CN112421025A - High-energy-density iron-based lithium ion battery cathode material and preparation method thereof - Google Patents
High-energy-density iron-based lithium ion battery cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion battery cathode materials and preparation thereof, and particularly provides a high-energy-density iron-based lithium ion battery cathode material and a preparation method thereof; the chemical expression of the lithium ion battery negative electrode material is as follows: alpha-LiFe5O8The crystal phase structure is spinel structure. The invention discovers that the iron-based composite oxide material alpha-LiFe for the first time5O8The lithium ion battery anode material can be applied to a lithium ion battery as an anode material, and has the characteristics of excellent electrochemical performance, high specific capacity and high energy density; when the charge-discharge rate is 0.1C, the first discharge specific capacity of the spinel type cathode material can reach 2918.25 mAh/g. Meanwhile, the single-phase sodium prepared by combining the normal-temperature liquid-phase reaction with the high-temperature sintering method has good crystal quality and uniform sizeMeter grade spinel type alpha-LiFe5O8(ii) a The preparation process is easy to control, no special equipment is required, the preparation flow is simple and easy to implement, and the used raw materials are low in price, non-toxic and pollution-free, so that the requirement of large-scale industrial production can be met.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials and preparation thereof, and particularly relates to a lithium ion battery cathode materialThe material and the preparation method thereof, the material has the following chemical formula: alpha-LiFe5O8。
Background
Traditional non-renewable fossil energy sources such as petroleum, coal, natural gas and the like are greatly consumed along with the continuous deepening of the modern industrial process, and due to the limited environment bearing capacity, the fossil energy sources can not meet the increasingly diversified demands of people on energy sources; CO produced by fossil energy simultaneously2、SO2、H2S and the like cause serious pollution to the environment, and the greenhouse effect caused by the S and the like becomes a great environmental problem for human beings. The lithium ion battery as a green and environment-friendly secondary battery with excellent performance has the advantages of flexibility, convenience, high storage capacity, repeated charge and discharge, safety, no pollution, high voltage, high energy density, no memory effect and the like, becomes the strongest competitor in a new generation battery system, is a hotspot of research in the world scientific research and industrial circles, is also the most widely applied power battery at present, and has infinite development prospect.
At present, the commercial lithium ion battery mainly adopts carbon-based negative electrode materials such as graphite, Li4Ti5O12Materials such as Si-based materials have only just started to be used as anode materials, and a large number of problems still remain to be solved. Wherein the theoretical specific capacity of the graphite type carbon is only 372mAh g-1The application requirement of high energy density of the lithium ion battery cannot be met; in addition, its lower working platform (-0.2V Vs Li)+/Li) can lead to the deposition of metallic lithium layers on the graphite surface during cycling, and lithium dendrites can cause potential safety problems. Spinel type Li4Ti5O12Is another important commercial anode material, is called as a 'zero strain' electrode material because the volume change is only 0.3 percent in the charge and discharge processes, and has good cycling stability, but the theoretical specific capacity is only 172mAh g-1And a higher voltage operating platform (1.5vs. Li/Li)+) Is not beneficial to improving the energy density. The silicon-based negative electrode material has the advantages of low cost and high specific capacity, and the theoretical capacity of the silicon-based negative electrode material reaches 4200mAh g-1The voltage platform is only about 0.37V, the generation of lithium dendrite can be reduced by the higher voltage platform, and the safety performance is better than that of a graphite type negative electrode; however, when the amount of lithium is too much, the volume expansion rate reaches 320%, and the stress effect caused by the volume change leads to pulverization of the particles, which causes rapid capacity decline. The applications and developments of several of the above currently major commercial negative electrode materials are limited by their performance; therefore, the development of a novel negative electrode material with high specific capacity, high safety and low price becomes the key for developing a high-performance power lithium ion battery.
Iron-based composite oxide materials, e.g. Fe2O3、Fe3O4And LiFeO2All have low cost, no toxicity and high specific capacity (1000 mAh g)-1) Safe working voltage (0.8V), abundant raw material sources and the like, thereby being widely researched as a potential next-generation lithium ion electrode material. Based on the above, the invention provides a novel high-energy-density iron-based lithium ion battery cathode material and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a novel high-energy-density iron-based lithium ion battery cathode material and a preparation method thereof aiming at various problems of the existing lithium ion battery cathode material; the invention discovers that the iron-based composite oxide material alpha-LiFe for the first time5O8The lithium ion battery can be applied to a lithium ion battery as a cathode material, and has the advantages of high initial discharge specific capacity, good cycle performance, long cycle life and the like; meanwhile, the lithium ion battery cathode material is prepared by combining a normal-temperature liquid-phase reaction and a high-temperature sintering method, has a spinel structure, is uniform in particle size, and is high in crystallinity and purity.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high energy density iron-based lithium ion battery cathode material is characterized in that the chemical expression of the lithium ion battery cathode material is as follows: alpha-LiFe5O8The crystal phase structure is spinel structure.
The preparation method of the high-energy-density iron-based lithium ion battery cathode material comprises the following steps:
step 3, drying the sample washed cleanly in the step 2 at 80-120 ℃ for 12-24 hours to obtain a dried sample;
step 4, grinding the dried sample obtained in the step 3 into powder at room temperature, and sintering at 650-950 ℃ for 6-12 h to obtain the spinel-type alpha-LiFe5O8A lithium ion battery negative electrode material;
further, in the step 1, the lithium source raw material is at least one of lithium hydroxide, lithium nitrate, lithium carbonate, lithium acetate, and lithium chloride.
Further, in the step 1, the iron source raw material is at least one of ferric nitrate nonahydrate, ferric trichloride hexahydrate, ferric sulfate, ferrous sulfate, ferric ammonium sulfate, ferric acetate and ferric oxide.
Further, in the step 1, the solvent medium is absolute ethyl alcohol or other non-aqueous solvents.
Further, in the step 4, the sintering atmosphere for sintering is an air atmosphere, a nitrogen atmosphere, or an argon atmosphere.
Further, in the step 4, the temperature rise rate of the sintering is 1-10 ℃/min.
The invention has the beneficial effects that:
1. the invention discovers that the iron-based composite oxide material alpha-LiFe for the first time5O8The lithium ion battery anode material can be applied to a lithium ion battery as an anode material, and has the characteristics of excellent electrochemical performance, high specific capacity and high energy density. Spinel type alpha-LiFe5O8As one of iron-based materials, Fe3+In the reduction process are involvedTransfer of one electron, thus alpha-LiFe5O8The theoretical specific capacity can reach 969mAh g-1More than 2 times of the graphite carbon cathode; at the same time, alpha-LiFe5O8Belonging to P4332 space group, structure with partial Fe3+Occupying 8c position of tetrahedron, and remaining Fe3+And Li+The stable structure of the cation order is suitable for being used as a lithium ion battery cathode material. The invention adopts spinel type alpha-LiFe5O8As the lithium ion battery cathode material, the lithium ion battery cathode material has higher charge-discharge specific capacity, stable cycle performance and a charge-discharge voltage platform which can be well matched with the anode material without any modification, and is suitable for the requirement of making a high-energy-density charge-discharge lithium ion battery; when the charge-discharge rate is 0.1C, the first discharge specific capacity of the spinel type cathode material can reach 2918.25 mAh/g.
2. The invention also provides the high-energy density iron-based lithium ion battery cathode material alpha-LiFe5O8The preparation method of (1); adopting a method combining normal temperature liquid phase reaction with high temperature sintering, directly reacting an iron source and a lithium source in an absolute ethyl alcohol solvent medium to form reddish brown alpha-LiFe under the normal temperature liquid phase condition5O8A precursor, which forms single-phase nano spinel type alpha-LiFe with good crystallization quality and uniform size in the high-temperature sintering process5O8(ii) a Raw materials used in the preparation process are common chemical raw materials, the raw material sources are rich, particularly, the iron source raw material is low in price, non-toxic and pollution-free, the green environmental protection concept is met, and the production cost can be reduced for enterprises in the commercial production process; and the equipment used in the preparation process is simple, the preparation process is easy to control, no special equipment is required, the preparation process is simple and easy to implement, and the requirement of large-scale industrial production can be met.
Drawings
FIG. 1 shows the high energy density iron-based lithium ion battery cathode material alpha-LiFe of the present invention5O8The preparation flow chart of (1);
FIG. 2 shows a tip prepared in an example of the present inventionalpha-LiFe as negative electrode material of lithium ion battery5O8Characteristic charge-discharge curve at 0.1C;
FIG. 3 shows α -LiFe, which is a spinel-type lithium ion battery cathode material prepared in the embodiment of the present invention5O8A charge-discharge cycle curve chart under different multiplying powers;
FIG. 4 shows α -LiFe, which is a spinel-type lithium ion battery cathode material prepared in the embodiment of the present invention5O8X-ray diffraction (XRD) profile of (a);
FIG. 5 shows α -LiFe, which is a spinel-type lithium ion battery cathode material prepared in the embodiment of the present invention5O8Scanning Electron Microscope (SEM) and High Resolution Transmission Electron Microscope (HRTEM) photographs;
FIG. 6 shows α -LiFe, which is a spinel type lithium ion battery cathode material prepared in the embodiment of the present invention5O8Nyquist plot of electrodes in open circuit state (OCV) and after 50 cycles (the built-in plot is the equivalent circuit plot);
FIG. 7 shows α -LiFe, which is a spinel-type lithium ion battery cathode material prepared in the embodiment of the present invention5O8Schematic diagram of button half cell with electrode assembly.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a high energy density iron-based lithium ion battery cathode material: spinel type alpha-LiFe5O8The process is shown in FIG. 1; ferric nitrate nonahydrate and lithium hydroxide are respectively used as an iron source and a lithium source, and absolute ethyl alcohol is used as a solvent medium; the method specifically comprises the following steps:
firstly, 0.10mol of ferric nitrate nonahydrate and 1.50mol of lithium hydroxide are dissolved in 600ml of absolute ethyl alcohol, and are continuously stirred for 2 hours at normal temperature to obtain a reddish brown suspension solution;
then, carrying out centrifugal separation on the suspension solution to obtain a solid, repeatedly and alternately washing the solid with deionized water and absolute ethyl alcohol to obtain a reddish brown solid, and drying the solid in a blast drying oven at 100 ℃ for 12 hours;
and finally, fully grinding the dried reddish brown solid into powder by using an agate mortar, then transferring the powder into a ceramic boat, placing the ceramic boat into a muffle furnace, sintering the ceramic boat at the temperature rise rate of 3 ℃/min for 6 hours at the temperature of 800 ℃ in an oxygen atmosphere, and cooling the sintered ceramic boat to room temperature along with the furnace to obtain the lithium ion battery cathode material: spinel type alpha-LiFe5O8。
XRD test is carried out on the obtained target material, and the result is shown in figure 4, and the material is typical of spinel type alpha-LiFe5O8A crystalline phase. The obtained target material is subjected to SEM and HRTEM tests, and the result is shown in FIG. 5, and the material is spherical-like nano-scale to submicron-scale particles. The obtained spinel-type alpha-LiFe5O8The composite material is used as a lithium ion battery cathode material, and is mixed with an acetylene black conductive agent and a Polyvinylidene Fluoride (PVDF) binder to prepare an electrode according to a mass ratio of 85:10: 5; the specific process is as follows: firstly, mixing an electrode material and a conductive agent, namely mixing the electrode material and the conductive agent in a ratio of 85:10, then grinding in an agate mortar until the mixture is fully and uniformly mixed, wherein the grinding time is more than or equal to 30 min; then weighing 0.425g of the mixture, adding 1ml of 2.5 wt% PVDF solution prepared in advance, and grinding for 20min again to obtain slurry in which the three are uniformly mixed; uniformly coating the obtained slurry on the surfaces of a cleaned and dried aluminum foil (positive electrode) and a cleaned and dried copper foil (negative electrode) by using a scraper, and placing the coated aluminum foil pole piece and the coated copper foil pole piece in a forced air drying oven to be dried for 1h at the temperature of 80 ℃; finally, cutting the metal foil pole piece dried in the blast drying oven, wherein the diameter of the pole piece is 9.5mm, placing the cut pole piece at 100 ℃ for vacuum drying for 20h, and transferring the dried pole piece into a drying dish for standing for later use to prevent moisture absorption; the active material loading of each pole piece is 1.5-2.5mg/cm2(ii) a Finally, the obtained electrode pole piece is assembled into a button type half cell to carry out performance test, and the half cell is assembled in a stainless steel glove box filled with Ar to finish the performance test. In this embodiment, a CR2025 button cell is selected, a lithium plate is used as a counter electrode, a diaphragm is Celgard 2320, and an electrolyte is LiPF with 1mol/L6Dissolving into a mixed solution of EC and DEC with a volume ratio of 1: 1; structure of CR2025 button cell as shown in fig. 7As shown. The button cell made of the obtained target material is subjected to constant current charge and discharge test, and the result is shown in figure 2, and the material obtains the first ultrahigh specific discharge capacity of 2918mAh/g at the rate of 0.1C. The button cell made of the obtained target material is subjected to constant-current charge-discharge rate cycle performance test, and the result is shown in fig. 3, and it can be seen from the figure that although the discharge specific capacities of the materials under different rates are different, the cycle performance under different rates is still good. The ac impedance change test was performed on the button cell made of the target material, and the result is shown in fig. 6, which shows that although the impedance of the material after the cycle slightly changes, the change is not obvious, and the ac impedance only slightly increases after 50 cycles.
Example 2
The embodiment provides a high energy density iron-based lithium ion battery cathode material: spinel type alpha-LiFe5O8The preparation method comprises the steps of taking ferric nitrate nonahydrate and lithium nitrate as an iron source and a lithium source respectively, and taking absolute ethyl alcohol as a solvent medium; the method specifically comprises the following steps:
firstly, 0.10mol of ferric nitrate nonahydrate and 2.00mol of lithium nitrate are dissolved in 600ml of absolute ethyl alcohol, and the mixture is continuously stirred for 3 hours at normal temperature to obtain a reddish brown suspension solution;
then, carrying out centrifugal separation on the suspension solution to obtain a solid, repeatedly and alternately washing the solid with deionized water and absolute ethyl alcohol to obtain a reddish brown solid, and then drying the solid in a blast drying oven at 120 ℃ for 24 hours;
and finally, fully grinding the dried reddish brown solid into powder by using an agate mortar, then transferring the powder into a ceramic boat, placing the ceramic boat into a tubular furnace, sintering the ceramic boat at the temperature rise rate of 3 ℃/min for 10 hours at the temperature of 750 ℃ in an argon atmosphere, and cooling the sintered solid to room temperature along with the furnace to obtain the lithium ion battery cathode material: spinel type alpha-LiFe5O8。
The test was carried out by the same test method as in example 1, and the effects and properties were substantially the same as in example 1.
Example 3
The embodiment provides a high-energy-density iron-based lithium ion battery cathode material: spinel type alpha-LiFe5O8The preparation method comprises the steps of respectively taking ferric trichloride hexahydrate and lithium hydroxide as an iron source and a lithium source, and taking absolute ethyl alcohol as a solvent medium; the method specifically comprises the following steps:
firstly, 0.10mol of ferric trichloride hexahydrate and 2.00mol of lithium hydroxide are dissolved in 600ml of absolute ethyl alcohol, and the mixture is continuously stirred for 3 hours at normal temperature to obtain a reddish brown suspension solution;
then, carrying out centrifugal separation on the suspension solution to obtain a solid, repeatedly and alternately washing the solid with deionized water and absolute ethyl alcohol to obtain a reddish brown solid, and drying the solid for 20 hours in a blast drying oven at 120 ℃;
and finally, fully grinding the dried reddish brown solid into powder by using an agate mortar, then transferring the powder into a ceramic boat, placing the ceramic boat into a tubular furnace, sintering the ceramic boat at the temperature rise rate of 3 ℃/min for 12 hours at the temperature of 850 ℃ in a nitrogen atmosphere, and cooling the sintered solid to room temperature along with the furnace to obtain the lithium ion battery cathode material: spinel type alpha-LiFe5O8。
The test was carried out by the same test method as in example 1, and the effects and properties were substantially the same as in example 1.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (7)
1. A high energy density iron-based lithium ion battery cathode material is characterized in that the chemical expression of the lithium ion battery cathode material is as follows: alpha-LiFe5O8The crystal phase structure is spinel structure.
2. The preparation method of the high energy density iron-based lithium ion battery cathode material according to claim 1, comprising the following steps:
step 1, dissolving a lithium source raw material and an iron source raw material in a solvent medium according to a molar ratio of Li to Fe (10-20): 1, and stirring at room temperature for 2-5 hours to obtain a suspension solution;
step 2, performing centrifugal separation on the suspension solution to obtain a solid, and repeatedly and alternately washing the solid with absolute ethyl alcohol and deionized water to obtain a solid sample;
step 3, drying the washed solid sample at 80-120 ℃ for 12-24 h to obtain a dried sample;
and 4, grinding the dried sample into powder at room temperature, and sintering at 650-950 ℃ for 6-12 h to prepare the high-energy-density iron-based lithium ion battery cathode material.
3. The method for preparing a high energy density iron-based lithium ion battery negative electrode material according to claim 2, wherein in the step 1, the lithium source material is at least one of lithium hydroxide, lithium nitrate, lithium carbonate, lithium acetate and lithium chloride.
4. The method for preparing the high energy density iron-based lithium ion battery cathode material according to claim 2, wherein in the step 1, the iron source material is at least one of ferric nitrate nonahydrate, ferric trichloride hexahydrate, ferrous sulfate, ferric ammonium sulfate, ferric acetate and ferric oxide.
5. The method for preparing the high energy density iron-based lithium ion battery negative electrode material according to claim 2, wherein in the step 1, the solvent medium is absolute ethyl alcohol or other non-aqueous solvents.
6. The method for preparing the high energy density iron-based lithium ion battery cathode material according to claim 2, wherein in the step 4, the sintering atmosphere for sintering is air atmosphere, nitrogen atmosphere or argon atmosphere.
7. The preparation method of the high energy density iron-based lithium ion battery cathode material according to claim 2, wherein in the step 4, the temperature rise rate of the sintering is 1-10 ℃/min.
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| CN114804211A (en) * | 2022-05-20 | 2022-07-29 | 洛阳师范学院 | High-first-efficiency lithium ferrate negative electrode material for lithium ion battery and preparation method thereof |
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Application publication date: 20210226 |