CN111689524A - Lithium ion battery material FeVO4Process for producing microparticles - Google Patents
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- CN111689524A CN111689524A CN202010351570.0A CN202010351570A CN111689524A CN 111689524 A CN111689524 A CN 111689524A CN 202010351570 A CN202010351570 A CN 202010351570A CN 111689524 A CN111689524 A CN 111689524A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a lithium ion battery material FeVO4A preparation method of microparticles belongs to the technical field of lithium ion battery materials. The device comprises the following steps: weighing ammonium metavanadate and ferric nitrate nonahydrate according to the molar ratio of V to Fe being 1 to 1, and respectively dissolving the ammonium metavanadate and the ferric nitrate nonahydrate in deionized water; adding glucose into a ferric nitrate nonahydrate solution, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is (1:1) - (1.1: 1); adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W to 1 (0.01-0.05); slowly adding the mixture into ferric nitrate nonahydrate solution dropwise to obtainObtaining a precursor solution; stirring the precursor solution in a water bath at 50-60 ℃ until the solution is evaporated to dryness; calcining for 1-2 hours at the temperature of 450-550 ℃. The method provided by the invention has simple process and is easy to control. The negative electrode material (1) prepared by the method has small particle size, and most of the particle size is distributed in the range of about 60 nm; (2) the conductivity is good; (3) the charge-discharge specific capacity is large, and the cycling stability is good.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a lithium ion battery material FeVO4The modification method and the material thereof.
Background
The lithium ion battery has the advantages of high charge-discharge specific capacity, long cycle life, good safety performance and the like, and has wide application. However, with the development of science and technology, such as the development of large power equipment and energy storage power stations, higher requirements are put forward on lithium ion batteries. Lithium ion batteries are expected to have higher energy densities, longer cycle lives, and more excellent rate performance.
The negative electrode material is an important component of the lithium ion battery, and the excellent performance of the negative electrode material is indispensable for obtaining the lithium ion battery with excellent performance. FeVO4Has larger theoretical specific capacity, and the discharge specific capacity can reach 1253 mAh/g. The theoretical capacity of the carbon negative electrode which is widely used commercially at present is only 372 mAh/g. However, FeVO4Poor conductivity and poor cycling stability due to material pulverization caused by volume change during charge and discharge.
Disclosure of Invention
The invention provides a lithium ion battery cathode material FeVO4The modification method and the material can solve the problem of FeVO which is a cathode material of the lithium ion battery in the prior art4Poor cycle stability.
Lithium ion battery cathode material FeVO4The modification method comprises the following steps:
s1, weighing ammonium metavanadate and ferric nitrate nonahydrate according to a molar ratio of V: Fe-1: 1, and respectively dissolving the ammonium metavanadate and ferric nitrate nonahydrate solutions in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the concentrations of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution are both 0.05mol/L-0.2 mol/L;
s2, adding glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose is dissolved to obtain a solution A, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is (1:1) - (1.1: 1); adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W to 1 (0.01-0.05), and obtaining a solution B after the ammonium metatungstate and the ammonium metavanadate are completely dissolved;
s3, slowly dripping the solution B into the solution A to obtain a precursor solution;
s4, stirring the precursor solution in a water bath at 50-60 ℃ until the solution is evaporated to dryness to obtain tungsten-doped FeVO4A precursor;
s5, mixing FeVO4Grinding the precursor, calcining for 1-2 hours at the temperature of 450-550 ℃, and naturally cooling to obtain the tungsten-doped FeVO4And (3) a negative electrode material.
More preferably, in S1, the concentrations of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution are both 0.1 mol/L.
Preferably, in S4, the precursor solution is stirred in a water bath condition at 55 ℃ until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor.
More preferably, in S5, FeVO is introduced4After grinding, the precursor was calcined at 500 ℃ for 1.5 hours.
More preferably, in S2, ammonium metatungstate is added to the ammonium metavanadate solution at a molar ratio of V: W of 1: 0.03.
A lithium ion battery negative electrode material is prepared by any one of the methods.
The invention provides a lithium ion battery cathode material FeVO4The method has simple process and is easy to control.
The anode material prepared by the method has the following advantages: (1) the particle size is small, and most of the particle size ranges are about 60 nm; (2) the conductivity is good; (3) the charge-discharge specific capacity is large, and the cycling stability is good.
Drawings
FIG. 1 is an XRD pattern of a sample prepared according to each example;
FIG. 2 is a scanning electron micrograph of a sample prepared according to each example;
FIG. 3 is a graph of the charge and discharge cycle performance of samples prepared in each example;
FIG. 4 is a graph of the AC impedance of the samples prepared in each example.
Detailed Description
An embodiment of the present invention will be described in detail below with reference to the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the embodiment.
The invention provides a lithium ion battery cathode material FeVO4And the negative electrode prepared by the methodA pole material. Adding ammonium metatungstate in the preparation process to obtain tungsten-doped FeVO4Thereby improving the charge-discharge specific capacity, the cycling stability and the like of the cathode material.
Example 1 (control group)
After ammonium metavanadate and ferric nitrate nonahydrate are weighed according to the molar ratio of V: Fe being 1:1, respectively dissolved in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the solution concentration of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution is 0.1 mol/L. Adding a certain amount of glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose is dissolved to obtain a solution A, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is 1.1: 1. And after the ammonium metavanadate is completely dissolved, obtaining a solution B, slowly dripping the solution B into the ferric nitrate nonahydrate solution, and continuously stirring to obtain a precursor solution. Stirring the precursor solution under the condition of 60 ℃ water bath until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor. The obtained FeVO4Grinding the precursor, putting the ground precursor into a crucible, calcining the precursor for 1 hour in a muffle furnace at 500 ℃, and naturally cooling to obtain pure FeVO4And (3) a negative electrode material.
Example 2.
After ammonium metavanadate and ferric nitrate nonahydrate are weighed according to the molar ratio of V: Fe being 1:1, respectively dissolved in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the solution concentration of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution is 0.1 mol/L. Adding a certain amount of glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose and the ferric nitrate nonahydrate are dissolved, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is 1.1: 1. Adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W of 1 to 0.01, and obtaining an intermediate mixed solution after the ammonium metatungstate and the ammonium metavanadate are completely dissolved. And slowly dripping the intermediate mixed solution into the ferric nitrate nonahydrate solution, and continuously stirring to obtain an extracting solution. Stirring the extracting solution under the condition of 50 ℃ water bath until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor. The obtained FeVO4Grinding the precursor, putting the ground precursor into a crucible, calcining the precursor for 1 hour in a muffle furnace at 500 ℃, and naturally cooling to obtain pure FeVO4And (3) a negative electrode material.
Example 3.
After ammonium metavanadate and ferric nitrate nonahydrate are weighed according to the molar ratio of V: Fe being 1:1, respectively dissolved in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the solution concentration of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution is 0.1 mol/L. Adding a certain amount of glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose and the ferric nitrate nonahydrate are dissolved, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is 1.1: 1. Adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W of 1 to 0.03, and obtaining an intermediate mixed solution after the ammonium metatungstate and the ammonium metavanadate are completely dissolved. And slowly dripping the intermediate mixed solution into the ferric nitrate nonahydrate solution, and continuously stirring to obtain an extracting solution. Stirring the extracting solution under the condition of water bath at 55 ℃ until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor. The obtained FeVO4Grinding the precursor, putting the ground precursor into a crucible, calcining the precursor for 1.5 hours in a muffle furnace at 500 ℃, and naturally cooling the calcined precursor to obtain pure FeVO4And (3) a negative electrode material.
Example 4.
After ammonium metavanadate and ferric nitrate nonahydrate are weighed according to the molar ratio of V: Fe being 1:1, respectively dissolved in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the solution concentration of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution is 0.1 mol/L. Adding a certain amount of glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose and the ferric nitrate nonahydrate are dissolved, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is 1.1: 1. Adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W of 1 to 0.05, and obtaining an intermediate mixed solution after the ammonium metatungstate and the ammonium metavanadate are completely dissolved. And slowly dripping the intermediate mixed solution into the ferric nitrate nonahydrate solution, and continuously stirring to obtain an extracting solution. Stirring the extracting solution under the condition of 60 ℃ water bath until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor. The obtained FeVO4Grinding the precursor, putting the ground precursor into a crucible, calcining the precursor for 2 hours in a muffle furnace at 500 ℃, and naturally cooling to obtain pure FeVO4And (3) a negative electrode material.
Fig. 1 shows XRD patterns of samples prepared in the respective examples. Fig. 2 shows a scanning electron microscope image of the samples prepared in each example, and it can be seen from the image that the particle size of the samples prepared in examples 1 to 4 gradually decreases, and the addition of ammonium metatungstate effectively improves the particle size, so that the particle size of the prepared anode material is smaller. However, in example 4, since the particle size is too small, the particles are agglomerated, which affects the electrochemical performance, and thus the discharge performance is inferior to that of example 3. Fig. 3 shows a graph of the charge-discharge cycle performance of the samples prepared in the examples, and it can be seen from the graph that the decay tendency of each example is similar, but the charge-discharge cycle stability and the specific discharge capacity of example 3 are much better than those of the other examples, and example 1 without adding ammonium metatungstate has the worst performance. Fig. 4 shows an ac impedance plot of the samples prepared in the examples. It can be seen that the conductivity of the material is significantly improved after the ammonium metatungstate is added, and the internal resistance of example 3 is the minimum.
The above disclosure is only for a few specific embodiments of the present invention, however, the present invention is not limited to the above embodiments, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (6)
1. Lithium ion battery cathode material FeVO4The method for modifying (c) is characterized by comprising the following steps:
s1, weighing ammonium metavanadate and ferric nitrate nonahydrate according to a molar ratio of V: Fe-1: 1, and respectively dissolving the ammonium metavanadate and ferric nitrate nonahydrate solutions in deionized water to obtain an ammonium metavanadate solution and a ferric nitrate nonahydrate solution, wherein the concentrations of the ammonium metavanadate solution and the ferric nitrate nonahydrate solution are both 0.05mol/L-0.2 mol/L;
s2, adding glucose into the ferric nitrate nonahydrate solution, and stirring until the glucose is dissolved to obtain a solution A, wherein the molar ratio of the glucose to the ferric nitrate nonahydrate is (1:1) - (1.1: 1); adding ammonium metatungstate into an ammonium metavanadate solution according to a molar ratio of V to W to 1 (0.01-0.05), and obtaining a solution B after the ammonium metatungstate and the ammonium metavanadate are completely dissolved;
s3, slowly dripping the solution B into the solution A to obtain a precursor solution;
s4, stirring the precursor solution in a water bath at 50-60 ℃ until the solution is evaporated to dryness to obtain tungsten-doped FeVO4A precursor;
s5, mixing FeVO4Grinding the precursor, calcining for 1-2 hours at the temperature of 450-550 ℃, and naturally cooling to obtain the tungsten-doped FeVO4And (3) a negative electrode material.
2. The lithium ion battery cathode material FeVO of claim 14The modification method of (3), wherein in S1, the concentrations of the ammonium metavanadate solution and the iron nitrate nonahydrate solution are both 0.1 mol/L.
3. The lithium ion battery cathode material FeVO of claim 14The modification method is characterized in that in S4, the precursor solution is stirred under the condition of water bath at 55 ℃ until the solution is evaporated to dryness to obtain tungsten-doped FeVO4And (3) precursor.
4. The lithium ion battery cathode material FeVO of claim 14The modification method of (3), wherein in S5, FeVO is added4After grinding, the precursor was calcined at 500 ℃ for 1.5 hours.
5. The negative electrode material FeVO of the lithium ion battery of any one of claims 1 to 44The modification method of (3), wherein in S2, ammonium metatungstate is added to an ammonium metavanadate solution at a molar ratio of V: W of 1: 0.03.
6. A lithium ion battery negative electrode material, characterized by being produced by the method of any one of claims 1 to 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259718A (en) * | 2020-10-22 | 2021-01-22 | 中国人民武装警察部队后勤学院 | FeVO applied to lithium secondary battery4Preparation method of/C composite material |
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| CN102942221A (en) * | 2012-11-14 | 2013-02-27 | 陕西科技大学 | Method for preparing rodlike Fe4(VO4)4.5H2O microcrystal through hydrothermal synthesis |
| CN103825025A (en) * | 2014-02-27 | 2014-05-28 | 三峡大学 | Negative electrode material FeVO4 of lithium ion battery and preparation method thereof |
| CN104971751A (en) * | 2015-06-29 | 2015-10-14 | 陕西科技大学 | Magnetic alpha-Fe2O<3-[delta]>C<[delta]>/FeVO<4-x+[delta]>C<x-[delta]> heterojunction photocatalyst, preparation method and applications thereof |
| CN106356510A (en) * | 2016-10-13 | 2017-01-25 | 中南大学 | Preparation method for Li-ion anode material FeVO4/C |
| CN107512740A (en) * | 2017-08-29 | 2017-12-26 | 合肥国轩电池材料有限公司 | A kind of lithium ion battery negative material FeVO4The preparation method of nano wire |
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2020
- 2020-04-28 CN CN202010351570.0A patent/CN111689524A/en active Pending
Patent Citations (6)
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| JPS58201255A (en) * | 1982-05-18 | 1983-11-24 | Nippon Telegr & Teleph Corp <Ntt> | Lithium battery |
| CN102942221A (en) * | 2012-11-14 | 2013-02-27 | 陕西科技大学 | Method for preparing rodlike Fe4(VO4)4.5H2O microcrystal through hydrothermal synthesis |
| CN103825025A (en) * | 2014-02-27 | 2014-05-28 | 三峡大学 | Negative electrode material FeVO4 of lithium ion battery and preparation method thereof |
| CN104971751A (en) * | 2015-06-29 | 2015-10-14 | 陕西科技大学 | Magnetic alpha-Fe2O<3-[delta]>C<[delta]>/FeVO<4-x+[delta]>C<x-[delta]> heterojunction photocatalyst, preparation method and applications thereof |
| CN106356510A (en) * | 2016-10-13 | 2017-01-25 | 中南大学 | Preparation method for Li-ion anode material FeVO4/C |
| CN107512740A (en) * | 2017-08-29 | 2017-12-26 | 合肥国轩电池材料有限公司 | A kind of lithium ion battery negative material FeVO4The preparation method of nano wire |
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| Title |
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| MEHDI GHOLAMZADEH BAEIS ET AL.: ""Controlled synthesis and characterization of iron vanadate magnetic nanoparticles: investigation it’s photodegradation of Rhodamine B"", 《J MATER SCI: MATER ELECTRON》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259718A (en) * | 2020-10-22 | 2021-01-22 | 中国人民武装警察部队后勤学院 | FeVO applied to lithium secondary battery4Preparation method of/C composite material |
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