposing organic matters; secondly, the price of the raw material hydrogen peroxide used in the preparation method is high, and the temperature and time during the reaction are too high and too long, so that the production cost is difficult to reduce, and the commercial application of the final product is not facilitated.
Research shows that the composite material has good conductivity after being compounded with some high-conductivity base materials (such as graphene, carbon fibers and two-dimensional carbide crystals), wherein the two-dimensional carbide crystal base materials can assist the growth of the material and provide structural support for the whole material while providing conductivity.
At present, regarding the method for modifying iron oxide by using MXene as a two-dimensional carbide crystal, mainly in the aspect of chemical modification, for example, CN 109904426A is used for preparing a composite material of iron oxide and MXene through in-situ chemical composite modification, so as to improve the electrochemical performance of the iron oxide. However, such means of chemical modification have some inevitable disadvantages, firstly, due to the agglomeration that may occur before the chemical modification, the adsorption and decomposition of the subsequent functional groups are not favoured; secondly, the surface tension of the particles can be changed by in-situ modification, the growth mode is influenced, a part of two-dimensional carbide crystal substrate material is subjected to the function of structural support, the excellent conductivity of the two-dimensional carbide crystal substrate material cannot be exerted, and the electrochemical performance of the composite material is influenced. In view of this, it is critical to explore a more uniform and more efficient compound method.
Disclosure of Invention
The invention aims to solve the problems and provide a two-dimensional carbide crystal MXene-based iron oxide negative electrode material, and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a two-dimensional carbide crystal MXene-based ferric oxide negative electrode material comprises the steps of dissolving ferric salt in deionized water to obtain a ferric salt solution, adding the MXene aqueous solution into the ferric salt solution, carrying out magnetic stirring and ultrasonic treatment, carrying out hydrothermal reaction for 10-14 hours at the temperature of 70-90 ℃, obtaining a product after reaction, repeatedly washing with deionized water, and finally carrying out vacuum drying to obtain the two-dimensional carbide crystal MXene-based ferric oxide negative electrode material.
Preferably, the iron salt is ferric chloride.
Preferably, the hydrothermal reaction is carried out at a temperature of 80 ℃ for 12 hours.
Preferably, the mass ratio of the iron salt to the deionized water to the MXene is 15-20: 1: 1.
further preferably, the mass ratio of the iron salt to the deionized water to the MXene is 16:1: 1.
preferably, the concentration of MXene in the MXene aqueous solution is 10-15 mg/mL.
Further preferably, the concentration of MXene in the MXene aqueous solution is 11 mg/mL.
Preferably, the magnetic stirring time is 10-15 minutes and the sonication time is 10-15 minutes.
The two-dimensional carbide crystal MXene-based iron oxide negative electrode material is used as a negative electrode material of a lithium ion battery.
The invention compounds ferric oxide and two-dimensional carbide crystal MXene, FeCl3Hydrolysis reaction in waterFe should be formed3+When the cations and the two-dimensional carbide crystal MXene are mixed together through hydrothermal reaction, the cations and the two-dimensional carbide crystal MXene can be compounded more uniformly through the closed environment and electrostatic interaction, and the particle agglomeration is reduced. The two-dimensional carbide crystal has high specific surface area, high conductivity and excellent chemical stability, so that the two-dimensional carbide crystal can be effectively compounded very stably. The composite material has higher specific surface area and more electron transmission channels, has more excellent electrical properties, and is expected to be applied to lithium ion batteries as a negative electrode material.
Compared with the prior art, the invention has the following advantages:
1. the MXene-based iron oxide cathode material of the two-dimensional carbide crystal is prepared by a hydrothermal method, in the hydrothermal process, the assembly of the MXene structure of the two-dimensional carbide crystal and the in-situ uniform polymerization of iron oxide on the surface of the MXene substrate can be completed in one step, and the method is simple and convenient;
2. the hydrothermal reaction is carried out under the conditions of 70-90 ℃ and 10-14 hours, compared with other methods, the method has the advantages of short time, high temperature avoidance, closed hydrothermal reaction environment and high reaction efficiency and is easy to operate, wherein the two can be very stably and effectively compounded, and the compounded material has higher specific surface area and more electron transmission channels and more excellent electrical properties;
3. the concentration of MXene in the MXene aqueous solution is 10-15mg/mL, the concentration is high, the addition amount is small, and the MXene aqueous solution has more excellent electrical properties;
4. the composite material is prepared by taking the ferric chloride and the MXene as raw materials, and the raw materials are easy to obtain, designable and low in cost;
5. the two-dimensional carbide crystal MXene-based iron oxide cathode material prepared by the method has good electrical properties, high reversible capacity, good cycle stability, greenness and sustainability, and has wide application prospects in the field of lithium ion batteries.
Drawings
FIG. 1 is an SEM topography of MXene-based iron oxide of two-dimensional carbide crystals obtained in example 1;
FIG. 2 is a graph of the cycle performance of MXene-based iron oxide two-dimensional carbide crystals obtained in example 1 as a negative electrode material of a lithium ion battery;
FIG. 3 is a graph showing rate capability of MXene-based iron oxide, a two-dimensional carbide crystal, obtained in example 1, as a negative electrode material for a lithium ion battery.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The preparation method of the MXene-based iron oxide cathode material with the two-dimensional carbide crystals comprises the following steps:
(1) dissolving 640mg ferric chloride in 40ml deionized water;
(2) preparing an MXene aqueous solution into a solution with the concentration of 11mg/ml, and carrying out ultrasonic treatment on the solution to form a uniformly mixed dispersion liquid;
(3) slowly dripping the dispersion into a ferric chloride aqueous solution, magnetically stirring for 10 minutes, and carrying out ultrasonic treatment for 10 minutes; wherein the mass ratio of the added ferric chloride, the deionized water and the MXene is 16:1: 1;
(4) carrying out hydrothermal reaction on the solution at 80 ℃ for 12 hours;
(5) repeatedly washing the material obtained by the hydrothermal method by deionized water, and finally drying the material in vacuum to obtain a two-dimensional carbide crystal MXene-based iron oxide cathode material, wherein the shape and appearance of the two-dimensional carbide crystal MXene-based iron oxide cathode material are shown in figure 1, as can be seen from figure 1, the cathode material prepared by the method has a nanoscale, and the iron oxide is coated on the surface of MXene, so that stable and good combination can be seen;
(6) the obtained composite material is used as a lithium ion battery negative electrode material to assemble a lithium ion button type half battery, the composite material, carbon black (Super-P) and polyvinylidene fluoride (PVDF) are mixed according to the weight ratio of 7:2:1, then the mixture is uniformly coated on pure aluminum foil (99.6%) by a coating method to prepare a negative electrode, a pure lithium sheet is used as a counter electrode, the button type half battery is used for electrochemical test, and a cycle performance diagram and a multiplying power performance diagram of the battery are respectively shown in figures 2 and 3As shown in FIG. 2, the negative electrode material prepared by the present invention has a high reversible capacity at 100mA · g-1The capacity of the battery can reach 800 mAh.g under the charge-discharge current-1(ii) a As can be seen from FIG. 3, the cathode material prepared by the invention has very good cycle stability, and the initial capacity can be stably recovered after 4000 cycles, so that the iron oxyhydroxide/two-dimensional carbide crystal MXene cathode material prepared by the invention has wide application prospects in the field of lithium ion batteries.
Example 2
The preparation method of the MXene-based iron oxide cathode material with the two-dimensional carbide crystals comprises the following steps:
(1) dissolving 640mg ferric chloride in 40ml deionized water;
(2) preparing an MXene aqueous solution into a solution with the concentration of 10mg/ml, and carrying out ultrasonic treatment on the solution to form a uniformly mixed dispersion liquid;
(3) slowly dripping the dispersion into a ferric chloride aqueous solution, magnetically stirring for 15 minutes, and carrying out ultrasonic treatment for 15 minutes; wherein the mass ratio of the added ferric chloride, the deionized water and the MXene is 16:1: 1;
(4) carrying out hydrothermal reaction on the solution at 70 ℃ for 14 hours;
(5) and repeatedly washing the material obtained by the hydrothermal process by using deionized water, and finally drying the material in vacuum to obtain the MXene-based iron oxide cathode material of the two-dimensional carbide crystal.
Example 3
The preparation method of the MXene-based iron oxide cathode material with the two-dimensional carbide crystals comprises the following steps:
(1) dissolving 800mg of ferric chloride in 40ml of deionized water;
(2) preparing MXene aqueous solution into solution with the concentration of 13mg/ml, and carrying out ultrasonic treatment on the solution to form uniformly mixed dispersion liquid;
(3) slowly dripping the dispersion into a ferric chloride aqueous solution, magnetically stirring for 10 minutes, and carrying out ultrasonic treatment for 10 minutes; wherein the mass ratio of the added ferric chloride, the deionized water and the MXene is 20:1: 1;
(4) carrying out hydrothermal reaction on the solution at 90 ℃ for 10 hours;
(5) and repeatedly washing the material obtained by the hydrothermal process by using deionized water, and finally drying the material in vacuum to obtain the MXene-based iron oxide cathode material of the two-dimensional carbide crystal.
Example 4
The preparation method of the MXene-based iron oxide cathode material with the two-dimensional carbide crystals comprises the following steps:
(1) dissolving 640mg ferric chloride in 40ml deionized water;
(2) preparing an MXene aqueous solution into a solution with the concentration of 15mg/ml, and carrying out ultrasonic treatment on the solution to form a uniformly mixed dispersion liquid;
(3) slowly dripping the dispersion into a ferric chloride aqueous solution, magnetically stirring for 12 minutes, and carrying out ultrasonic treatment for 12 minutes; wherein the mass ratio of the added ferric chloride, the deionized water and the MXene is 16:1: 1;
(4) carrying out hydrothermal reaction on the solution at 85 ℃ for 13 hours;
(5) and repeatedly washing the material obtained by the hydrothermal process by using deionized water, and finally drying the material in vacuum to obtain the MXene-based iron oxide cathode material of the two-dimensional carbide crystal.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a two-dimensional carbide crystal MXene-based iron oxide negative electrode material is characterized by comprising the steps of dissolving iron salt in deionized water to obtain an iron salt solution, adding an MXene aqueous solution into the iron salt solution, carrying out magnetic stirring and ultrasonic treatment, carrying out hydrothermal reaction for 10-14 hours at the temperature of 70-90 ℃, obtaining a product after reaction, repeatedly washing with deionized water, and finally carrying out vacuum drying to obtain the two-dimensional carbide crystal MXene-based iron oxide negative electrode material.
2. The method for preparing the MXene-based iron oxide anode material with the two-dimensional carbide crystals according to claim 1, wherein the iron salt is ferric chloride.
3. The method for preparing the MXene-based iron oxide anode material with the two-dimensional carbide crystals as claimed in claim 1, wherein the hydrothermal reaction is carried out at a temperature of 80 ℃ for 12 hours.
4. The preparation method of the MXene-based iron oxide anode material with the two-dimensional carbide crystals as claimed in claim 1, wherein the mass ratio of the iron salt to the deionized water to MXene is 15-20: 1: 1.
5. the method for preparing the MXene-based iron oxide anode material with the two-dimensional carbide crystals according to claim 4, wherein the mass ratio of the iron salt to the MXene is 16:1: 1.
6. the method for preparing the MXene-based iron oxide anode material with the two-dimensional carbide crystals as claimed in claim 1, wherein the concentration of MXene in the MXene aqueous solution is 10-15 mg/mL.
7. The method for preparing the MXene-based iron oxide anode material with the two-dimensional carbide crystals as claimed in claim 6, wherein the concentration of MXene in the MXene aqueous solution is 11 mg/mL.
8. The preparation method of the two-dimensional carbide crystal MXene-based iron oxide negative electrode material as claimed in claim 1, wherein the magnetic stirring time is 10-15 minutes, and the ultrasonic time is 10-15 minutes.
9. The MXene-based iron oxide anode material of two-dimensional carbide crystals prepared by the preparation method according to any one of claims 1 to 8.
10. The two-dimensional carbide crystal MXene-based iron oxide negative electrode material of claim 9 as a negative electrode material of a lithium ion battery.
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