CN108258215B - Method for preparing carbon-coated lithium iron phosphate material and application thereof - Google Patents
Method for preparing carbon-coated lithium iron phosphate material and application thereof Download PDFInfo
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Abstract
The application discloses a method for preparing a carbon-coated lithium iron phosphate material, which is characterized by adopting a one-pot synthesis method and at least comprising the following steps of: a) grinding a mixture containing a melamine compound, a lithium source and an iron source to obtain a precursor I; b) adding phosphoric acid into the precursor I, and grinding to obtain a precursor II; c) drying the precursor II in vacuum, and performing ball milling to obtain a precursor III; d) and (3) placing the precursor III in an inactive atmosphere for sectional calcination to obtain the carbon-coated lithium iron phosphate material. The method is obtained by adopting a one-pot synthesis method and one-step reaction synthesis. The method has the advantages of simple and controllable reaction conditions, low requirement on experimental equipment, environmental friendliness and high product yield, and the prepared carbon-coated lithium iron phosphate (LiFePO)4and/C), the electrochemical performance of the material is effectively improved through carbon coating. The method has simple production process, is easy for industrial amplification and realizes commercialization.
Description
Technical Field
The application relates to a method for synthesizing carbon-coated lithium iron phosphate, belonging to the field of chemical engineering.
Background
Lithium ion batteries, the foremost rechargeable batteries, have attracted widespread attention throughout the world in the last decade. At present, the portable electronic equipment portable power supply market is led, the portable electronic equipment portable power supply becomes the only power supply equipment of a mobile phone and a notebook computer, and even the power supply equipment further advances the power battery field. Since Padhi et al broke through the technical difficulty of the polyanion of olive-type phosphate, LiFePO4And is also increasingly becoming a dazzling "star" for the lithium battery industry. The lithium iron phosphate has the advantages of low cost, no toxicity, environmental friendliness, wide iron source, higher specific capacity (the theoretical capacity is 170mAh/g, and the energy density is 550wh/kg), high discharge platform (3.6V), longer cycle life, good high-temperature heating stability and the like. In the field of development and application of new energy automobiles, lithium ion batteries with low price, low energy consumption, environmental protection, no pollution and high specific energy are required, and the traditional battery system is difficult to meet the requirement of high energy density, so that the development of novel high specific capacity lithium ion batteries is urgently needed. Lithium iron phosphateThe lithium ion battery cathode material has excellent electrochemical performance and is one of ideal lithium ion battery cathode materials.
Disclosure of Invention
According to one aspect of the present application, a method of preparing conductive carbon-coated lithium iron phosphate is provided. The method is obtained by adopting a one-pot synthesis method and one-step reaction synthesis. The method has the advantages of simple and controllable reaction conditions, low requirement on experimental equipment, environmental friendliness and high product yield, and the prepared carbon-coated lithium iron phosphate (LiFePO)4and/C), the electrochemical performance of the material is effectively improved through carbon coating. The method has simple production process, is easy for industrial amplification and realizes commercialization.
The method for preparing the carbon-coated lithium iron phosphate material is characterized by adopting a one-pot synthesis method and at least comprising the following steps of:
a) grinding a mixture containing a melamine compound, a lithium source and an iron source to obtain a precursor I;
b) adding phosphoric acid into the precursor I, and grinding to obtain a precursor II;
c) drying the precursor II in vacuum, and performing ball milling to obtain a precursor III;
d) and (3) placing the precursor III in an inactive atmosphere for sectional calcination to obtain the carbon-coated lithium iron phosphate material.
Preferably, the melamine-based compound in step a) is at least one selected from the group consisting of compounds having the formula shown in formula I:
wherein R is1、R2、R3、R4、R5、R6Independently selected from H, methyl, ethyl, propyl.
Preferably, the melamine-based compound in step a) is melamine.
Preferably, the lithium source in step a) is lithium oxalate; the iron source is ferric oxide.
Preferably, in the mixture containing melamine compound, lithium source and iron source in step a), the molar ratio of melamine compound to lithium source to iron source is:
melamine compound: li: fe is 1-3: 1: 1-2;
wherein the mole number of the melamine compound is calculated by the mole number of the melamine compound; the number of moles of the lithium source is calculated by the number of moles of lithium element contained in the lithium source; the number of moles of the iron source is based on the number of moles of the iron element contained in the iron source.
Further preferably, in the mixture containing melamine compound, lithium source and iron source in step a), the molar ratio of melamine compound to lithium source to iron source is:
melamine compound: li: fe ═ 1:1: 1.
Preferably, the molar ratio of phosphoric acid to lithium in the precursor I in the step b) is 1-3: 1;
preferably, the molar ratio of the phosphoric acid in the step b) to the iron element in the precursor I is 1-1.5: 1.
preferably, the vacuum drying in the step c) is vacuum drying at 60-80 ℃ for 3-6 h; the ball milling is carried out for 6-12 h at the rotating speed of 400-600 rpm.
Optionally, the upper limit of the vacuum drying temperature is selected from 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃; the lower limit is selected from 30 deg.C, 40 deg.C, 50 deg.C, 60 deg.C, 70 deg.C.
Optionally, the upper limit of the vacuum drying time is selected from 4h, 5h, 6h, 7h, 8h, 9 h; the lower limit is selected from 1h, 2h, 3h and 4 h.
Preferably, the inert atmosphere in step d) is selected from at least one of nitrogen, helium, argon, krypton and xenon.
Preferably, the staged calcination in step d) is a two-stage calcination comprising:
firstly, heating to 150-350 ℃ at a heating rate of 1-5 ℃/min, and preserving heat for 1-5 h (first-stage calcination); then heating to 600-800 ℃ at a heating rate of 1-8 ℃/min and calcining for 8-12 h (second stage calcining).
Optionally, the upper limit of the heating temperature of the first stage calcination is selected from 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 500 ℃; the lower limit is selected from the group consisting of 50 deg.C, 100 deg.C, 150 deg.C, and 200 deg.C.
Optionally, the upper limit of the holding time for the first stage calcination is selected from 3h, 4h, 5h, 8h, 10 h; the lower limit is selected from 0.5h, 1h, 2h, 3h and 5 h.
Optionally, the upper limit of the heating rate of the first stage calcination is selected from 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min, 9 ℃/min, 10 ℃/min; the lower limit is selected from 0.5 deg.C/min, 1 deg.C/min, 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min.
Optionally, the upper limit of the heating temperature of the second stage calcination is selected from 500 ℃, 550 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃; the lower limit is selected from 100 deg.C, 200 deg.C, 300 deg.C, 500 deg.C, 600 deg.C.
Optionally, the upper limit of the holding time of the second stage calcination is selected from 8h, 10h, 12h, 15h, 20 h; the lower limit is selected from 5h, 6h, 7h, 8h and 10 h.
Optionally, the upper limit of the heating rate of the second stage calcination is selected from 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min, 9 ℃/min, 10 ℃/min; the lower limit is selected from 0.5 deg.C/min, 1 deg.C/min, 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, 6 deg.C/min.
As a specific embodiment, the method for preparing conductive carbon-coated lithium iron phosphate includes:
(1) accurately weighing 3.784g of melamine, 1.529g of lithium oxalate and 2.396g of ferric oxide, placing the materials in a mortar for full grinding to obtain red powder, weighing 2.05mL of phosphoric acid, adding the phosphoric acid into the mixture, and grinding the mixture until the mixture becomes uniform sticky wet powder;
(2) drying the sticky wet powder for 3-5 h at 60-80 ℃ in vacuum, grinding the powder by using a mortar after drying, and performing ball milling for 6-12 h at the rotating speed of 600rpm to obtain a precursor;
(3) placing the obtained precursor into a tube furnace, filling argon, heating to 150-350 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 1-5 h, heating to 600-800 ℃ at a heating rate of 1-8/min, calcining for 8-12 h, cooling to room temperature, taking out the product, and grinding to obtain black powder. Black powder is the final product of the preparation.
According to another aspect of the present application, there is provided a lithium ion battery, wherein the lithium ion battery contains the carbon-coated lithium iron phosphate material prepared according to any of the above methods. Namely, the carbon-coated lithium iron phosphate material is applied to a lithium ion battery.
Benefits that can be produced by the present application include, but are not limited to:
1) according to the method provided by the application, a one-pot synthesis method is adopted, and the carbon-coated lithium iron phosphate material can be prepared through one-step reaction.
2) The method provided by the application has the advantages of simple production process, simple and controllable reaction conditions, low requirement on experimental equipment, environmental friendliness, high product yield and easiness in industrial amplification and commercialization realization.
3) The method provided by the application, the prepared carbon-coated lithium iron phosphate (LiFePO)4and/C), the electrochemical performance of the material is effectively improved.
Drawings
FIG. 1 is a schematic process flow diagram of the process described herein.
FIG. 2 shows sample 1#Scanning electron micrograph (c).
FIG. 3 shows sample 1#X-ray diffraction spectrum and LiFePO of4And (5) comparison of standard spectrograms.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials in the examples were all purchased commercially and used without special treatment.
FIG. 1 is a schematic process flow diagram of the process described herein. In fig. 1, the raw material corresponds to the precursor II, the precursor corresponds to the precursor III, and the target product corresponds to the carbon-coated lithium iron phosphate material.
In the examples, the scanning electron microscope of the sample was characterized by a field emission scanning electron microscope model FEI Nova NanoSEM 450.
In the examples, the X-ray diffraction analysis (XRD) of the samples was characterized using Bruker D8 ADVANCE.
In the examples, ball milling was carried out using a ball mill model QM-3SP04 from Nanjing, Nanda instruments Ltd. (ball-to-feed ratio by mass: 12.5; average ball diameter: 8 mm).
Example 1 sample 1#Preparation of
Pretreatment of raw materials: 3.784g of melamine, 1.529g of lithium oxalate and 2.396g of ferric oxide were accurately weighed by an electronic balance, and were put in a mortar to be sufficiently ground to obtain red powder, 2.05mL of phosphoric acid was weighed, and then added to the above mixture to be ground until it became uniformly sticky and wet powder.
Ball milling: and (3) drying the sticky wet powder for 5h in vacuum at 80 ℃, grinding the powder by using a mortar after the powder is dried, and then performing ball milling for 10h at the rotating speed of 600rpm to obtain a precursor.
And (3) calcining: placing the obtained precursor in a tube furnace, filling argon, heating to 350 ℃ at a heating rate of 4 ℃/min, preserving heat for 4h, heating to 700 ℃ at a heating rate of 3 ℃/min, calcining for 12h, cooling to room temperature, taking out the product, and grinding to obtain black powder. The black powder is the final product of the present invention and is designated as sample 1#。
Example 2 sample 2#～9#Preparation of
Sample 2#～9#The procedure of preparation, the raw materials used were the same as in sample 1 of example 1#Except that the conditions in the ball milling process and the calcination process were changed. The sample numbers and the preparation conditions are shown in Table 1.
TABLE 1
EXAMPLE 3 structural characterization of the samples
For sample 1#～9#X-ray powder diffraction phase analysis (XRD) was performed. The results show that sample 1 prepared in examples 1 and 2#～9#All samples were of high purity and high crystallinity.
With sample 1#Is a typical representation, and the XRD spectrum thereof is similar to that of LiFePO4The pair of standard spectra is shown in figure 3. As can be seen from FIG. 3, sample 1#The heights of the XRD diffraction patterns are consistent, and the obtained samples are proved to be high-purity and high-crystallinity samples. Sample 2#Sample 9#XRD spectrum of (1) and sample#Similarly, the peak position was substantially unchanged, and the peak intensity varied within a range of. + -. 5% depending on the synthesis conditions.
EXAMPLE 4 topographical characterization of samples
For sample 1#～9#And carrying out shape characterization by using a scanning electron microscope. The results show that sample 1#～9#The average particle size is uniformly distributed, and no obvious large block formed by particle agglomeration is seen.
With sample 1#As a representative, SEM photograph thereof is shown in fig. 2. As can be seen from FIG. 2, sample 1#The particle size of the composite material is about 1 micron, no obvious large block agglomeration exists, and the composite material is in a short rod shape with uniform distribution. Sample 2#Sample 9#SEM picture of (1) and sample#The shapes are similar and are all short rod-shaped, the overall shape of the sample changes with the synthesis temperature, and the particle size changes within the range of +/-50%.
Example 5 preparation of lithium ion batteries
Respectively with sample 1#～9#The performance of the positive electrode material is measured, and specifically comprises the following steps:
respectively and uniformly dispersing the obtained carbon-coated lithium iron phosphate material sample with conductive carbon black Super-P as a conductive agent and polyvinylidene fluoride (PVDF is abbreviated as the binder, and the mass percentage of the polyvinylidene fluoride in the binder is 10%) in N-methylpyrrolidone (NMP) as a solvent to prepare the carbon-coated lithium iron phosphate material sampleA positive electrode slurry. The solid content of the positive electrode slurry is 75 wt%, and the solid component comprises 80 wt% of carbon-coated lithium iron phosphate material, 10 wt% of PVDF and 10 wt% of conductive carbon black Super-P. The anode slurry is evenly coated on an anode current collector aluminum foil with the diameter of 16mm, and the solid coating weight is about 0.008g/cm2. And (3) drying at 80 ℃, punching and tabletting, and drying at 120 ℃ for 4h under a vacuum condition to obtain the positive plate.
The electrolyte adopts a mixed solution of 1mol/L lithium hexafluorophosphate in ethylene carbonate, diethyl carbonate and dimethyl carbonate; wherein the volume ratio of the ethylene carbonate, the diethyl carbonate and the dimethyl carbonate is 1:1:1, the diaphragm adopts a polypropylene porous membrane (Celgard2400), the negative electrode adopts a round lithium sheet with the diameter of 15mm, and the round lithium sheet is assembled into a CR2032 type button battery in a glove box.
Respectively with sample 1#～9#The batteries prepared for the cathode materials are respectively marked as C1#～C9#。
Example 6 electrochemical Performance characterization
For battery C1#～C9#Specifically, the electrochemical performance of (a) is evaluated as follows:
the charging and discharging were repeated under the conditions of an ambient temperature of 25 ℃ and a current magnification of 1C. The voltage range is 2.5V-4.2V.
The result shows that the lithium ion battery prepared by taking the carbon-coated lithium iron phosphate material obtained by the application as the anode material can still reach 110mAh g after 500 cycles of discharge cycle-1。
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A method for preparing a carbon-coated lithium iron phosphate material is characterized by adopting a one-pot synthesis method and at least comprising the following steps of:
a) grinding a mixture containing a melamine compound, a lithium source and an iron source to obtain a precursor I;
b) adding phosphoric acid into the precursor I, and grinding to obtain a precursor II;
c) drying the precursor II in vacuum, and performing ball milling to obtain a precursor III;
d) placing the precursor III in an inactive atmosphere for sectional calcination to obtain the carbon-coated lithium iron phosphate material;
the step d) of the sectional calcination is divided into two sections of calcination, and comprises the following steps:
firstly, heating to 150-350 ℃ at a heating rate of 1-5 ℃/min, and keeping the temperature for 1-5 h; heating to 600-800 ℃ at a heating rate of 1-8 ℃/min and calcining for 8-12 h;
in the mixture containing the melamine compound, the lithium source and the iron source in the step a), the molar ratio of the melamine compound to the lithium source to the iron source is as follows:
melamine compound: li: fe is 1-3: 1: 1-2;
wherein the mole number of the melamine compound is calculated by the mole number of the melamine compound; the number of moles of the lithium source is calculated by the number of moles of lithium element contained in the lithium source; the number of moles of the iron source is based on the number of moles of the iron element contained in the iron source.
2. The method as claimed in claim 1, wherein the melamine-based compound in step a) is at least one compound selected from the group consisting of compounds having the formula shown in formula I:
wherein R is1、R2、R3、R4、R5、R6Independently selected from H, methyl, ethyl, propyl.
3. The process according to claim 1, characterized in that the melamine-based compound in step a) is melamine.
4. The method according to claim 1, wherein the lithium source in step a) is lithium oxalate; the iron source is ferric oxide.
5. The method according to claim 1, wherein in the mixture containing the melamine compound, the lithium source and the iron source in step a), the molar ratio of the melamine compound to the lithium source to the iron source is as follows:
melamine compound: li: fe ═ 1:1: 1.
6. The method according to claim 1, wherein the molar ratio of phosphoric acid to lithium in the precursor I in the step b) is 1-3: 1.
7. the method according to claim 6, wherein the molar ratio of phosphoric acid to lithium in the precursor I in the step b) is 1-1.5: 1.
8. the method according to claim 1, wherein the vacuum drying in step c) is vacuum drying at 60-80 ℃ for 3-6 h; the ball milling is carried out for 6-12 h at the rotating speed of 400-600 rpm.
9. The method according to claim 1, wherein the inert atmosphere in step d) is selected from at least one of nitrogen, helium, argon, krypton and xenon.
10. A lithium ion battery characterized by containing the carbon-coated lithium iron phosphate material prepared by the method according to any one of claims 1 to 9.
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