CN109860573B - Graphene-based vehicle lithium ion battery positive electrode material and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene-based vehicle lithium ion battery anode material and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a mixed solution of PVP glue solution, lithium salt, ferric salt, graphene oxide dispersion liquid and ethyl orthosilicate ethanol solution, spray-drying the mixed solution to obtain a precursor, and sintering the precursor. By reacting Li according to the invention2FeSiO4The control of the generated particle size and the construction of the graphene and the carbon conductive network enhance the conductivity of the material, reduce the diffusion distance of lithium ions, reduce polarization and improve the multiplying power performance2FeSiO4The surface is coated with the carbon material and the graphene, so that the occurrence of side reactions is effectively reduced, the cycle performance of the material is improved, and the safety performance of the material is excellent.
Description
Technical Field
The invention relates to the technical field of lithium ion battery material preparation, in particular to a graphene-based vehicle lithium ion battery anode material and a preparation method thereof.
Background
Global climate change, anthropogenic greenhouse gas release and increasing energy demand are the most pressing problems currently placed on mankind, mainly caused by the huge consumption of fossil fuels (mainly coal, oil, natural gas). Therefore, energy diversification and the development of renewable green energy are not essential, and among various technologies in the renewable energy field, energy storage and conversion technology, especially electrochemical energy storage, is one of the fields with the greatest prospect and the fastest development.
The lithium ion battery is one of the most excellent secondary batteries in electrochemical energy storage at present, and has very high energy and power density, so that the lithium ion battery becomes the best choice for energy storage of electric tools, electronic mobile equipment, pure electric vehicles, hybrid electric vehicles and the like. The electrode material is the key for determining the performance of the lithium ion battery, and researches on the negative electrode material and an electrolyte system are carried out for decades, particularly the specific capacity, the safety stability and the cycle performance of the negative electrode material reach higher levels, but the research on the positive electrode material is relatively lagged while the requirements of people on various aspects of the lithium ion battery are improved.
The ternary positive electrode material and the high-nickel positive electrode material which are greatly popular in the market at present have (1) poor high-temperature cycle performance and capacity retention at high temperature although the capacities are high; (2) the nickel content of the material is high, the material synthesis has strict requirements on the atmosphere, and the material is easy to absorb water and deteriorate when stored in the atmospheric environment, so that the synthesis is difficult; (3) the compact density is relatively low and the safety of the battery is deteriorated due to the gas generated during the charging process. For electric vehicles, in addition to having a suitable capacity, the rate capability and safety performance of the battery are very critical, and a lithium ion battery cathode material having high ion electronic conductivity and high thermal stability is needed at present.
In recent years, because the novel polyanion lithium silicate positive electrode material can effectively and reversibly insert and remove lithium ions, the electrochemical performance is excellent, and the structure of the Si-O bond is relatively strong, the thermal stability of the material is excellent, and the research and development interests of people are widely aroused; wherein Li2FeSiO4The method is well focused by researchers, because the contents of Si and Fe in the crust of the earth respectively account for the second and fourth sites, the raw materials are naturally reserved and are rich, the theoretical capacity is high, the cycle stability is good, the thermal stability is good, and the method has a good development prospect. But Li2FeSiO4The first several circles of capacity has fast attenuation speed and the materialThe conductivity and lithium ion diffusion coefficient of the material are low. There is still a lack of targeting for Li2FeSiO4A better modification scheme with poor conductivity and poor cycle performance.
The invention uses graphene and PVP (polyvinylpyrrolidone) to react with Li2FeSiO4The size of the generated particles is limited, the lithium ion transmission path is reduced, and the lithium ion transmission speed of the material is improved; the preparation method realizes Li2FeSiO4The small particles are uniformly distributed in the graphene/carbon conductive network, so that the graphene/carbon conductive network has better conductivity; the coating of the graphene/carbon also prevents the direct contact of the electrolyte and the lithium ion battery anode material, and inhibits the reaction between the lithium ion battery anode material and the electrolyte, so that the lithium ion battery anode material has more excellent cycle performance; the structural stability of the material also enables the material to have more excellent safety performance than the traditional lithium ion battery material for the vehicle.
Disclosure of Invention
The invention provides a graphene-based vehicle lithium ion battery anode material and a preparation method thereof, and solves the problem of Li in the prior art2FeSiO4Low conductivity and lithium ion diffusion coefficient, poor safety and poor cycle performance.
The invention provides a graphene-based vehicle lithium ion battery positive electrode material and a preparation method thereof, wherein the preparation method comprises the following steps:
PVP and deionized water are mixed according to the weight ratio of 1: mixing at a ratio of 10-100, stirring for 0.5-2 hr, and making into PVP glue solution;
step 2, preparing a graphene oxide mixed solution:
lithium salt and iron salt are added according to the proportion of lithium element: mixing the iron element with a molar ratio of 2:1 to obtain mixed salt, and uniformly mixing the mixed salt and water according to a weight ratio of 1:10-50 to obtain mixed salt solution; mixing the mixed salt solution with the PVP glue solution, stirring for 1-6 hours, adding the graphene oxide dispersion liquid, and stirring for 1-6 hours to obtain a graphene oxide mixed solution;
wherein the weight ratio of graphene oxide to lithium salt in the graphene oxide dispersion liquid is 0.5-1: 1;
the weight ratio of PVP to lithium salt is 1-15: 1;
step 3, preparing carbon/graphene/Li2FeSiO4Precursor:
preparing ethyl orthosilicate ethanol solution with the concentration of 0.01-1 g/mL; then mixing the ethyl orthosilicate ethanol solution with the graphene oxide mixed solution obtained in the step 2, and stirring for 1-3 hours to obtain carbon/graphene/Li2FeSiO4Precursor solution; mixing carbon/graphene/Li2FeSiO4Spray drying the precursor solution to obtain carbon/graphene/Li2FeSiO4A precursor;
the molar ratio of silicon element in the ethyl orthosilicate to lithium element in the lithium salt is 1: 2;
step 4, preparing carbon/graphene/Li2FeSiO4A positive electrode material:
under reducing atmosphere, adding carbon/graphene/Li2FeSiO4Sintering the precursor at the temperature of 450-900 ℃ for 6-24 hours, and cooling the sintered sample along with the furnace to obtain the carbon/graphene/Li2FeSiO4A positive electrode material, the carbon/graphene/Li2FeSiO4The anode material is the anode material of the lithium ion battery for the vehicle.
Preferably, the lithium salt in step 2 is one of anhydrous lithium hydroxide, lithium carbonate and lithium acetate.
Preferably, the ferric salt in step 2 is one of ferrous acetate, ferrous oxalate, ferrous citrate, ferric acetate, ferric oxalate pentahydrate and ferric citrate.
Preferably, the atmosphere in the step 4 is formed by a mixed gas of an inert gas and a reducing gas, the inert gas accounts for 90-99% of the mixed gas by volume, and the rest gas is the reducing gas; the inert gas is one or more of nitrogen and argon; the reducing gas is one or more of hydrogen and carbon monoxide.
Preferably, the spray drying conditions in step 3 are as follows: the temperature of the air inlet is 145-165 ℃, and the temperature of the air outlet is 90-110 ℃.
The second purpose of the invention is to provide carbon/graphene/Li prepared by the method2FeSiO4And (3) a positive electrode material.
Compared with the prior art, the invention has the beneficial effects that:
1) in the invention, Li is formed in situ in PVP solution and graphene oxide solution2FeSiO4Can effectively limit Li2FeSiO4The size of the particle generation. The control of the size of the material particles in a smaller range is equivalent to effectively shortening the lithium ion diffusion path, and simultaneously can also improve the utilization rate of active substances around the particles.
2) In the invention, through the organic combination of PVP and graphene, the graphene serving as a framework is formed in the finally generated cathode material, and the small-particle Li is wrapped2FeSiO4And the multistage conductive network filled with the carbon material further improves the conductivity of the material, reduces polarization and improves the rate capability of the material.
3) According to the invention, the precursor is pelletized by a spray drying method, so that the production is easy, the tap density of spherical particles is high, and the volume energy density of the full cell can be greatly improved.
4) Because of the stability of the material, the material has excellent safety performance, and the overall safety of the battery is greatly improved.
5) By reaction of Li with2FeSiO4The surface is coated with the carbon material and the graphene, so that the occurrence of side reactions is effectively reduced, and the cycle performance of the material is improved.
Drawings
FIG. 1 shows carbon/graphene/Li in example 1 of the present invention2FeSiO4A Scanning Electron Microscope (SEM) image of the cathode material at 5 ten thousand times;
FIG. 2 shows carbon/graphene/Li in example 1 of the present invention2FeSiO4A scanning electron microscope with 10 ten thousand times of the anode material;
FIG. 3 shows carbon/graphene/Li in example 2 of the present invention2FeSiO4A scanning electron microscope image of the cathode material under 5 ten thousand times;
FIG. 4 shows carbon/graphene/Li in example 2 of the present invention2FeSiO4Scanning electron microscope images of the anode material under 10 ten thousand times;
FIG. 5 shows carbon/graphene/Li in examples 1 and 2 of the present invention2FeSiO4XRD pattern of cathode material, where a is carbon/graphene/Li of example 12FeSiO4XRD pattern of the positive electrode material; b is carbon/graphene/Li of example 22FeSiO4XRD pattern of the positive electrode material;
FIG. 6 carbon/graphene/Li in example 1 of the present invention2FeSiO4Cycle performance diagram of the positive electrode material;
FIG. 7 carbon/graphene/Li in example 2 of the present invention2FeSiO4Cycle performance diagram of the positive electrode material.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are commercially available, wherein the graphene oxide dispersion used is available from senixi materials science and technology ltd, usa under model No. SE 3521; the spray dryer used was purchased from Shanghai Johnupon industries, Inc. and was model QFN-8000 ST.
Example 1
A graphene-based vehicle lithium ion battery anode material and a preparation method thereof comprise the following steps:
mixing 20g of PVP and 250g of deionized water, and stirring the PVP glue solution for 1 hour to prepare a PVP glue solution;
step 2, preparing a graphene oxide mixed solution:
mixing 2g of lithium carbonate and 4.7g of ferrous acetate, and adding 70g of water to prepare a mixed salt solution; mixing the mixed salt solution with 270g of PVP glue solution, stirring for 3 hours, adding 60g of graphene oxide dispersion liquid (3 wt.%), and stirring for 3 hours to obtain a graphene oxide mixed solution;
step 3, preparing carbon/graphene/Li2FeSiO4Precursor:
dissolving 6g of tetraethoxysilane in 13ml of ethanol to prepare an ethanol solution of tetraethoxysilane; then mixing the ethyl orthosilicate ethanol solution with the graphene oxide mixed solution obtained in the step 2, and stirring for 2 hours to obtain carbon/graphene/Li2FeSiO4Precursor solution; mixing carbon/graphene/Li2FeSiO4And carrying out spray drying on the precursor solution to obtain a precursor. The temperature of the air inlet of the spray drying is 150 ℃, and the temperature of the air outlet is 95 ℃;
the molar ratio of silicon element in the ethyl orthosilicate to lithium element in the lithium carbonate is 1: 2;
and 4, sintering the precursor:
sintering for 12 hours at 650 ℃ in a mixed atmosphere of nitrogen and hydrogen with a volume ratio of 95:5, and cooling the sintered sample along with the furnace to obtain the carbon/graphene/Li2FeSiO4And (3) a positive electrode material.
Example 2
A graphene-based vehicle lithium ion battery anode material and a preparation method thereof comprise the following steps:
mixing 60g of PVP and 600g of deionized water, and stirring the PVP glue solution for 0.5 hour to prepare a PVP glue solution;
step 2, preparing a graphene oxide mixed solution:
60g of anhydrous lithium hydroxide and 292g of ferric oxalate pentahydrate are mixed, 3520g of water is added, and a mixed salt solution is prepared; mixing the mixed salt solution with 660g of PVP glue solution, stirring for 1 hour, then adding 1000g of graphene oxide dispersion liquid (3 wt.%), and stirring for 1 hour to obtain a graphene oxide mixed solution;
step 3, preparing carbon/graphene/Li2FeSiO4Precursor:
dissolving 1044g of tetraethoxysilane in 104400ml of ethanol to prepare an ethanol solution of tetraethoxysilane; then mixing the ethyl orthosilicate ethanol solution with the graphene oxide mixed solution obtained in the step 2, and stirring for 1 hour to obtain carbon/graphene/Li2FeSiO4Precursor solution; mixing carbon/graphene/Li2FeSiO4And carrying out spray drying on the precursor solution to obtain a precursor. The temperature of the air inlet of the spray drying is 145 ℃, and the temperature of the air outlet of the spray drying is 90 ℃;
the molar ratio of silicon element in the ethyl orthosilicate to lithium element in the anhydrous lithium hydroxide is 1: 2;
and 4, sintering the precursor:
sintering for 6 hours at 450 ℃ in a mixed atmosphere of argon and hydrogen with the volume ratio of 90:10, and cooling the sintered sample along with the furnace to obtain the carbon/graphene/Li2FeSiO4And (3) a positive electrode material.
Example 3
A graphene-based vehicle lithium ion battery anode material and a preparation method thereof comprise the following steps:
mixing 15g of PVP and 1500g of deionized water, and stirring the PVP glue solution for 2 hours to prepare a PVP glue solution;
step 2, preparing a graphene oxide mixed solution:
mixing 1g of anhydrous lithium hydroxide and 3g of ferrous oxalate, adding 200g of water, and preparing a mixed salt solution; mixing the mixed salt solution with 1515g of PVP glue solution, stirring for 6 hours, adding 33g of graphene oxide dispersion liquid (3 wt.%), and stirring for 6 hours to obtain a graphene oxide mixed solution;
step 3, preparing carbon/graphene/Li2FeSiO4Precursor:
dissolving 17g of tetraethoxysilane in 17ml of ethanol to prepare an ethanol solution of tetraethoxysilane; then the ethyl orthosilicate ethanol solution is mixed with the ethanol solution obtained in the step 2Mixing the graphene oxide mixed solution, and stirring for 3 hours to obtain carbon/graphene/Li2FeSiO4Precursor solution; mixing carbon/graphene/Li2FeSiO4And carrying out spray drying on the precursor solution to obtain a precursor. The temperature of the air inlet of the spray drying is 165 ℃, and the temperature of the air outlet is 110 ℃;
the molar ratio of silicon element in the ethyl orthosilicate to lithium element in the anhydrous lithium hydroxide is 1: 2;
and 4, sintering the precursor:
sintering the mixture for 24 hours at 900 ℃ in a mixed atmosphere with the volume ratio of nitrogen to hydrogen being 99:1, and cooling the sintered sample along with the furnace to obtain the carbon/graphene/Li2FeSiO4And (3) a positive electrode material.
For the carbon/graphene/Li prepared in examples 1 to 3 of the present invention2FeSiO4The positive electrode material is detected and characterized, and the specific experimental result is as follows:
1. SEM image analysis
Scanning electron microscope is adopted to carry out scanning electron microscopy on each prepared carbon/graphene/Li2FeSiO4The morphology of the cathode material is characterized, and specific SEM images are shown in fig. 1-4, wherein fig. 1 is the carbon/graphene/Li prepared in example 12FeSiO4An SEM image of the cathode material at 5 ten thousand times, and FIG. 2 shows carbon/graphene/Li prepared in example 1 of the present application2FeSiO4SEM image of the positive electrode material at 10 ten thousand times. As can be seen from FIGS. 1-2, the carbon/graphene/Li prepared in example 1 of the present application2FeSiO4The anode material is mainly micron-sized spherical particles, Li2FeSiO4The particle size of the graphene is small, and the graphene and carbon are wrapped well, so that the material is proved to have good conductivity and a short lithium ion diffusion path.
FIG. 3 is the carbon/graphene/Li prepared in example 22FeSiO4An SEM image of the cathode material at 5 ten thousand times, and FIG. 4 shows carbon/graphene/Li prepared in example 2 of the present application2FeSiO4SEM image of the positive electrode material at 10 ten thousand times. As can be seen from FIGS. 3-4, the carbon/graphene prepared in example 2 of the present application/Li2FeSiO4The positive electrode material has similar shape and state as those in example 1, and is micron-sized spherical particles, Li2FeSiO4The particle size of the graphene is small, and the graphene and carbon are wrapped well, so that the material is proved to have good conductivity and a short lithium ion diffusion path.
2. XRD Pattern analysis
In FIG. 5, the carbon/graphene/Li of example 1-22FeSiO4XRD pattern of positive electrode material, wherein curve a is carbon/graphene/Li in example 12FeSiO4XRD pattern of the cathode material, curve b is carbon/graphene/Li in example 22FeSiO4XRD pattern of the positive electrode material. From both a and b in fig. 5, it can be seen that the sample synthesized in example 1-2 has characteristic derivative peaks at angles of 16.68 °, 24.29 °, 28.47 °, 33.07 °, 35.67 °, 37.67 °, 48.25 ° and 59.83 °, and the diffraction peaks are relatively sharp and have relatively good intensity, indicating that the composite structure strengthens Li2FeSiO4The crystallinity of (a). No characteristic peaks of carbon were found in the XRD pattern, probably because the carbon material was mainly amorphous.
3. Analysis of electrochemical Properties
To examine the carbon/graphene/Li prepared in examples 1 to 3 of the present invention2FeSiO4And (3) assembling the positive electrode material into a half cell for testing according to various performance parameters of the positive electrode material. The half cell uses a metal lithium sheet as a negative electrode, and uses the carbon/graphene/Li of the embodiment2FeSiO4The anode material is the anode, and the button cell is assembled in a glove box which is filled with argon and strictly controls the water oxygen index.
carbon/graphene/Li in example 12FeSiO4The positive electrode material is charged and discharged at 0.1C under the voltage of 1.5-4.8V, and the first reversible specific capacity is 135.6mAh g-15C charging and discharging, the first discharge point capacity is 126.3mAh g-1The capacity of the material after 50 cycles is 123.3mAh g-1The capacity retention rate was 97.62%. FIG. 6 shows carbon/graphene/Li in example 12FeSiO4The cycle performance of the anode material is better.
Carbon/graphene in example 2/Li2FeSiO4The positive electrode material is charged and discharged at 0.1C under the voltage of 1.5-4.8V, and the first reversible specific capacity is 134.2mAh g-15C charging and discharging, the first discharge point capacity is 99.7mAh g-1The capacity of the material after 50 cycles is 98.6mAh g-1The capacity retention rate was 98.90%. FIG. 7 shows carbon/graphene/Li in example 22FeSiO4The cycle performance of the anode material is better.
From the performance, the carbon/graphene/Li2FeSiO4The positive electrode material has high reversible capacity, high reversible capacity and good cycle performance under 5C high multiplying power, the coating layer isolates the contact between the positive electrode material and electrolyte, the occurrence of side reactions is reduced, the electrochemical performance of the material is improved, and the construction of the conductive network enables the material to have low polarization.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (5)
1. A preparation method of a graphene-based vehicle lithium ion battery positive electrode material is characterized by comprising the following steps:
step 1, preparing PVP glue solution
PVP and deionized water are mixed according to the weight ratio of 1: mixing at a ratio of 10-100, stirring for 0.5-2 hr, and making into PVP glue solution;
step 2, preparing a graphene oxide mixed solution
Lithium salt and iron salt are added according to the proportion of lithium element: mixing the iron element with a molar ratio of 2:1 to obtain mixed salt, and uniformly mixing the mixed salt and water according to a weight ratio of 1:10-50 to obtain mixed salt solution; mixing the mixed salt solution with the PVP glue solution, stirring for 1-6 hours, adding the graphene oxide dispersion liquid, and stirring for 1-6 hours to obtain a graphene oxide mixed solution;
wherein the weight ratio of graphene oxide to lithium salt in the graphene oxide dispersion liquid is 0.5-1: 1;
the weight ratio of PVP to lithium salt is 1-15: 1;
step 3, preparing carbon/graphene/Li2FeSiO4Precursor body
Preparing ethyl orthosilicate ethanol solution with the concentration of 0.01-1 g/mL; then mixing the ethyl orthosilicate ethanol solution with the graphene oxide mixed solution obtained in the step 2, and stirring for 1-3 hours to obtain carbon/graphene/Li2FeSiO4Precursor solution; mixing carbon/graphene/Li2FeSiO4Spray drying the precursor solution to obtain carbon/graphene/Li2FeSiO4A precursor;
the molar ratio of silicon element in the ethyl orthosilicate to lithium element in the lithium salt is 1: 2;
step 4, preparing carbon/graphene/Li2FeSiO4A positive electrode material:
under reducing atmosphere, adding carbon/graphene/Li2FeSiO4Sintering the precursor at the temperature of 450-900 ℃ for 6-24 hours, and cooling the sintered sample along with the furnace to obtain the carbon/graphene/Li2FeSiO4A positive electrode material, the carbon/graphene/Li2FeSiO4The anode material is the anode material of the lithium ion battery for the vehicle;
the reducing atmosphere in the step 4 is formed by mixed gas of inert gas and reducing gas, the inert gas accounts for 90-99% of the mixed gas by volume, and the rest gas is the reducing gas; the inert gas is one or more of nitrogen and argon; the reducing gas is one or more of hydrogen and carbon monoxide.
2. The method for preparing the graphene-based positive electrode material for the lithium ion battery for the vehicle according to claim 1, wherein the lithium salt in the step 2 is one of anhydrous lithium hydroxide, lithium carbonate and lithium acetate.
3. The method for preparing the graphene-based positive electrode material for the lithium ion battery for the vehicle according to claim 1, wherein the iron salt in the step 2 is one of ferrous acetate, ferrous oxalate, ferrous citrate, ferric acetate, ferric oxalate and ferric citrate.
4. The preparation method of the graphene-based lithium ion battery cathode material for the vehicle according to claim 1, wherein the spray drying conditions in the step 3 are as follows: the temperature of the air inlet is 145-165 ℃, and the temperature of the air outlet is 90-110 ℃.
5. The graphene-based vehicle lithium ion battery cathode material prepared by the method of claim 1.
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