CN112234186B - MXene nanodot coated modified lithium ion battery cathode material and preparation method thereof - Google Patents
MXene nanodot coated modified lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
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Abstract
The invention discloses an MXene nanodot-coated modified lithium ion battery anode material and a preparation method thereof, wherein the MXene nanodot-coated modified lithium ion battery anode material is composed of an MXene nanodot material and a lithium ion battery anode material, the MXene nanodot material is coated on the surface of the lithium ion battery anode material, the particle size of the MXene nanodot material is 3-20 nm, and the coating amount of the MXene nanodot material accounts for 0.5-10% of the total mass of the MXene nanodot material and the lithium ion battery anode material.
Description
Technical Field
The invention relates to the field of secondary batteries, in particular to an MXene nanodot-coated modified lithium ion battery cathode material and a preparation method thereof.
Background
The lithium ion battery has the advantages of long cycle life, high power density, high energy density, high voltage platform and the like, is widely used in the field of electronic products such as mobile phones and portable computers at present, but is still difficult to meet the requirements of products such as electric automobiles and electric tools on multiplying power performance and cycle performance. The positive electrode material is a key factor affecting the performance of the battery.
In order to improve the cycling stability of the positive electrode material (NCA) of lithium ion batteries, researchers have generally employed surface coating and the like to avoid direct contact between the electrolytes of the materials, the coating layers being generally electrochemically inert oxides, phosphates and fluorides, however, the above coating materials are semiconductor materials or insulator materials, which increases the number of timesThe polarization of the anode reduces electrochemical indexes such as capacity, rate performance and the like of the anode material. In order to avoid polarization increase of the anode, researchers coat the surface of the anode material of the lithium ion battery by adopting conductive oxides, conductive polymers and carbon materials with electronic conductive properties, and effectively improve the rate capability of the material. Among the above three types of electron conductive materials, the carbon material has the best conductivity. However, carbon materials are suitable for coating lithium ion battery positive electrode materials synthesized in a reducing atmosphere, such as LiFePO 4 ，Li 3 V 2 (PO 4 ) 3 And the like, are not suitable for coating a lithium ion battery cathode material synthesized in an oxidizing atmosphere because: if the coating material and the anode material are tightly combined, the phenomenon that the coating falls off and the cycle performance is not improved ideally due to volume expansion and shrinkage in the lithium desorption process of the anode material is avoided, the material needs to be roasted at high temperature in the air or oxygen atmosphere at the final stage of the coating process, but the carbon material is burnt to generate carbon dioxide in the oxidizing atmosphere.
MXene material is an emerging two-dimensional layered structure material with electronic conductivity similar to that of a metal material. MXene materials can withstand firing in air, oxygen, and inert atmospheres. Therefore, the MXene material is used for coating the surface of the lithium ion battery anode material, is more favorable for improving the electronic conductivity of the surface of the material and improving the rate capability of the material, and is suitable for the lithium ion battery anode material synthesized in an oxidizing atmosphere and a reducing atmosphere. However, the conventional MXene material has a two-dimensional sheet layered structure with a micron size, and most of the positive electrode materials of lithium ion batteries are also in the micron size, so that it is difficult to coat the MXene material with the micron size on the surface of the positive electrode material.
Disclosure of Invention
Aiming at the defects and defects mentioned in the background technology, the invention aims to provide an MXene nanodot-coated modified lithium ion battery cathode material and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme that the lithium ion battery anode material coated and modified by the MXene nanodots is composed of the MXene nanodot material and the lithium ion battery anode material, the MXene nanodot material is coated on the surface of the lithium ion battery anode material, and the coating amount of the MXene nanodots accounts for 0.5-10% of the total mass of the MXene nanodots and the lithium ion battery anode material.
Preferably, the MXene nanodot material is a metal carbide or nitride material M n+1 X n Wherein M is Sc, Ti, Zr, V, Nb, Cr, Mo, Hf, etc., X represents C or N element, N is 1, 2, 3; the particle size of the MXene nanodot material is 3-20 nm.
Preferably, the positive electrode material of the lithium ion battery is a positive electrode material having a layered structure, a spinel structure, or an olivine structure.
The invention also discloses a preparation method of the lithium ion battery anode material coated and modified by MXene nanodots, which comprises the following steps,
step one, preparing the MXene nanodot material:
preparing MXene nanodot material: preparing a MXene nanosheet material with a micron size by etching an A layer in an MAX phase (M is an early transition metal, A is a main group element and X is carbon or nitrogen atoms) of a three-dimensional layered structure by acid etching or electrochemical etching; then, cutting MXene nanosheets into MXene nanodot materials by adopting a hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 100-150 ℃, the reaction time is 2-6 h, centrifugally washing dispersion liquid obtained after the reaction for 3-8 times by using deionized water, and freeze-drying to obtain the MXene nanodot materials;
step two, preparing the MXene nanodot-coated lithium ion battery anode material:
firstly, adding chitosan oligosaccharide into an aqueous solution to prepare a solution with the concentration of 0.5-1 mg/mL, and adding acid to adjust the pH to be less than 5 so as to hydrolyze chitosan oligosaccharide to obtain NH 4 + And then the positive electricity is charged, the MXene nanodots obtained in the step one are added, and ultrasonic dispersion is carried out for 1-24 hours to obtain a positive electricity chitosan adsorbed MXene nanodot material; preparing 0.2-1 mg/mL pectin solution, Carboxyl (COO) of pectin - ) And (3) enabling the material to be negatively charged, then adding the lithium ion battery anode material, and continuously stirring for 0.5-1 h to obtain the pectin-adsorbed lithium ion battery anode material with negative charge. Will be provided withAdding the MXene nanodot dispersion liquid adsorbed by chitosan into the lithium ion battery anode material dispersion liquid adsorbed by pectin, stirring for 1-5 h, completely and uniformly coating MXene nanodots on the surface of the lithium ion battery anode material due to the electrostatic acting force and the hydrogen bond acting force between the chitosan and the pectin, filtering and drying, and carrying out heat treatment on the obtained product at 400-800 ℃ for 0.5-2 h in an oxygen atmosphere to obtain the MXene nanodot-coated lithium ion battery anode material; adjusting acid of the chitosan oligosaccharide solution to be hydrochloric acid, acetic acid or sulfuric acid; the mass ratio of the lithium ion battery anode material to the MXene nanodots obtained in the first step is 100: (0.5 to 10); the mass ratio of the chitosan oligosaccharide to the pectin is (0.1-0.8): 1.
preferably, the reaction temperature for preparing the MXene nanodots by hydrothermal cutting of the MXene nanosheets in the first step is 140 ℃.
Preferably, the reaction time for preparing the MXene nanodots by hydrothermal cutting of the MXene nanosheets in the first step is 3 h.
Preferably, the mass ratio of the chitosan oligosaccharide and the pectin in the second step is 0.6: 1.
preferably, the mass ratio of the lithium ion battery anode material obtained in the step two to the MXene nanodots obtained in the step one is 100: 5.
compared with the prior art, the invention has the advantages that:
(1) the MXene nanodots coated with the MXene nanodots prepared by the method have more uniform size of 3-20 nm. The MXene nanodots are used for adsorbing positively charged chitosan and negatively charged pectin respectively, so that the MXene nanodots can be coated on the surface of the lithium ion battery positive material more uniformly and completely under the action of static electricity and hydrogen bonds. From SEM images and TEM images (figure 1 and figure 2), it can be seen that the NCA cathode material coated with MXene nanodots prepared by the method has good coating effect, the MXene nanodots are uniformly and completely coated on the surface of the NCA material, and the coating thickness is about 40 nm.
(2) The MXene nanodot-coated lithium ion battery anode material prepared by the method improves the LiNi of the lithium ion battery anode material 0.8 Co 0.15 Al 0.05 O 2 Magnification of (2)Performance and cycling performance (fig. 3 and 4). LiNi at 5C multiplying power in a voltage range of 3-4.3V 0.8 Co 0.15 Al 0.05 O 2 The capacity of the material is 110 mAh/g-120 mAh/g, and the MXene nano-dots are coated with LiNi 0.8 Co 0.15 Al 0.05 O 2 The capacity of the material is 130 mAh/g-140 mAh/g, and is improved by 18 mAh/g-20 mAh/g. In the voltage range of 3-4.3V, the 1C multiplying power is cycled for 200 times, LiNi 0.8 Co 0.15 Al 0.05 O 2 The capacity retention rate of the material is 83-88%, and the porous graphene is coated with LiNi 0.8 Co 0.15 Al 0.05 O 2 The capacity retention rate of the material is improved by 10-15%.
(3) The MXene nanodot-coated lithium ion battery anode material prepared by the method not only solves the problem of poor electronic conductivity caused by coating of semiconductor and insulator materials such as oxide, phosphate and fluoride on the anode material, but also solves the problem that subsequent high-temperature treatment cannot be carried out under an oxidizing atmosphere when the carbon material is coated, and the MXene nanodot material is suitable for lithium ion battery anode materials synthesized under various inert and oxidizing atmospheres. The MXene nanodot coating can reduce polarization, improve the capacity and rate performance of the material, reduce the contact area between the material and electrolyte, reduce side reaction and improve the structural stability of the material.
Drawings
FIG. 1 is Ti of example 1 of the present invention 3 C 2 Lithium ion battery anode material LiNi coated with MXene nanodots 0.8 Co 0.15 Al 0.05 O 2 SEM picture of (a);
FIG. 2 shows Ti in example 1 of the present invention 3 C 2 Lithium ion battery anode material LiNi coated with MXene nanodots 0.8 Co 0.15 Al 0.05 O 2 A TEM picture of (4);
FIG. 3 shows LiNi, a positive electrode material for a lithium ion battery according to example 1 of the present invention 0.8 Co 0.15 Al 0.05 O 2 And Ti 3 C 2 MXene nanodot-coated LiNi 0.8 Co 0.15 Al 0.05 O 2 Multiplying power of materialA performance curve;
FIG. 4 shows LiNi, a positive electrode material for a lithium ion battery according to example 1 of the present invention 0.8 Co 0.15 Al 0.05 O 2 And Ti 3 C 2 MXene nanodot-coated LiNi 0.8 Co 0.15 Al 0.05 O 2 Cycle performance curve of the material.
Detailed Description
The invention is further described in the following with reference to the drawings and the specific examples of the description, but without thereby limiting the scope of protection of the invention.
Example 1:
mixing Ti, Al and graphite powder according to the molar ratio of Ti to Al to C of 3:1:2, ball-milling for 2 hours to obtain a mixed raw material, and then preparing Ti by carrying out vacuum hot-pressing sintering on the raw material 3 AlC 2 MAX phase, wherein the adopted sintering temperature is 1300 ℃, the sintering time is 3h, and the vacuum degree is 6.5 × 10 -3 Pa. Then, Ti was etched away with a 48% HF solution 3 AlC 2 Al element in MAX phase to obtain micron-sized Ti 3 C 2 MXene nanoplatelets. Then, Ti is reacted by hydrothermal reaction 3 C 2 Cutting MXene nano sheet into Ti 3 C 2 The hydrothermal reaction temperature of the MXene nanodot material is 140 ℃, the reaction time is 4h, the dispersion liquid obtained after the reaction is centrifugally washed by deionized water for 3-8 times, and the Ti is obtained after freeze drying 3 C 2 MXene nanodot material.
10mL of chitosan oligosaccharide aqueous solution with the concentration of 0.6mg/mL is prepared, the pH is adjusted to 4.5 by adding acetic acid, and then 10mg of Ti with the mass is added 3 C 2 MXene nanodots are ultrasonically dispersed for 10h to obtain Ti 3 C 2 MXene nanodot dispersion; preparing 20mL of 0.5mg/mL pectin solution, adding 1g of lithium ion battery anode material, and continuously stirring for 0.5-1 h to obtain the lithium ion battery anode material dispersion solution. Adding the lithium ion battery anode material dispersion liquid into Ti 3 C 2 Stirring MXene nanodot dispersion liquid for 2h, filtering and drying the material, and then carrying out heat treatment on the obtained powder at 450 ℃ for 1.5h in an oxygen atmosphere to obtain Ti 3 C 2 MXene nanodot packageCoated lithium ion battery positive electrode materials. Ti (titanium) 3 C 2 Lithium ion battery anode material LiNi coated with MXene nanodots 0.8 Co 0.15 Al 0.05 O 2 Shown in FIG. 1, the SEM picture of (A) is that of Ti 3 C 2 Lithium ion battery anode material LiNi coated with MXene nanodots 0.8 Co 0.15 Al 0.05 O 2 Is shown in fig. 2.
Ti 3 C 2 MXene nanodot-coated LiNi 0.8 Co 0.15 Al 0.05 O 2 The rate capability of the material is shown in figure 3, the first discharge capacity is 181.12mAh/g, the 0.5C rate capacity is 165.17mAh/g, and the 5C rate capacity is 130.40mAh/g in a voltage range of 3-4.3V and at 0.1C rate. Ti 3 C 2 MXene nanodot-coated LiNi 0.8 Co 0.15 Al 0.05 O 2 The cycle performance of the material is shown in FIG. 4, the voltage range of 3-4.3V, 1C cycle 200 times, and the capacity retention rate is 97%.
Claims (8)
1. An MXene nanodot-coated modified lithium ion battery cathode material is characterized in that: the lithium ion battery anode material is composed of an MXene nanodot material and a lithium ion battery anode material, wherein the MXene nanodot material is coated on the surface of the lithium ion battery anode material, the coating amount of the MXene nanodots accounts for 0.5-10% of the total mass of the MXene nanodot material and the lithium ion battery anode material, and the MXene nanodot material is a metal carbide or nitride material M n+1 X n Wherein M is Sc, Ti, Zr, V, Nb, Cr, Mo, Hf, X represents C or N element, N is 1, 2, 3.
2. The positive electrode material of the lithium ion battery coated and modified by MXene nanodots according to claim 1, characterized in that: the particle size of the MXene nanodot material is 3-20 nm.
3. The positive electrode material of the lithium ion battery coated and modified by MXene nanodots according to claim 1, characterized in that: the positive electrode material of the lithium ion battery is a positive electrode material with a layered structure, a spinel structure or an olivine structure.
4. A preparation method of the lithium ion battery cathode material coated and modified by the MXene nanodots is used for preparing the lithium ion battery cathode material coated and modified by the MXene nanodots in any one of claims 1 to 3, and is characterized by comprising the following steps,
step one, preparing the MXene nanodot material: etching the A layer in the MAX phase of the three-dimensional layered structure by acid etching or electrochemical etching to prepare a micron-sized MXene nanosheet material; then, cutting MXene nanosheets into MXene nanodot materials by adopting a hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 100-150 ℃, the reaction time is 2-6 h, centrifugally washing dispersion liquid obtained after the reaction for 3-8 times by using deionized water, and freeze-drying to obtain the MXene nanodot materials;
step two, preparing the MXene nanodot-coated lithium ion battery anode material: firstly, adding chitosan oligosaccharide into an aqueous solution to prepare a solution with the concentration of 0.5-1 mg/mL, adjusting the pH to be less than 5 by adding acid, then adding the MXene nanodots obtained in the first step, and performing ultrasonic dispersion for 1-24 hours to obtain an MXene nanodot material adsorbed by chitosan; preparing 0.2-1 mg/mL of pectin solution, adding a lithium ion battery anode material, continuously stirring for 0.5-1 h to obtain a pectin-adsorbed lithium ion battery anode material, adding MXene nanodot dispersion liquid adsorbed by chitosan into the pectin-adsorbed lithium ion battery anode material dispersion liquid, stirring for 1-5 h to ensure that MXene nanodots are completely and uniformly coated on the surface of the lithium ion battery anode material, filtering and drying, and carrying out heat treatment on the obtained product at 400-800 ℃ for 0.5-2 h in an oxygen atmosphere to obtain the MXene nanodot-coated lithium ion battery anode material; adjusting acid of the chitosan oligosaccharide solution to be hydrochloric acid, acetic acid or sulfuric acid; the mass ratio of the lithium ion battery anode material to the MXene nanodots obtained in the first step is 100: 0.5 to 10; the mass ratio of the chitosan oligosaccharide to the pectin is 0.1-0.8: 1.
5. the preparation method of the MXene nanodot-coated modified lithium ion battery cathode material according to claim 4, wherein the preparation method comprises the following steps: the reaction temperature for preparing the MXene nanodots by hydrothermal cutting of the MXene nanosheets in the first step is 140 ℃.
6. The preparation method of the MXene nanodot-coated modified lithium ion battery cathode material according to claim 4, wherein the preparation method comprises the following steps: the reaction time for preparing the MXene nanodots by hydrothermal cutting of the MXene nanosheets in the first step is 3 h.
7. The preparation method of the MXene nanodot-coated modified lithium ion battery cathode material according to claim 4, wherein the preparation method comprises the following steps: the mass ratio of the chitosan oligosaccharide to the pectin in the second step is 0.6: 1.
8. the preparation method of the MXene nanodot-coated modified lithium ion battery cathode material according to claim 4, wherein the preparation method comprises the following steps: the mass ratio of the lithium ion battery anode material obtained in the step two to the MXene nanodots obtained in the step one is 100: 5.
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