CN110957489A - Porous iron oxide negative electrode material and preparation method and application thereof - Google Patents
Porous iron oxide negative electrode material and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention belongs to the technical field of battery materials, and particularly relates to a porous iron oxide negative electrode material and a preparation method and application thereof. The preparation method comprises the steps of reacting solid organic acid with ferric nitrate, calcining, mixing with a carbon source, and calcining again to obtain a finished product. The cycle life of the finished product in the battery charging and discharging process is remarkably prolonged, the contact area between the finished product and electrolyte can be increased due to the porous structure of the finished product, more active sites are provided, and the multiplying power capability is improved.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to a porous iron oxide negative electrode material and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIB) are stable due to their high energy density and cyclingQualitative and design flexibility are considered to be preferred power sources for energy storage devices, transportation devices, and other electronic devices. Metal Organic Frameworks (MOFs) can be used as direct electrode materials for LIBs, are composed of metal ions and organic ligands, have the advantages of adjustable porosity, large surface area and the like, and represent a new class of mixed porous materials. Fe2O3Belongs to one of transition metal oxides, has the advantages of high theoretical capacity (about 1007mAh/g), low cost and rich resources, and can be used as a negative electrode material for preparing MOFs. However Fe2O3The disadvantage of large volume change and low conductivity during repeated charge/discharge results in Fe2O3The anode material has the defects of poor cycling capability and poor rate capability, so that the practical application of the anode material in the LIB is not optimistic.
Disclosure of Invention
For Fe2O3The invention provides a preparation method of a porous iron oxide negative electrode material, which is used for solving the problems of poor cycle capacity and poor rate capability of the negative electrode material.
The invention also provides a porous iron oxide negative electrode material.
The invention also provides application of the porous ferric oxide negative electrode material in preparation of a lithium ion battery.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of a porous iron oxide negative electrode material specifically comprises the following steps:
dissolving solid organic acid and ferric nitrate in a solvent, adding a catalyst, stirring for 30-60 min, reacting for 10-30 min at 60-120 ℃, washing and drying the obtained product after the reaction is finished, and calcining for 10-20 min at 300-500 ℃ to obtain a primary product;
grinding and mixing the obtained primary product and a carbon source, and calcining for 10-30 min at 300-500 ℃ in an inert atmosphere; wherein the solid organic acid is at least one of terephthalic acid and fumaric acid.
The preparation method of the invention firstly obtains a primary product, namely nano-grade Fe through reaction and primary calcination2O3. The solid organic acid species and the combined action of the reaction temperature and the reaction time lead the obtained nanoscale Fe2O3The particles of (a) are smaller and uniform in morphology, having reduced absolute volume change and shortened ion and electron transfer distances compared to their bulk counterparts during repeated charge/discharge processes, thereby increasing their cycle life; the time and temperature of the first calcination enable the organic components to be completely calcined, and the calcination process does not need to limit the atmosphere, so that the process requirement is low. Then, the nanoscale Fe2O3Mixing with carbon source, calcining in inert atmosphere to oxidize iron to generate partial iron simple substance and promote carbon source to generate graphite carbon, so as to realize nano-scale Fe2O3The carbon coating on the surface further reduces the volume change, improves the conductivity of the obtained product, improves the specific discharge capacity and ensures that the obtained product has better electrochemical performance. The invention prepares the nano-scale carbon-coated porous iron oxide cathode material by a simple method, the material has longer cycle life in the process of charging and discharging the battery, and the porous structure can increase the contact area between the material and the electrolyte, increase the number of active sites and improve the multiplying power capability.
As can be seen by a scanning electron microscope and a transmission electron microscope, the porous iron oxide negative electrode material prepared by the preparation method has a uniform morphology, and a scanning electron microscope image (SEM image) is shown in figure 2, and a transmission electron microscope image (TEM image) is shown in figure 3. According to TEM images, the porous iron oxide negative electrode material has a uniform coating layer with the thickness of 5-20 microns, and the crystal lattice stripes prove that the composition of the phase of the coating layer is a graphitized carbon layer which is graphite carbon generated by secondary calcination in an inert atmosphere.
The ferric nitrate in the preparation method can be selected from anhydrous substances or nonahydrate thereof.
Preferably, the catalyst is 4-Dimethylaminopyridine (DMAP), which promotes the formation of an organometallic framework to produce nanoscale Fe2O3More uniform morphology can be obtained at lower temperatures and shorter holding times.
Preferably, the mass of the catalyst is 1-10% of the mass of the organic acid.
Preferably, the solvent is N, N-Dimethylformamide (DMF). The use of the solvent can make the product appearance better.
Preferably, the mass of the solvent is 0.1-0.3 times of the mass of the organic acid.
Preferably, the mass ratio of the solid organic acid to the ferric nitrate is 0.1-0.5: 1.
Preferably, the carbon source is at least one of β -cyclodextrin, γ -cyclodextrin, methyl- β -cyclodextrin, 2-hydroxypropyl- β -cyclodextrin, (2-hydroxypropyl) - γ -cyclodextrin, 2, 6-di-O-methyl- β -cyclodextrin and hepta (2,3, 6-tri-O-methyl) - β -cyclodextrin.
Preferably, the mass ratio of the carbon source to the primary product is 0.5-2: 1.
The embodiment of the invention also provides a porous iron oxide negative electrode material which is prepared by the preparation method of the porous iron oxide negative electrode material.
The embodiment of the invention also provides application of the porous ferric oxide negative electrode material in preparation of a lithium ion battery. After the porous ferric oxide negative electrode material is prepared into the lithium ion battery, the obtained battery has obviously higher specific discharge capacity than the lithium ion battery prepared by the conventional ferric oxide under the high rate of 10C, and still has higher cycle retention rate after 200 cycles of cycling at the high temperature of 60 ℃. Due to the existence of the carbon coating layer, an alternating current impedance test (EIS) shows that the ionic conductivity of the lithium ion battery is obviously improved and the performance of the lithium ion battery is obviously improved compared with that of a conventional iron oxide sample after 100 cycles.
Drawings
FIG. 1 is a schematic process flow diagram of an embodiment of the present invention;
FIG. 2 is an SEM image of a porous iron oxide negative electrode material in example 1 of the present invention;
fig. 3 is a TEM image of the porous iron oxide anode material in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a porous iron oxide negative electrode material, and the preparation method comprises the following steps:
42mg of fumaric acid and 160mg of Fe (NO)3)3·9H2O (containing 95.8mgFe (NO)3)3) Mix in 8mL DMF to make a homogeneous precursor solution. 4mg DMAP was added and stirred at room temperature for 45min, then kept at 80 ℃ for 20 min. Centrifuging, washing the obtained product with DMF and methanol, drying in a drying oven at 60 ℃ for 24h, and calcining in a muffle furnace at 400 ℃ for 20min to obtain 31.7mg of an initial product;
the crude product obtained was trituratively mixed with 26mg of hepta (2,3, 6-tri-O-methyl) - β -cyclodextrin and 21mg of β -cyclodextrin, and then calcined at 400 ℃ for 20 minutes under a mixed gas atmosphere of hydrogen and argon.
Example 2
The embodiment provides a porous iron oxide negative electrode material, and the preparation method comprises the following steps:
the reactants 50mg of terephthalic acid and 50mg of fumaric acid were mixed with 200mg of anhydrous ferric nitrate in 10.5ml of DMMF, then 10mg of DMAP was added and stirred at room temperature for 30min, and placed in a 60 ℃ dry box for reaction for 30 min. Centrifuging, washing the obtained product with DMF and methanol, drying in a drying oven at 100 deg.C for 12h, and calcining in a muffle furnace at 500 deg.C for 10min to obtain 66.1mg of initial product;
the obtained crude product was mixed with 66mg of 2-hydroxypropyl- β -cyclodextrin, 33mg of (2-hydroxypropyl) - γ -cyclodextrin, and 33mg of 2, 6-di-O-methyl- β -cyclodextrin by grinding, and calcined at 500 ℃ for 30min under a mixed atmosphere of hydrogen and argon.
Example 3
The embodiment provides a porous iron oxide negative electrode material, and the preparation method comprises the following steps:
the reactant 20mg terephthalic acid and 200mg anhydrous ferric nitrate in 2.1mLDMF mixed, then add 0.2mg DMAP and stir at room temperature for 60min, placed in 120 ℃ dry box reaction for 10 minutes. Centrifuging, washing the obtained product with DMF and methanol, drying in a drying oven at 80 deg.C for 18h, and calcining in a muffle furnace at 300 deg.C for 20min to obtain 66.0mg of initial product;
and grinding and mixing the calcined product with 16.5mg of gamma-cyclodextrin and 16.5mg of methyl- β -cyclodextrin to obtain the initial product, and calcining the initial product at 300 ℃ for 10min in a nitrogen atmosphere.
The process flow diagrams of examples 1-3 are shown in FIG. 1.
Example 4
The embodiment provides application of a porous iron oxide negative electrode material in preparation of a lithium ion battery.
The porous iron oxide negative electrode material is assembled into a button cell in a glove box, and then the electrochemical performance is tested by using a blue test system and a Princeton electrochemical workstation, and the result shows that the button cell has 20% higher specific discharge capacity than a conventional iron oxide sample (the specific discharge capacity is 458mAh/g) under the high multiplying power of 10C, and the specific discharge capacity reaches 550 mAh/g. Under the high-temperature condition of 60 ℃, the capacity of a conventional iron oxide sample is sharply reduced after 100 cycles, and the porous iron oxide negative electrode material still has a cycle retention rate of 99.1% after 200 cycles. Due to the existence of the carbon coating layer, an alternating current impedance test (EIS) shows that the ion conductivity of the button cell is obviously improved and the performance of the button cell is obviously improved compared with that of a conventional iron oxide sample after 100 cycles.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a porous ferric oxide negative electrode material is characterized in that solid organic acid and ferric nitrate are dissolved in a solvent, a catalyst is added, the mixture is stirred for 30-60 min, the mixture is reacted for 10-30 min at the temperature of 60-120 ℃, and the obtained product is washed, dried and calcined at the temperature of 300-500 ℃ for 10-20 min to obtain a primary product;
grinding and mixing the obtained primary product and a carbon source, and calcining for 10-30 min at 300-500 ℃ in an inert atmosphere;
wherein the solid organic acid is at least one of terephthalic acid and fumaric acid.
2. The method for preparing the porous iron oxide anode material according to claim 1, wherein the catalyst is 4-dimethylaminopyridine.
3. The preparation method of the porous iron oxide negative electrode material as claimed in claim 2, wherein the mass of the catalyst is 1-10% of the mass of the organic acid.
4. The method for preparing the porous iron oxide anode material according to claim 2, wherein the solvent is N, N-dimethylformamide.
5. The method for preparing the porous iron oxide negative electrode material according to claim 4, wherein the mass of the solvent is 0.1 to 0.3 times of the mass of the organic acid.
6. The preparation method of the porous iron oxide negative electrode material as claimed in claim 1, wherein the mass ratio of the solid organic acid to the iron nitrate is 0.1-0.5: 1.
7. The method of preparing the porous iron oxide anode material of claim 1, wherein the carbon source is at least one of β -cyclodextrin, γ -cyclodextrin, methyl- β -cyclodextrin, 2-hydroxypropyl- β -cyclodextrin, (2-hydroxypropyl) - γ -cyclodextrin, 2, 6-di-O-methyl- β -cyclodextrin, and hepta (2,3, 6-tri-O-methyl) - β -cyclodextrin.
8. The preparation method of the porous iron oxide negative electrode material as claimed in claim 7, wherein the mass ratio of the carbon source to the primary product is 0.5-2: 1.
9. A porous iron oxide negative electrode material is characterized by being prepared by the preparation method of the porous iron oxide negative electrode material according to any one of claims 1 to 8.
10. Use of the porous iron oxide negative electrode material of claim 9 in the preparation of a lithium ion battery.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115745006A (en) * | 2022-10-19 | 2023-03-07 | 景德镇陶瓷大学 | Low-temperature carbon coating method for amorphous oxide and application |
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Application publication date: 20200403 |