CN107978754B - Ferrite-lithium titanate composite negative electrode material for lithium ion battery and preparation method thereof - Google Patents
Ferrite-lithium titanate composite negative electrode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN107978754B CN107978754B CN201711413501.2A CN201711413501A CN107978754B CN 107978754 B CN107978754 B CN 107978754B CN 201711413501 A CN201711413501 A CN 201711413501A CN 107978754 B CN107978754 B CN 107978754B
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Abstract
The invention discloses a ferrite-lithium titanate composite negative electrode material for a lithium ion battery and a preparation method thereof, wherein the negative electrode material contains lithium titanate Li4Ti5O12And coating Li4Ti5O12A coating layer on the surface. The coating layer is made of ferrite material and comprises CoFe2O4、ZnFe2O4、CuFe2O4And MgFe2O4One or more of (a). The invention firstly mixes and dissolves the metal nitrate and the combustion improver in the deionized water, and then Li is added4Ti5O12And performing strong ultrasonic dispersion for 2 hours, adjusting the pH value to be neutral by using ammonia water, evaporating the solution to dryness at the temperature of 80-130 ℃ to obtain gel, heating the gel to 200-300 ℃, keeping the temperature for 5-15 min, and then performing an air atmosphere calcination process to obtain the composite material. The lithium ion battery composite negative electrode material has high capacity and excellent cycle stability and durability.
Description
Technical Field
The invention belongs to the technical field of material synthesis and energy, and particularly relates to a ferrite-lithium titanate material for a lithium ion battery and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, high working voltage, long cycle life, no memory and the like, is widely applied to the fields of digital codes, energy storage, electric automobiles and the like, and becomes a high-energy battery system with the most bright application prospect.
At present, the commercial lithium ion battery is mainly made of graphite cathode materials, but the graphite materials have many defects, such as insufficient cycle performance, easy failure under high temperature conditions, easy generation of lithium crystal branches and potential safety hazards. The lithium titanate material has the advantages of small volume change, high stability, strong cycle performance, difficult generation of lithium crystal branches, high safety and the like in the lithium ion de-intercalation/intercalation process, and is an electrode material with great prospect. However, the lithium titanate has a low theoretical capacity (175 mAh/g), and is difficult to satisfy the demand of people for high energy density lithium ion batteries.
Disclosure of Invention
Aiming at the defects of lithium titanate, the invention provides a ferrite-lithium titanate composite negative electrode material for a lithium ion battery and a preparation method thereof, wherein a high-capacity ferrite material (the theoretical capacity is more than 880 mAh/g) is coated on the surface of lithium titanate so as to solve the defect of low capacity of the lithium titanate. In addition, by virtue of the advantage of high cycle stability of lithium titanate, the pseudocapacitance effect of the ferrite coating layer can increase the reversible capacity of the composite electrode material after being cycled for dozens of times. The preparation method has the advantages of simple process and low cost. The obtained material contains a certain hole structure, so that the transmission of lithium ions can be accelerated, and the electrochemical activity is improved; but also can increase the stability of the material and improve the processability and the storage stability of the material.
In order to achieve the above object, the present invention provides a ferrite-lithium titanate composite negative electrode material for a lithium ion battery, wherein the composite negative electrode material comprises lithium titanate Li4Ti5O12And coating the Li4Ti5O12A ferrite coating layer on the surface, wherein the ferrite is CoFe2O4、ZnFe2O4、CuFe2O4And MgFe2O4At least one of (1).
Further, the Li4Ti5O12Accounting for 50-90% of the total mass of the composite negative electrode material.
Further, the thickness of the ferrite coating layer is 20-2000 nm.
The invention also provides a preparation method of the ferrite-lithium titanate composite negative electrode material for the lithium ion battery, which comprises the following steps.
(1) Weighing M (NO)3)2、Fe(NO3)3And a combustion improver are mixed and dissolved in deionized water, and the M element is at least one of Co, Zn, Cu and Mg.
(2) Adding Li to the solution4Ti5O12And carrying out strong ultrasonic dispersion for 2 hours, and adjusting the pH value of the solution to 6.5-7.0 by using ammonia water.
(3) Evaporating the solution to dryness at the temperature of 80-130 ℃ to obtain gel, heating the gel to 200-300 ℃, keeping the temperature for 5-15 min, and then performing an air atmosphere calcination process to obtain the composite negative electrode material.
Further, the combustion aid is one or a mixture of glycine, citric acid and urea in any ratio.
Further, said M (NO)3)2With Fe (NO)3)3In a molar ratio of 1: 2, the molar ratio of the nitrate to the combustion improver is 1: (0.5 to 6).
Further, the calcination conditions were: the calcining temperature is 600-900 ℃, and the calcining time is 0.5-5 h.
The beneficial effects of the invention are as follows.
1. The method for preparing the ferrite-lithium titanate material by using the gel-combustion method is quick and simple to operate, and avoids complex operation steps in the traditional method.
2. The lithium titanate material is coated in the ferrite, so that the lithium titanate is protected from being corroded and decomposed by electrolyte, and the circulation capacity of the material is improved.
3. The electrode material prepared by the method has a porous micro-nano structure. The porous structure can relieve the volume change in the circulation process, and is beneficial to the transmission of electrons and lithium ions of the electrolytic material, thereby improving the electrochemical performance of the material; the micro-nano structure increases the stability of material preparation and storage, and reduces the production and storage cost to a certain extent.
4. The composite electrode material prepared by the invention has stronger cycle performance, and the reversible capacity is greatly improved compared with that of a single lithium titanate electrode.
Drawings
Fig. 1 is a TEM image of a composite anode material in example 1.
FIG. 2 is a graph of the cycling performance of the composite anode material in example 1 at a current density of 200 mA/g.
FIG. 3 is a graph of the cycling performance of the composite anode material in example 2 at a current density of 200 mA/g.
FIG. 4 is a graph of the cycling performance of the composite anode material in example 3 at a current density of 200 mA/g.
FIG. 5 is a graph of the cycling performance of the composite anode material at a current density of 200mA/g in example 4.
FIG. 6 is a graph showing the cycle characteristics of the negative electrode material in comparative example 1 at a current density of 200 mA/g.
Detailed Description
The present invention will be described in detail with reference to the following examples, but the scope of the present invention is not limited to the examples.
Example 1
(1) 2.91g of cobalt nitrate, 8.08g of iron nitrate and 0.9g of urea were weighed out and dissolved in deionized water.
(2) Weighing 2.35g of lithium titanate, adding the lithium titanate into the mixed solution, performing strong ultrasonic dispersion for 2 hours, and adjusting the pH value of the solution to 6.8 by using ammonia water.
(3) Evaporating the solution to dryness at the temperature of 80 ℃ to obtain gel, heating the gel to 300 ℃ and keeping the temperature constant for 5min, and calcining the obtained product at the temperature of 800 ℃ for 2h in air atmosphere to obtain the ferrite-lithium titanate composite negative electrode material. Li in composite negative electrode material4Ti5O12The content was 50 wt%.
FIG. 1 is a TEM image of the ferrite-lithium titanate composite negative electrode material of the embodiment, wherein 1 is Li4Ti5O12Particles, 2 being CoFe2O4And (4) coating. FIG. 1 shows Li4Ti5O12Particle coating CoFe2O4And (3) completely coating, wherein the thickness of the coating layer is 20-200 nm.
And (3) electrochemical performance testing: the prepared electrode material ferrite-lithium titanate, acetylene black and polyvinylidene fluoride (PVDF) are uniformly mixed in N-2-methyl pyrrolidone (NMP) according to the mass ratio of 8: 1, and the slurry is coated on a copper foil to prepare the electrode. Drying the test electrode in a vacuum oven at 110 ℃ for 24h, assembling the test electrode into a CR2016 button cell in a glove box in a high-purity argon atmosphere, wherein the electrolyte adopts 1mol/L LiPF6The EC/DEC mixture of (1: 1 by volume) of (1) was used with Celgard2400 as a separator and metallic Li as a counter electrode. Discharging and charging conditions: discharged to 0.02V at the same current density and then recharged to 3V, the current density was selected to be 200 mA/g. The above batteries were tested, and the test results are shown in FIG. 2As can be seen from FIG. 2, the electrode material prepared according to the method of example 1 was charged and discharged at a current density of 200mA/g, and the reversible capacity was maintained at 299.6 mAh/g after 100 cycles.
Example 2
(1) 2.97g of zinc nitrate, 8.08g of ferric nitrate and 3.84g of citric acid were weighed out and dissolved in deionized water.
(2) 3.61g of lithium titanate is weighed and added into the mixed solution, the mixture is dispersed for 2 hours by strong ultrasonic, and the pH value of the solution is adjusted to 6.7 by ammonia water.
(3) Evaporating the solution to dryness at the temperature of 100 ℃ to obtain gel, heating the gel to 200 ℃ and keeping the temperature constant for 15min, and calcining the obtained product at the temperature of 600 ℃ for 5h in the air atmosphere to obtain the ferrite-lithium titanate composite negative electrode material. Li in composite negative electrode material4Ti5O12The content was 60 wt%.
And (3) electrochemical performance testing: the electrochemical test of this example was the same as that of example 1, and the test results are shown in FIG. 3. from FIG. 3, it can be seen that the electrode material prepared by the method of example 1 was charged and discharged at a current density of 200mA/g, and the reversible capacity was maintained at 383.6 mAh/g after 100 cycles.
Example 3
(1) 2.41g of copper nitrate, 8.08g of iron nitrate and 4.49g of glycine were weighed out and dissolved in deionized water.
(2) 9.56g of lithium titanate is weighed and added into the mixed solution, the mixture is dispersed for 2 hours by strong ultrasonic, and the pH value of the solution is adjusted to 6.9 by ammonia water.
(3) Evaporating the solution to dryness at the temperature of 90 ℃ to obtain gel, heating the gel to 250 ℃ and keeping the temperature constant for 10min, and calcining the obtained product at the temperature of 900 ℃ in air atmosphere for 0.5h to obtain the ferrite-lithium titanate composite negative electrode material. Li in composite negative electrode material4Ti5O12The content was 80 wt%.
And (3) electrochemical performance testing: the electrochemical test of this example was the same as that of example 1, and the test results are shown in FIG. 4. from FIG. 4, it can be seen that the electrode material prepared by the method of example 1 was charged and discharged at a current density of 200mA/g, and the reversible capacity was maintained at 265.4 mAh/g after 100 cycles.
Example 4
(1) A mixture of 2.56g of magnesium nitrate, 8.08g of ferric nitrate, 3.3g of citric acid and glycine was weighed out and dissolved in deionized water.
(2) Weighing 17.92g of lithium titanate, adding the lithium titanate into the mixed solution, performing strong ultrasonic dispersion for 2 hours, and adjusting the pH value of the solution to 6.5 by using ammonia water.
(3) Evaporating the solution to dryness at 130 ℃ to obtain gel, heating the gel to 250 ℃ and keeping the temperature constant for 10min, and calcining the obtained product at 900 ℃ for 0.5h in air atmosphere to obtain the ferrite-lithium titanate composite negative electrode material. Li in composite negative electrode material4Ti5O12The content was 90 wt%.
And (3) electrochemical performance testing: the electrochemical test of this example was the same as that of example 1, and the test results are shown in FIG. 5. from FIG. 5, it can be seen that the electrode material prepared by the method of example 1 was charged and discharged at a current density of 200mA/g, and the reversible capacity was maintained at 231.2mAh/g after 100 cycles.
Example 5
The procedure was substantially the same as in example 1, except that in step (1), 2.76g of a mixture of cobalt nitrate and magnesium nitrate, 8.08g of iron nitrate, 5.20g of a mixture of citric acid and glycine were weighed. Electrochemical test results show that the material of the example is charged and discharged under the current density of 200mA/g, and the reversible capacity is kept at 282.2mAh/g after 100 cycles.
Example 6
The procedure was substantially the same as in example 1, except that in step (1), 2.81g of a mixture of cobalt nitrate, copper nitrate and magnesium nitrate, 8.08g of iron nitrate, 5.60g of a mixture of citric acid, urea and glycine were weighed out. Electrochemical test results show that the material of the example is charged and discharged under the current density of 200mA/g, and the reversible capacity is kept at 278.6mAh/g after 100 cycles.
Example 7
The procedure was substantially the same as in example 1 except that in step (1), 2.64g of cobalt nitrate, zinc nitrate, a mixture of copper nitrate and magnesium nitrate, 8.08g of iron nitrate, 4.48g of citric acid, urea and glycine were weighed. Electrochemical test results show that the material of the example is charged and discharged at a current density of 200mA/g, and the reversible capacity is kept at 284.3mAh/g after 100 cycles.
Example 8
The procedure was substantially the same as in example 1, except that 18.10g of lithium titanate was weighed in the step (2). Electrochemical test results show that the material of the example is charged and discharged under the current density of 200mA/g, and the reversible capacity is kept at 197.5mAh/g after 100 cycles.
Example 9
The procedure was substantially the same as in example 1, except that in step (3), the solution was evaporated to dryness at 110 ℃ to obtain a gel, the gel was heated to 290 ℃ and kept at the constant temperature for 12min, and the product was calcined at 800 ℃ for 3.6h in an air atmosphere. Electrochemical test results show that the material of the example is charged and discharged at a current density of 200mA/g, and the reversible capacity is kept at 277.6mAh/g after 100 cycles.
Comparative example 1
A lithium titanate material which is not coated with ferrite.
And (3) electrochemical performance testing: the electrochemical performance test of this comparative example was the same as example 1, and the test results are shown in FIG. 6, Li4Ti5O12The material has a reversible capacity of 122.1mAh/g when cycled 100 times at a current density of 200 mA/g.
Comparative example 2
(1) 2.91g of cobalt nitrate, 8.08g of iron nitrate and 0.9g of urea were weighed out and dissolved in deionized water.
(2) 0.58g of lithium titanate is weighed and added into the mixed solution, the mixture is dispersed for 2 hours by strong ultrasonic, and the pH value of the solution is adjusted to 6.8 by ammonia water.
(3) Evaporating the solution to dryness at the temperature of 80 ℃ to obtain gel, heating the gel to 300 ℃ and keeping the temperature constant for 5min, and calcining the obtained product at the temperature of 800 ℃ for 2h in air atmosphere to obtain the ferrite-lithium titanate composite negative electrode material. Li in composite negative electrode material4Ti5O12The content is 20wt%, and the thickness of the coating layer is 3000 nm.
And (3) electrochemical performance testing: the electrochemical performance test of this comparative example was the same as example 1, and the obtained negative electrode material had a reversible capacity of 159.1 mAh/g after 100 cycles at a current density of 200 mA/g.
Claims (5)
1. A preparation method of a ferrite-lithium titanate composite negative electrode material for a lithium ion battery is characterized by comprising the following steps:
(1) weighing M (NO)3)2、Fe(NO3)3Mixing with combustion improver and dissolving in deionized water, wherein the M element is at least one of Co, Zn, Cu and Mg; m (NO)3)2With Fe (NO)3)3In a molar ratio of 1: 2, the molar ratio of the nitrate to the combustion improver is 1: (0.5 to 6);
(2) adding Li to the solution4Ti5O12Strongly ultrasonically dispersing for 2h, and adjusting the pH value of the solution to 6.5-7.0 by using ammonia water;
(3) evaporating the solution to dryness at the temperature of 80-130 ℃ to obtain gel, heating the gel to 200-300 ℃, keeping the temperature for 5-15 min, and then performing an air atmosphere calcination process to obtain the composite negative electrode material.
2. The preparation method of claim 1, wherein the combustion improver is one of glycine, citric acid and urea or a mixture of more than one of glycine, citric acid and urea.
3. The method of claim 1, wherein the calcining conditions are: the calcining temperature is 600-900 ℃, and the calcining time is 0.5-5 h.
4. The method of claim 1, wherein the composite negative electrode material comprises lithium titanate Li4Ti5O12And coating the Li4Ti5O12A ferrite coating layer on the surface, wherein the ferrite is CoFe2O4、ZnFe2O4、CuFe2O4And MgFe2O4At least one of, the Li4Ti5O12The composite negative electrode material accounts for 50-90% of the total mass of the composite negative electrode material, and the composite negative electrode material has a porous micro-nano structure.
5. The method of claim 4, wherein the ferrite coating has a thickness of 20 to 2000 nm.
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| CN106512874A (en) * | 2015-09-09 | 2017-03-22 | 中国科学院理化技术研究所 | Method of coating glass hollow microsphere surface with spinel type ferrite shell, obtained hollow composite microsphere and application thereof |
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| CN102769128A (en) * | 2011-05-04 | 2012-11-07 | 三星电子株式会社 | Electrode active material, preparation method thereof, and electrode and lithium battery containing the same |
| CN106512874A (en) * | 2015-09-09 | 2017-03-22 | 中国科学院理化技术研究所 | Method of coating glass hollow microsphere surface with spinel type ferrite shell, obtained hollow composite microsphere and application thereof |
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