CN111769263A - Three-dimensional C/Fe3O4Lithium ion battery cathode material and preparation method thereof - Google Patents
Three-dimensional C/Fe3O4Lithium ion battery cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional C/Fe3O4Lithium ion battery negative electrode material and preparation method thereof, and three-dimensional C/Fe3O4The lithium ion battery cathode material is prepared by taking cellulose as a template and ferric salt as a precursor, firstly loading ferric ions on the template through impregnation treatment, and then calcining under inert atmosphere. Three-dimensional C/Fe prepared by the invention3O4The negative electrode material of the lithium ion battery can be gramClothes made of Fe3O4The defects of poor conductivity of the cathode material and large volume change in circulation can greatly improve Fe3O4Electrochemical properties of the negative electrode.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to three-dimensional C/Fe3O4A lithium ion battery cathode material and a preparation method thereof.
Background
Compared with carbon materials, transition metal oxides (MxOy, M ═ Fe, Co, Cu, and Ti) as negative electrode materials of lithium ion batteries have higher theoretical capacity, better safety performance, and rate capability, and attract attention of people. Wherein Fe3O4More on account of its high theoretical capacity (927 mAhg)-1)Highest electron conductivity (σ 2 × 10)4S/m is superior to other transition metal oxides), has the advantages of rich resources, no toxicity, environmental friendliness, good corrosion resistance, low cost and the like, and is favored. However, Fe3O4The violent volume change (more than 200%) in the charging and discharging process causes the iron to be pulverized, fall off, agglomerated and the like, even loses electric contact, and seriously hinders Fe3O4The lithium ion battery cathode material is practically applied.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides three-dimensional C/Fe3O4A lithium ion battery cathode material and a preparation method thereof, aiming at improving Fe3O4The negative electrode material has the defects of poor conductivity and large volume change in circulation, and improves Fe3O4Electrochemical properties of the negative electrode.
The invention provides three-dimensional C/Fe3O4The lithium ion battery cathode material is prepared by taking cellulose as a template and ferric salt as a precursor, firstly loading ferric ions on the template through impregnation treatment, and then calcining the iron ions in an inert atmosphereProcessing to obtain the three-dimensional C/Fe3O4A lithium ion battery cathode material.
Preferably, the weight ratio of the cellulose to the iron salt is 1 (0.2-7).
Preferably, the cellulose is citric acid modified bacterial cellulose.
Preferably, the preparation method of the citric acid modified bacterial cellulose comprises the following steps: adding the bacterial cellulose into an aqueous solution of citric acid, stirring for 30-60 min at 20-80 ℃, then washing until the pH value is 4-8, and drying to obtain the bacterial cellulose.
Preferably, the weight ratio of the bacterial cellulose to the citric acid is 1 (0.2-3).
Preferably, the diameter of the bacterial cellulose is 40-60 nm.
Preferably, the bacterial cellulose is synthesized by a microorganism of the genus acetobacter, agrobacterium rhizobium or sarcina; more preferably, the bacterial cellulose is synthesized by acetobacter xylinum.
Preferably, the iron salt is a trivalent iron salt.
The three-dimensional C/Fe3O4The preparation method of the lithium ion battery negative electrode material comprises the following steps:
s1, adding cellulose into an aqueous solution of ferric salt for dipping treatment, then filtering and drying, and repeating dipping, filtering and drying treatment for a plurality of times;
and S2, calcining the material obtained in the step S1 in an inert atmosphere, and cooling to obtain the catalyst.
Preferably, in step S1, the conditions of the immersion treatment are: the temperature is 30-40 ℃, and the dipping time is 5-8 h.
Preferably, in step S2, the calcining conditions are: and in a nitrogen atmosphere, raising the temperature to 300-500 ℃ at a heating rate of 3-6 ℃/min, and preserving the temperature for 1-3 h.
The invention has the following beneficial effects:
since cellulose has a three-dimensional structure, the porosity of the structure can increase the contact area between the electrolyte and the electrode surface, and the large specific surface area can promote the electricity of the electrode/electrolyte interfaceThe charge is transferred, active substances in the hole walls are in direct contact with electrolyte, so that the transmission path of ions can be reduced, the porous nano structure can easily process discrete active substance nano particles, and a small amount of binder can be used or even no binder can be used in some cases; the active substance in the large space can inhibit the volume change of the active substance in the charge and discharge process, and the porous composite material can show a second conductive phase to improve the conductivity of the battery. Therefore, the invention synthesizes three-dimensional C/Fe by taking cellulose as a template3O4The lithium ion battery cathode material has a three-dimensional interpenetrating network structure provided by taking cellulose as a template, has larger space and specific surface area, and can contain Fe3O4The volume expansion generated in the charging and discharging process effectively releases the stress, and effectively solves the problem of the traditional Fe3O4The problem of severe volume expansion exists; but also greatly shortens the transmission path of electrons and lithium ions and increases Fe3O4Contact area with electrolyte, increase utilization rate, and improve Fe3O4The defects of poor conductivity of the negative electrode material and large volume change in circulation effectively improve Fe3O4Electrochemical properties of the negative electrode.
Furthermore, the citric acid modified bacterial cellulose is selected as the template, so that the adsorption performance on metal ions can be greatly improved, the load of iron ions on the template is promoted, and the Fe content is improved3O4Binding capacity to three-dimensional networks, resulting in better improvement of three-dimensional C/Fe3O4The electrochemical performance of the lithium ion battery cathode material.
Drawings
FIG. 1 is a three-dimensional C/Fe of the present invention3O4The synthetic route of the lithium ion battery cathode material is shown schematically.
FIG. 2 is a three-dimensional C/Fe of the present invention3O4Scanning Electron Micrographs (SEM) of the lithium ion battery negative electrode material.
FIG. 3 is a three-dimensional C/Fe of the present invention3O4Lithium ion battery cathode material and conventional Fe3O4And (3) a cycle performance diagram of the lithium ion battery negative electrode material under the current density of 250 mA.
FIG. 4 is a three-dimensional C/Fe of the present invention3O4Lithium ion battery cathode material and conventional Fe3O4And (3) a rate performance diagram of the lithium ion battery cathode material.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Preparing citric acid modified bacterial cellulose:
dissolving 3.84g of citric acid in 200mL of water to prepare a citric acid aqueous solution, adding 5g of bacterial cellulose with the diameter of 40-60nm into the citric acid aqueous solution, stirring and reacting at 20 ℃ for 30min, washing until the pH value is 6-7, and drying to obtain the citric acid modified bacterial cellulose.
Preparation of three-dimensional C/Fe3O4Lithium ion battery negative electrode material:
s1, firstly, 1.35g of FeCl3·6H2Dissolving O in 20mL of water to prepare FeCl3·6H2O water solution, 5g of the citric acid modified bacterial cellulose prepared above is added into FeCl3·6H2Soaking in O water solution at 30 deg.C for 5 hr, filtering, drying, and repeating soaking, filtering, and drying for 2 times;
s2, heating the material obtained in the step S1 to 300 ℃ at a heating rate of 3 ℃/min in a nitrogen atmosphere, preserving heat for 1h, and cooling to obtain the three-dimensional C/Fe3O4A lithium ion battery cathode material.
Example 2
Preparing citric acid modified bacterial cellulose:
dissolving 11.52g of citric acid in 200mL of water to prepare a citric acid aqueous solution, adding 5g of bacterial cellulose with the diameter of 40-60nm into the citric acid aqueous solution, stirring and reacting at 80 ℃ for 60min, washing until the pH value is 6-7, and drying to obtain the citric acid modified bacterial cellulose.
Preparation of three-dimensional C/Fe3O4Lithium ion battery negative electrode material:
s1, firstly 33.83g FeCl3·6H2Dissolving O in 100mL of water to prepare FeCl3·6H2O water solution, 5g of the citric acid modified bacterial cellulose prepared above is added into FeCl3·6H2Soaking in O water solution at 40 deg.C for 8 hr, filtering, drying, and repeating soaking, filtering, and drying for 3 times;
s2, heating the material obtained in the step S1 to 500 ℃ at a heating rate of 6 ℃/min in a nitrogen atmosphere, preserving heat for 3h, and cooling to obtain the three-dimensional C/Fe3O4A lithium ion battery cathode material.
Example 3
Preparing citric acid modified bacterial cellulose:
dissolving 10g of citric acid in 200mL of water to prepare a citric acid aqueous solution, adding 5g of bacterial cellulose with the diameter of 40-60nm into the citric acid aqueous solution, stirring and reacting at 60 ℃ for 40min, washing until the pH value is 6-7, and drying to obtain the citric acid modified bacterial cellulose.
Preparation of three-dimensional C/Fe3O4Lithium ion battery negative electrode material:
s1, 13.5g FeCl is firstly added3·6H2Dissolving O in 50mL of water to prepare FeCl3·6H2O water solution, 5g of the citric acid modified bacterial cellulose prepared above is added into FeCl3·6H2Soaking in O water solution at 35 deg.C for 6 hr, filtering, drying, and repeating soaking, filtering, and drying for 2 times;
s2, heating the material obtained in the step S1 to 400 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2h, and cooling to obtain the three-dimensional C/Fe3O4A lithium ion battery cathode material.
As can be seen from FIG. 2, three-dimensional C/Fe3O4The lithium ion battery cathode material has a three-dimensional interpenetrating network structure, Fe3O4The nanoparticles are encapsulated by a flexible carbon mesh.
As can be seen from FIG. 3, three-dimensional C/Fe3O4The lithium ion battery cathode material has excellent cycle stability, and the number of cycles of 700 weeks can still be maintained at 800mThe reversible capacity of Ah/g greatly improves Fe3O4The lithium ion battery can be used alone as the cycle performance of the lithium battery negative electrode material.
As can be seen from FIG. 4, the dimension C/Fe3O4The lithium ion battery cathode material has excellent rate performance, which shows that the expansion of active substances can be effectively relieved by the conventional three-dimensional porous structure, and the interpenetrating structure provides a quick channel for lithium ions and electrons, so that the rate performance is improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. Three-dimensional C/Fe3O4The lithium ion battery cathode material is characterized in that cellulose is used as a template, ferric salt is used as a precursor, ferric ions are loaded on the template through dipping treatment, and then the three-dimensional C/Fe is obtained through calcination treatment in inert atmosphere3O4A lithium ion battery cathode material.
2. Three-dimensional C/Fe of claim 13O4The lithium ion battery cathode material is characterized in that the weight ratio of the cellulose to the ferric salt is 1 (0.2-7).
3. Three-dimensional C/Fe of claim 13O4The lithium ion battery negative electrode material is characterized in that the cellulose is citric acid modified bacterial cellulose.
4. Three-dimensional C/Fe of claim 13O4The lithium ion battery negative electrode material is characterized in that the preparation method of the citric acid modified bacterial cellulose comprises the following steps: adding the bacterial cellulose into an aqueous solution of citric acid, stirring for 30-60 min at 20-80 ℃, then washing until the pH value is 4-8, and drying to obtain the bacterial cellulose。
5. Three-dimensional C/Fe of claim 43O4The lithium ion battery negative electrode material is characterized in that the weight ratio of the bacterial cellulose to the citric acid is 1 (0.2-3).
6. Three-dimensional C/Fe according to claim 4 or 53O4The lithium ion battery negative electrode material is characterized in that the diameter of the bacterial cellulose is 40-60 nm.
7. Three-dimensional C/Fe according to any of claims 1-63O4The lithium ion battery cathode material is characterized in that the ferric salt is a trivalent ferric salt.
8. Three-dimensional C/Fe of any of claims 1-73O4The preparation method of the lithium ion battery cathode material is characterized by comprising the following steps:
s1, adding cellulose into an aqueous solution of ferric salt for dipping treatment, then filtering and drying, and repeating dipping, filtering and drying treatment for a plurality of times;
and S2, calcining the material obtained in the step S1 in an inert atmosphere, and cooling to obtain the catalyst.
9. Three-dimensional C/Fe of claim 83O4The preparation method of the lithium ion battery negative electrode material is characterized in that in the step S1, the conditions of the dipping treatment are as follows: the temperature is 30-40 ℃, and the dipping time is 5-8 h.
10. Three-dimensional C/Fe of claim 93O4The preparation method of the lithium ion battery negative electrode material is characterized in that in the step S2, the calcining conditions are as follows: and in a nitrogen atmosphere, raising the temperature to 300-500 ℃ at a heating rate of 3-6 ℃/min, and preserving the temperature for 1-3 h.
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