CN114335485A - Tri-metal yolk shell structure material and preparation method and application thereof - Google Patents
Tri-metal yolk shell structure material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of new materials, relates to a lithium ion battery cathode material, and particularly relates to a tri-metal yolk shell structural materialMaterial prepared from Mn, its preparation method and application0.5Zn0.5Co2O4Complexing with carbon to form nanoparticles, Mn0.5Zn0.5Co2O4Coated with a carbon layer, Mn0.5Zn0.5Co2O4Is in a yolk shell structure; the preparation method comprises the following steps: adding manganese salt, zinc salt and cobalt salt into a mixed solvent of glycerol and isopropanol to carry out solvothermal reaction to obtain a precursor containing Zn, Co and Mn, and calcining the precursor in the air atmosphere to obtain the Mn with the trimetal core-shell structure0.5Zn0.5Co2O4Adding Mn in a trimetal core-shell structure0.5Zn0.5Co2O4Coating dopamine on the surface, and then calcining in an inert atmosphere to obtain the coating. The tri-metal yolk shell structure material provided by the invention can be used as a high-performance advanced negative electrode material.
Description
Technical Field
The invention belongs to the technical field of new materials, relates to a lithium ion battery cathode material, and particularly relates to a tri-metal yolk shell structure material and a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
However, according to the research of the inventor, the synthesis of the metal oxide with the yolk shell structure is mainly focused on a hard template and a soft template, the preparation process is complicated, and a large amount of raw materials are consumed.
Meanwhile, the inventor also finds that the synthesis of the metal oxide is mainly focused on single metal and bimetal, and the synergistic effect of multiple metals cannot be effectively utilized.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a trimetal yolk shell structure material, a preparation method and application thereof, and an advanced cathode material with controllable morphology and high performance is obtained while the synergistic effect of trimetal oxide is fully utilized.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in one aspect, a trimetal yolk shell structure material is prepared from Mn0.5Zn0.5Co2O4Complexing with carbon to form nanoparticles, Mn0.5Zn0.5Co2O4Coated with a carbon layer, Mn0.5Zn0.5Co2O4Is in yolk shell structure.
The method comprises the steps of feeding Zn and Mn according to a proportion to form trimetal Mn0.5Zn0.5Co2O4the/C not only makes the chemical element composition of the material rich, but also makes the ion composition of the synthesized material more complex due to the multiple oxidation states of Mn and Zn, forms rich defect sites, and simultaneously makes Mn, Co and Mn act synergistically, thereby making Mn rich0.5Zn0.5Co2O4the/C material has excellent electrochemical performance. Secondly, the material synthesized by the method is a yolk shell structure, and the yolk shell structure can provide larger specific surface area and porosity and can effectively buffer Li+Volume expansion during intercalation/deintercalation, and in addition, the yolk shell structure can shorten Li+The diffusion path of (2) accelerates the permeation of the electrolyte.
On the other hand, the preparation method of the trimetal yolk shell structure material comprises the steps of adding manganese salt, zinc salt and cobalt salt into a mixed solvent of glycerol and isopropanol to carry out solvothermal reaction to obtain a precursor containing Zn, Co and Mn, and calcining the precursor in the air atmosphere to obtain the trimetal yolk shell structure Mn0.5Zn0.5Co2O4Adding Mn in a trimetal core-shell structure0.5Zn0.5Co2O4Coating dopamine on the surface, and then calcining in an inert atmosphere to obtain the coating.
The preparation method can improve the dispersibility of the trimetal yolk shell structure material, thereby improving the electrochemical performance of the material.
In a third aspect, the three-metal yolk shell structure material is applied to a lithium ion battery cathode material and/or a lithium ion battery.
The trimetal yolk shell structure material provided by the invention is used as a lithium ion battery cathode and/or for preparing a lithium ion battery, and has more excellent electrochemical performance.
In a fourth aspect, the lithium ion battery negative electrode comprises a current collector, a binder and an active ingredient, wherein the active ingredient is the three-metal yolk shell structure material.
In a fifth aspect, a lithium ion battery includes a lithium ion positive electrode, an electrolyte, and the lithium ion battery negative electrode.
The invention has the beneficial effects that:
1. the three-metal yolk shell structure material is formed, only one temperature variable is needed, and the synthesis method is simple and easy to operate.
2. The method adopts the solvent-thermal method in cooperation with the calcination method to prepare the tri-metal yolk shell structure material, and the preparation process is safe and environment-friendly.
3. The method for calcining the trimetal cobalt, manganese and zinc precursor has low temperature and short calcining time, and can reduce energy consumption.
4. The material provided by the invention is of a yolk shell structure, so that the specific surface area can be increased, and the contact area of the electrode and electrolyte is increased; can also provide additional gaps, and effectively lighten Li+Volume change and mechanical strain during the insertion/extraction process.
5. The material provided by the invention is a trimetal system, can fully play the synergistic effect of different metal ions, provides higher specific capacity and improves the electrochemical performance.
6. The tri-metal yolk shell structure material provided by the invention has a rich pore size structure, and is beneficial to further permeation of electrolyte in an electrochemical circulation process and acceleration of electron ion transmission.
7. The trimetal yolk shell structure material provided by the invention has good dispersibility and no obvious aggregation, reduces the interfacial resistance in the charge transfer process, and further improves the electrochemical performance.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows Mn of a trimetal yolk shell structure prepared in example 1 of the present invention0.5Zn0.5Co2O4Wide angle X-ray diffraction patterns (XRD);
FIG. 2 shows Mn of the tri-metal yolk shell structure prepared in example 1 of the present invention0.5Zn0.5Co2O4(ii) electron micrographs of/C, (a) Transmission Electron Micrograph (TEM) and (b) Scanning Electron Micrograph (SEM);
FIG. 3 shows Mn of the tri-metal yolk shell structure prepared in example 1 of the present invention0.5Zn0.5Co2O4A charge-discharge performance curve diagram of/C;
FIG. 4 shows Mn of the tri-metal yolk shell structure prepared in example 1 of the present invention0.5Zn0.5Co2O4Long cycle performance plot of/C.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the fact that templates are needed to be adopted in the existing preparation of the yolk shell structure material, the preparation process is complex, and meanwhile, multiple metal materials cannot be effectively utilized in a synergistic mode, the invention provides a trimetal yolk shell structure material and a preparation method and application thereof.
In one exemplary embodiment of the present invention, a trimetal yolk shell structure material is provided, which is made from Mn0.5Zn0.5Co2O4Complexing with carbon to form nanoparticles, Mn0.5Zn0.5Co2O4Coated with a carbon layer, Mn0.5Zn0.5Co2O4Is in yolk shell structure.
The trimetal yolk shell structure material provided by the invention not only can form rich defect sites by utilizing various oxidation states of Zn, Co and Mn, but also can enable the Zn, Co and Mn to act synergistically, so that the material has excellent electrochemical performance, and can provide larger specific surface area and porosity, thereby effectively buffering Li+Volume expansion during intercalation/deintercalation and further improve electrochemical performance.
In some examples of this embodiment, the nanoparticles are between 300 and 350 nm.
In some examples of this embodiment, the yolk structure has a diameter of 75 to 80 nm.
In some examples of this embodiment, the eggshell structure has a thickness of 30 nm to 35 nm.
In some examples of this embodiment, the carbon layer has a thickness of 13 to 17 nm.
In some examples of this embodiment, Mn0.5Zn0.5Co2O4Is of spinel structure.
In another embodiment of the invention, a preparation method of the above trimetal yolk shell structure material is provided, wherein a manganese salt, a zinc salt and a cobalt salt are added into a mixed solvent of glycerol and isopropanol to carry out solvothermal reaction to obtain a precursor containing Zn, Co and Mn, and the precursor is calcined in an air atmosphere to obtain the trimetal core-shell structure Mn0.5Zn0.5Co2O4Adding Mn in a trimetal core-shell structure0.5Zn0.5Co2O4Coating dopamine on the surface, and then calcining in an inert atmosphere to obtain the coating.
The preparation method can improve the dispersibility of the trimetal yolk shell structure material, thereby improving the electrochemical performance of the material.
In some examples of this embodiment, the molar ratio of manganese salt, zinc salt, and cobalt salt is 1:0.9 to 1.1:1.9 to 2.1.
In some examples of this embodiment, the solvothermal reaction is at a temperature of 150 to 200 ℃.
In some embodiments of this embodiment, the temperature of the calcined precursor is from 400 to 500 ℃.
In some examples of this embodiment, the calcining temperature after coating with dopamine is 550 to 600 ℃.
The preferred steps of the invention are:
(1) adding zinc salt, cobalt salt and manganese salt into a mixed solution of isopropanol and glycerol, and stirring;
(2) carrying out solvothermal reaction on the solution prepared in the step (1), and cooling after the solvothermal reaction to obtain pink precipitate;
(3) separating, washing and drying the pink precipitate obtained in the step (2), grinding and calcining in the air atmosphere to obtain Mn with a core-shell structure0.5Zn0.5Co2O4；
(4) The core-shell structure Mn obtained in the step (3)0.5Zn0.5Co2O4Adding into Tris solution, adding dopamine, stirring, centrifuging, washing and drying to obtain Mn0.5Zn0.5Co2O4/PDA。
(5) Mn obtained in the step (4)0.5Zn0.5Co2O4Calcining PDA in inert atmosphere to obtain Mn0.5Zn0.5Co2O4and/C, namely the three-metal yolk shell structure material.
Specifically, in the step (1), the stirring time is 1-2 hours, and the optimal stirring time is 2 hours.
In the step (2), the solvothermal conditions are as follows: reacting for 6-10 h at 180-200 ℃, and preferably keeping the temperature of 180 ℃ for 8h under the solvothermal condition.
In the step (3), the calcination condition is 400-500 ℃ for 1-2 h, and the calcination temperature is preferably 400 ℃ for 2 h.
In the step (4), the stirring time is 4-8 h, and the optimal stirring time is 6 h.
In the step (5), the calcination temperature is 550-600 ℃, and the optimal temperature is 600 ℃.
The invention provides an application of the tri-metal yolk shell structure material as a lithium ion battery cathode material and/or in preparation of a lithium ion battery.
The trimetal yolk shell structure material provided by the invention is used as a lithium ion battery cathode and/or for preparing a lithium ion battery, and has more excellent electrochemical performance.
In a fourth embodiment of the invention, a lithium ion battery negative electrode is provided, which comprises a current collector, a binder and an active ingredient, wherein the active ingredient is the above three-metal yolk shell structure material.
In a fifth embodiment of the present invention, there is provided a lithium ion battery including a lithium ion positive electrode, an electrolyte, and the lithium ion battery negative electrode.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
A100 mL beaker was placed on a magnetic stirrer, 40mL of isopropanol and 10mL of glycerol were added, and 0.125mmol of Zn (NO) was added to the solvent with stirring3)2·6H2O、0.25mmol Co(NO3)2·6H2O、0.125mmol MnCl2The solution was stirred for 2h to dissolve completely to form a pink solution. The resulting pink solution was transferred to a 100mL reaction vessel and subjected to solvothermal reaction at 180 ℃ for 8 h. After cooling, the pink solution was centrifuged and washed. Drying the washed precipitate at 70 ℃ for 12h, grinding the dried precipitate, calcining at 400 ℃ for 2h to obtain Mn with a core-shell structure0.5Zn0.5Co2O4. Mixing 80mgMn0.5Zn0.5Co2O4Adding into 100mL of Tirs solution, adding dopamine, stirring for 6h, centrifuging, washing, drying, and adding Ar gasCalcining at the medium temperature of 600 ℃ for 2h to obtain Mn with an egg yolk shell structure0.5Zn0.5Co2O4/C。
core-Shell Mn obtained in this example0.5Zn0.5Co2O4The XRD of the material is shown in figure 1, the prepared material corresponds to a spinel structure, and the enlarged view of figure 1b shows that Mn is0.5Zn0.5Co2O4Just above the characteristic peak of ZnCo2O4And MnCo2O4In between, Mn is proved0.5Zn0.5Co2O4The preparation is successful. FIG. 2 shows Mn obtained0.5Zn0.5Co2O4Morphology of/C, from which the Mn produced can be seen0.5Zn0.5Co2O4the/C is a yolk shell structure, wherein the diameter of the yolk shell-shaped nanosphere is 320nm, the diameter of the inner core is about 78nm, the thickness of the outer shell is about 34nm, and the thickness of the carbon layer is about 15 nm.
Example 2
A100 mL beaker was placed on a magnetic stirrer, 40mL of isopropanol and 10mL of glycerol were added, and 0.125mmol of Zn (NO) was added to the solvent with stirring3)2·6H2O、0.25mmol Co(NO3)2·6H2O、0.125mmol MnCl2The solution was stirred for 1.5h to dissolve completely to form a pink solution. The resulting pink solution was transferred to a 100mL reaction vessel and subjected to solvothermal reaction at 180 ℃ for 6 h. After cooling, the pink solution was centrifuged and washed. Drying the washed precipitate at 70 ℃ for 12h, grinding the dried precipitate, calcining at 400 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4. Mixing 80mgMn0.5Zn0.5Co2O4Adding into 100mL of Tirs solution, adding dopamine, stirring for 6h, centrifuging, washing, drying, calcining in Ar gas at 600 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4/C。
Example 3
Placing 100mL beaker on magnetic stirrer, adding 40mL isopropanol and 10mL glycerol, and adding into solvent under stirring0.125mmol of Zn (NO)3)2·6H2O、0.25mmol Co(NO3)2·6H2O、0.125mmol MnCl2The solution was stirred for 1h to dissolve completely to form a pink solution. The resulting pink solution was transferred to a 100mL reaction vessel and subjected to solvothermal reaction at 180 ℃ for 8 h. After cooling, the pink solution was centrifuged and washed. Drying the washed precipitate at 70 ℃ for 12h, grinding the dried precipitate, calcining at 500 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4. Mixing 80mgMn0.5Zn0.5Co2O4Adding into 100mL of Tirs solution, adding dopamine, stirring for 10h, centrifuging, washing, drying, calcining in Ar gas at 600 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4/C。
Example 4
A100 mL beaker was placed on a magnetic stirrer, 40mL of isopropanol and 10mL of glycerol were added, and 0.125mmol of Zn (NO) was added to the solvent with stirring3)2·6H2O、0.25mmol Co(NO3)2·6H2O、0.125mmol MnCl2The solution was stirred for 1.5h to dissolve completely to form a pink solution. The resulting pink solution was transferred to a 100mL reaction vessel and subjected to solvothermal reaction at 180 ℃ for 6 h. After cooling, the pink solution was centrifuged and washed. Drying the washed precipitate at 70 ℃ for 12h, grinding the dried precipitate, calcining at 400 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4. Mixing 80mgMn0.5Zn0.5Co2O4Adding into 100mL of Tirs solution, adding dopamine, stirring for 10h, centrifuging, washing, drying, and calcining at 500 ℃ in Ar gas for 2h to obtain Mn0.5Zn0.5Co2O4/C。
Example 5
A100 mL beaker was placed on a magnetic stirrer, 40mL of isopropanol and 10mL of glycerol were added, and 0.125mmol of Zn (NO) was added to the solvent with stirring3)2·6H2O、0.25mmol Co(NO3)2·6H2O、0.125mmol MnCl2The solution was stirred for 2h to dissolve completely to form a pink solution. The resulting pink solution was transferred to a 100mL reaction vessel and subjected to solvothermal reaction at 160 ℃ for 6 h. After cooling, the pink solution was centrifuged and washed. Drying the washed precipitate at 70 ℃ for 12h, grinding the dried precipitate, calcining at 500 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4. Mixing 80mgMn0.5Zn0.5Co2O4Adding into 100mL of Tirs solution, adding dopamine, stirring for 6h, centrifuging, washing, drying, calcining in Ar gas at 600 ℃ for 2h to obtain Mn0.5Zn0.5Co2O4/C。
Example 6
A lithium ion battery, the electrode material of which adopts Mn with a three-metal yolk shell structure in example 10.5Zn0.5Co2O4C, Mn in a trimetal yolk shell structure0.5Zn0.5Co2O4the/C material is used as a negative electrode, a lithium sheet is used as a positive electrode, the diaphragm is a polypropylene film, and the electrolyte is LiPF6And a mixed solution of ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate. Firstly, putting prepared Mn with a trimetal yolk shell structure into a positive electrode shell0.5Zn0.5Co2O4And C, dropwise adding electrolyte into the material C, putting a diaphragm, dropwise adding the electrolyte again, adding a lithium sheet, sequentially putting a gasket and an elastic sheet, and finally putting a negative electrode shell to obtain the lithium ion battery. Through experimental verification, as shown in fig. 3 and 4, the lithium ion battery has good application in the electrochemical field. Meanwhile, FIG. 4 compares Mn0.5Zn0.5Co2O4C and ZnCo2O4C and MnCo2O4At 200mA g/C-1The performance of 100 times of charging and discharging can be found by comparing the graphs, and Mn0.5Zn0.5Co2O4the/C has better electrochemical performance.
Wherein, ZnCo2O4/C、MnCo2O4Preparation method of/C and Mn0.5Zn0.5Co2O4The preparation method of the/C is the same, except that: with 0.25mmol Zn (NO)3)2·6H2O、0.25mmol Co(NO3)2·6H2Preparation of ZnCo from O2O4C, with 0.25mmol of Co (NO)3)2·6H2O、0.25mmol MnCl2Preparation of MnCo2O4/C。
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A three-metal yolk shell structure material is characterized by comprising Mn0.5Zn0.5Co2O4Complexing with carbon to form nanoparticles, Mn0.5Zn0.5Co2O4Coated with a carbon layer, Mn0.5Zn0.5Co2O4Is in yolk shell structure.
2. The trimetal yolk shell structured material of claim 1, wherein the nanoparticles are between 300 and 350 nm;
or the diameter of the yolk structure is 75-80 nm;
or the thickness of the eggshell structure is 30-35 nm;
or the thickness of the carbon layer is 13-17 nm.
3. The trimetal yolk shell structured material of claim 1, wherein Mn is present0.5Zn0.5Co2O4Is of spinel structure.
4. A method for preparing a trimetal yolk shell structure material as defined in any one of claims 1 to 3, wherein manganese salt, zinc salt and cobalt salt are added to a mixed solvent of glycerin and isopropanol to carry out solvothermal reaction to obtain a compound containing Zn, Co,Calcining the precursor of Mn in the air atmosphere to obtain the Mn with the trimetal core-shell structure0.5Zn0.5Co2O4Adding Mn in a trimetal core-shell structure0.5Zn0.5Co2O4Coating dopamine on the surface, and then calcining in an inert atmosphere to obtain the coating.
5. The method for preparing a trimetal yolk shell structure material of claim 4, wherein the molar ratio of manganese salt, zinc salt and cobalt salt is 1: 0.9-1.1: 1.9-2.1.
6. The method for preparing a trimetal yolk shell structure material of claim 4, wherein the temperature of the solvothermal reaction is 150-200 ℃.
7. The method of preparing a trimetal yolk shell structure material of claim 4, wherein the temperature of the calcined precursor is 400-500 ℃;
or the calcining temperature after coating the dopamine is 550-600 ℃.
8. The application of the trimetal yolk shell structure material as defined in any one of claims 1 to 3 in serving as a lithium ion battery negative electrode material and/or preparing a lithium ion battery.
9. A lithium ion battery negative electrode, which comprises a current collector, a binder and an active ingredient, and is characterized in that the active ingredient is the trimetal yolk shell structure material of any one of claims 1 to 3.
10. A lithium ion battery comprising a lithium ion positive electrode, an electrolyte and the lithium ion battery negative electrode according to claim 9.
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