CN109860573A - A kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof - Google Patents
A kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof, the following steps are included: configuration PVP glue, lithium salts, molysite, the mixed solution of the ethanol solution of graphene oxide dispersion and ethyl orthosilicate, spray drying mixed liquor obtains presoma, sintered precursor.It is of the invention by Li2FeSiO4The control and graphene, the building of carbonaceous conductive network for generating granular size enhance the electric conductivity of material, reduce lithium ion diffusion length, reduce polarization, improve high rate performance, the present invention is also by Li2FeSiO4Coated with carbon material and graphene are effectively reduced the generation of side reaction, improve the cycle performance of material, and the security performance of material is excellent.
Description
Technical field
The present invention relates to lithium ion battery material preparation technical fields, and in particular to a kind of graphene-based automobile-used lithium ion
Cell positive material and preparation method thereof.
Background technique
Global climate change, artificial greenhouse gases release and be continuously increased energy demand be when forward swing in face of the mankind most
For urgent problem, these problems are mainly as caused by the huge consumption of fossil fuel (mainly coal, petroleum, natural gas).
Therefore, energy diversification and the development of renewable green energy resource are irresistible, in all kinds of technologies of field of renewable energy
In, energy stores and switch technology, especially electrochemical energy storage become most prospect, develop one of field the most quick.
Lithium ion battery is as one of secondary cell the most outstanding in current electrochemical energy storage, due to possessing very high energy
Amount and power density, become electric tool, electronic mobile device, and the energy stores such as pure electric vehicle and hybrid vehicle are best
Selection.And electrode material is the key that determine performance of lithium ion battery, for negative electrode material and electrolyte system, decades with
The research come all obtains the specific capacity of no small progress, especially negative electrode material, and security and stability and cycle performance have all reached
To higher level, but raising of the people to lithium ion battery various aspects demand is faced, the research of positive electrode but relatively lags behind.
Although the tertiary cathode material and nickelic positive electrode capacity propagated its belief on a large scale currently on the market are higher, it also has
There is capacity under (1) high temperature cyclic performance and high temperature to keep poor；(2) material is nickeliferous higher, and materials synthesis has harshness to atmosphere
Requirement and atmospheric environment under store and be easy water suction and rotten, synthesis is difficult；(3) compacted density is relatively low and charging process
The disadvantages of gas of generation causes battery security to be deteriorated.For electric car, other than with suitable capacity, electricity
The high rate performance and security performance in pond are very crucial, and one kind is needed to have macroion electron conduction at present, high thermal stability
Anode material for lithium-ion batteries.
Recent years because novel polyanion silicic acid lithium salts positive electrode can effective reversibly embedding lithium ionic insertion/deinsertion,
Chemical property is more excellent, and constructing relatively stronger Si-O key keeps the thermal stability of material more excellent, widely causes
The research and development interest of people；Wherein Li2FeSiO4By the concern of researcher, because of the content difference of Si and Fe in the earth's crust
Second and the 4th are accounted for, raw material is laid in naturally to be enriched, and theoretical capacity is higher, and cyclical stability is preferable, and thermal stability is good, there is very much hair
Exhibition prospect.But Li2FeSiO4Former circle capacity attenuation speed are fast, and the conductivity of material itself and lithium ion diffusion coefficient compared with
It is low.Still lack for Li at present2FeSiO4The preferable modified scheme of poorly conductive and poor circulation.
The present invention is by graphene and PVP (polyvinylpyrrolidone) to Li2FeSiO4The size of generation particle carry out
Limitation, reduces the path of lithium ion transport, improves the lithium ion transport speed of material；The preparation method realizes
Li2FeSiO4Little particle being uniformly distributed in graphene/carbon conductive network, makes it have preferable electric conductivity；And graphene/
The cladding of carbon also prevents electrolyte and contacts with the direct of anode material for lithium-ion batteries, it is suppressed that anode material for lithium-ion batteries
Reacting between electrolyte makes it have more excellent cycle performance；The structural stability of material itself also makes it have
The more excellent security performance of lithium ion battery material more automobile-used than tradition.
Summary of the invention
The present invention provides a kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof, solve existing
There is in technology/Li2FeSiO4Conductivity and lithium ion diffusion coefficient are lower, the problem that safety is poor, cycle performance is bad.
The first purpose of the invention is to provide a kind of graphene-based automobile-used anode material for lithium-ion batteries and its preparation
Method, comprising the following steps:
Step 1, PVP glue is configured:
It is stirred 0.5-2 hours after PVP, deionized water are mixed according to the ratio that weight ratio is 1:10-100, is configured to PVP
Glue；
Step 2, graphene oxide mixed solution is prepared:
By lithium salts, molysite according to elemental lithium: after the ratio mixing that ferro element molar ratio is 2:1, obtaining salt-mixture, will mix
Salt and water are uniformly mixed according to the ratio that weight ratio is 1:10-50, obtain mixing salt solution；By mixing salt solution and PVP glue
It is stirred 1-6 hours after mixing, is then charged with graphene oxide dispersion, stirring obtained graphene oxide after 1-6 hours
Mixed solution；
Wherein, the weight ratio of graphene oxide and lithium salts is 0.5-1:1 in graphene oxide dispersion；
The weight ratio of the PVP and lithium salts is 1-15:1；
Step 3, carbon graphite alkene/Li is prepared2FeSiO4Presoma:
Configuration concentration is the ethanol solution of the ethyl orthosilicate of 0.01-1g/mL；Then by the ethanol solution of ethyl orthosilicate
It mixes, and stirs 1-3 hours with graphene oxide mixed solution obtained in step 2, obtain carbon graphite alkene/Li2FeSiO4Before
Drive liquid solution；By carbon graphite alkene/Li2FeSiO4Precursor solution spray drying, obtains carbon graphite alkene/Li2FeSiO4Forerunner
Body；
Elemental lithium molar ratio is 1:2 in element silicon and the lithium salts in the ethyl orthosilicate；
Step 4, carbon graphite alkene/Li is prepared2FeSiO4Positive electrode:
Under reducing atmosphere, by carbon graphite alkene/Li2FeSiO4Presoma 450-900 DEG C sintering 6-24 hours, sintering
Sample furnace cooling afterwards to get arrive the carbon graphite alkene/Li2FeSiO4Positive electrode, the carbon graphite alkene/Li2FeSiO4
Positive electrode is automobile-used anode material for lithium-ion batteries.
Preferably, the lithium salts in the step 2 is anhydrous lithium hydroxide, lithium carbonate, one of lithium acetate.
Preferably, the molysite in the step 2 is ferrous acetate, ferrous oxalate, ferrous citrate, ferric acetate, five water plants
One of sour iron, ironic citrate.
Preferably, the atmosphere in the step 4 is formed by the mixed gas of inert gas and reducibility gas, inert gas
The volume ratio for accounting for mixed gas is 90%-99%, and remaining gas is reducibility gas；Inert gas is one in nitrogen and argon gas
Kind is a variety of；Reducibility gas is one of hydrogen and carbon monoxide or a variety of.
Preferably, spray drying condition in the step 3 are as follows: intake air temperature is 145-165 DEG C, and air outlet temperature is
90-110℃。
A second object of the present invention is to provide a kind of carbon graphite alkene/Li prepared according to the above method2FeSiO4Just
Pole material.
Compared with prior art, the beneficial effects of the present invention are:
1) by the way that Li is formed in situ in PVP solution and graphene oxide solution in the present invention2FeSiO4, can be effective
Limit Li2FeSiO4The size of particles generation.The size of control material granule is equivalent in smaller range effectively shortens lithium ion
The path of diffusion, while the utilization rate of particle peripheral activity substance can be also improved, the present invention is effective by reducing particle size
Improve the chemical property of material.
2) organic assembling for passing through PVP and graphene in the present invention, forms in the positive electrode ultimately generated with stone
Black alkene is skeleton, wraps up little particle Li2FeSiO4, and the multistage conductive network filled with carbon material, further improve material
Conductivity reduces polarization, improves the high rate performance of material.
3) pelletizing has been carried out for presoma by the method being spray-dried in the present invention, has not only been easy production, Er Qieqiu
The tap density of shape particle is higher, can greatly promote the volume energy density of full battery.
4) since the stability of material itself, material have excellent security performance, battery entirety is greatly promoted
Safety.
5) by Li2FeSiO4Coated with carbon material and graphene are effectively reduced the generation of side reaction, are promoted
The cycle performance of material.
Detailed description of the invention
Fig. 1 is carbon graphite alkene/Li of the embodiment of the present invention 12FeSiO4Scanning electron microscope (SEM) under 50,000 times of positive electrode
Figure；
Fig. 2 is carbon graphite alkene/Li of the embodiment of the present invention 12FeSiO4Scanning electron microscope under 100,000 times of positive electrode；
Fig. 3 is carbon graphite alkene/Li of the embodiment of the present invention 22FeSiO4Scanning electron microscope (SEM) photograph under 50,000 times of positive electrode；
Fig. 4 is carbon graphite alkene/Li of the embodiment of the present invention 22FeSiO4Scanning electron microscope (SEM) photograph under 100,000 times of positive electrode；
Fig. 5 is carbon graphite alkene/Li of Example 1 and Example 2 of the present invention2FeSiO4The XRD diagram of positive electrode, wherein a
For carbon graphite alkene/Li of embodiment 12FeSiO4The XRD diagram of positive electrode；B is carbon graphite alkene/Li of embodiment 22FeSiO4
The XRD diagram of positive electrode；
Carbon graphite alkene/Li of Fig. 6 embodiment of the present invention 12FeSiO4The cycle performance figure of positive electrode；
Carbon graphite alkene/Li of Fig. 7 embodiment of the present invention 22FeSiO4The cycle performance figure of positive electrode.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method and detection method described in following each embodiments are unless otherwise specified conventional method；The examination
Agent and material can be commercially available on the market unless otherwise specified, wherein graphene oxide dispersion purchase used is certainly
Changzhou No.6 Element Material Technology Co., Ltd., model SE3521；Spray dryer used is bought from Shanghai Qiao Feng
Industrial Co., Ltd., model QFN-8000ST.
Embodiment 1
A kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof, comprising the following steps:
Step 1, PVP solution is configured:
20gPVP is stirred PVP glue 1 hour after the mixing of 250g deionized water, is configured to PVP glue；
Step 2, graphene oxide mixed solution is prepared:
After 2g lithium carbonate, 4.7g ferrous acetate are mixed, the water of 70g is added, configures mixing salt solution；By mixing salt solution
It is stirred 3 hours after being mixed with 270g PVP glue, is then charged with 60g graphene oxide dispersion (3wt.%),
Stirring obtained graphene oxide mixed solution after 3 hours；
Step 3, carbon graphite alkene/Li is prepared2FeSiO4Presoma:
The ethyl orthosilicate of 6g is dissolved into 13ml ethyl alcohol, the ethanol solution of ethyl orthosilicate is configured；Then by positive silicon
The ethanol solution of acetoacetic ester is mixed with graphene oxide mixed solution obtained in step 2, and is stirred 2 hours, and carbon graphite is obtained
Alkene/Li2FeSiO4Precursor solution；By carbon graphite alkene/Li2FeSiO4Precursor solution is spray-dried, and presoma is obtained.
The intake air temperature of the spray drying is 150 DEG C, and air outlet temperature is 95 DEG C；
Elemental lithium molar ratio is 1:2 in element silicon and lithium carbonate in ethyl orthosilicate；
Step 4, sintered precursor:
In the case where the volume ratio of nitrogen and hydrogen is the mixed atmosphere of 95:5, it is sintered 12 hours at 650 DEG C, sintered sample
Furnace cooling to get arrive the carbon graphite alkene/Li2FeSiO4Positive electrode.
Embodiment 2
A kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof, comprising the following steps:
Step 1, PVP solution is configured:
60gPVP is stirred PVP glue 0.5 hour after the mixing of 600g deionized water, is configured to PVP glue；
Step 2, graphene oxide mixed solution is prepared:
After 60g anhydrous lithium hydroxide, five water ferric oxalate of 292g are mixed, the water of 3520g is added, configures mixing salt solution；
It is stirred 1 hour after mixing salt solution is mixed with 660g PVP glue, is then charged with 1000g graphene oxide point
Dispersion liquid (3wt.%), stirring obtained graphene oxide mixed solution after 1 hour；
Step 3, carbon graphite alkene/Li is prepared2FeSiO4Presoma:
The ethyl orthosilicate of 1044g is dissolved into 104400ml ethyl alcohol, the ethanol solution of ethyl orthosilicate is configured；Then
The ethanol solution of ethyl orthosilicate is mixed with graphene oxide mixed solution obtained in step 2, and is stirred 1 hour, is obtained
Carbon graphite alkene/Li2FeSiO4Precursor solution；By carbon graphite alkene/Li2FeSiO4Precursor solution is spray-dried, and is obtained
Presoma.The intake air temperature of the spray drying is 145 DEG C, and air outlet temperature is 90 DEG C；
Elemental lithium molar ratio is 1:2 in element silicon and anhydrous lithium hydroxide in ethyl orthosilicate；
Step 4, sintered precursor:
In the case where the volume ratio of argon gas and hydrogen is the mixed atmosphere of 90:10, it is sintered 6 hours at 450 DEG C, sintered sample
Furnace cooling to get arrive the carbon graphite alkene/Li2FeSiO4Positive electrode.
Embodiment 3
A kind of graphene-based automobile-used anode material for lithium-ion batteries and preparation method thereof, comprising the following steps:
Step 1, PVP solution is configured:
15gPVP is stirred PVP glue 2 hours after the mixing of 1500g deionized water, is configured to PVP glue；
Step 2, graphene oxide mixed solution is prepared:
After 1g anhydrous lithium hydroxide, 3g ferrous oxalate are mixed, the water of 200g is added, configures mixing salt solution；It will mixing
Salting liquid stirs 6 hours after being mixed with 1515g PVP glue, is then charged with 33g graphene oxide dispersion
(3wt.%), stirring obtained graphene oxide mixed solution after 6 hours；
Step 3, carbon graphite alkene/Li is prepared2FeSiO4Presoma:
The ethyl orthosilicate of 17g is dissolved into 17ml ethyl alcohol, the ethanol solution of ethyl orthosilicate is configured；Then by positive silicon
The ethanol solution of acetoacetic ester is mixed with graphene oxide mixed solution obtained in step 2, and is stirred 3 hours, and carbon graphite is obtained
Alkene/Li2FeSiO4Precursor solution；By carbon graphite alkene/Li2FeSiO4Precursor solution is spray-dried, and presoma is obtained.
The intake air temperature of the spray drying is 165 DEG C, and air outlet temperature is 110 DEG C；
Elemental lithium molar ratio is 1:2 in element silicon and the anhydrous lithium hydroxide in ethyl orthosilicate；
Step 4, sintered precursor:
In the case where the volume ratio of nitrogen and hydrogen is the mixed atmosphere of 99:1, it is sintered 24 hours at 900 DEG C, sintered sample
Furnace cooling to get arrive the carbon graphite alkene/Li2FeSiO4Positive electrode.
Carbon graphite alkene/Li that 1-3 of the embodiment of the present invention is prepared2FeSiO4Positive electrode is detected and is characterized, tool
Body experimental result is as follows:
1, SEM map analysis
Using scanning electron microscope to the above-mentioned each carbon graphite alkene/Li prepared2FeSiO4The pattern of positive electrode into
Row characterization, specific SEM figure are shown in Fig. 1-Fig. 4, and wherein Fig. 1 is the carbon graphite alkene/Li prepared in embodiment 12FeSiO4Anode
SEM figure of the material under 50,000 times, Fig. 2 is the carbon graphite alkene/Li prepared in the embodiment of the present application 12FeSiO4Positive electrode exists
SEM figure under 100000 times.From Fig. 1-2 as can be seen that carbon graphite alkene/Li that the embodiment of the present application 1 is prepared2FeSiO4Positive material
Material is mainly micron-size spherical particles, Li2FeSiO4Particle size it is smaller, and well wrapped up by graphene and carbon, it was demonstrated that the material
Material has good conductive property and the path of shorter lithium ion diffusion.
Fig. 3 is the carbon graphite alkene/Li prepared in embodiment 22FeSiO4SEM figure of the positive electrode under 50,000 times, Fig. 4
For the carbon graphite alkene/Li prepared in the embodiment of the present application 22FeSiO4SEM figure of the positive electrode under 100,000 times.From Fig. 3-4
As can be seen that carbon graphite alkene/Li that the embodiment of the present application 2 is prepared2FeSiO4Pattern and shape in positive electrode and embodiment 1
State is similar, is micron-size spherical particles, Li2FeSiO4Particle size it is smaller, and well wrapped up by graphene and carbon, it was demonstrated that
The material has good conductive property and the path of shorter lithium ion diffusion.
2, XRD diagram is analyzed
It is carbon graphite alkene/Li in embodiment 1-2 in Fig. 52FeSiO4The XRD diagram of positive electrode, wherein curve a is to implement
Carbon graphite alkene/Li in example 12FeSiO4The XRD diagram of positive electrode, curve b be embodiment 2 in carbon graphite alkene/
Li2FeSiO4The XRD diagram of positive electrode.From in Fig. 5 a and b can be found that in embodiment 1-2 that synthetic sample is in angle
Occur feature derivative peak at 16.68 °, 24.29 °, 28.47 °, 33.07 °, 35.67 °, 37.67 °, 48.25 ° and 59.83 °, and spreads out
It is more sharp to penetrate peak, intensity is preferable, illustrates that composite construction strengthens Li2FeSiO4Crystallinity.It is not found in XRD spectrum
The characteristic peak of carbon, it may be possible to because carbon material is predominantly unformed.
3, chemical property is analyzed
For the carbon graphite alkene/Li for examining 1-3 of the embodiment of the present invention to prepare2FeSiO4Positive electrode properties ginseng
Number, has been assembled into half-cell for positive electrode and has tested.Half-cell is using metal lithium sheet as cathode, with the present embodiment carbon graphite
Alkene/Li2FeSiO4Positive electrode is anode, assembles button cell in the glove box full of argon gas and strict control water oxygen index.
Carbon graphite alkene/Li in embodiment 12FeSiO4Positive electrode is under 1.5-4.8V voltage, 0.1C charge and discharge, for the first time
Reversible specific capacity is 135.6mAh g-1, 5C charge and discharge, putting a capacity for the first time is 126.3mAh g-1, material after 50 circulations
Capacity is 123.3mAh g-1, capacity retention ratio 97.62%.Fig. 6 is carbon graphite alkene/Li in embodiment 12FeSiO4Positive material
The cycle performance figure of material, cycle performance are preferable.
Carbon graphite alkene/Li in embodiment 22FeSiO4Positive electrode is under 1.5-4.8V voltage, 0.1C charge and discharge, for the first time
Reversible specific capacity is 134.2mAh g-1, 5C charge and discharge, putting a capacity for the first time is 99.7mAh g-1, 50 times circulation after material appearance
Amount is 98.6mAh g-1, capacity retention ratio 98.90%.Fig. 7 is carbon graphite alkene/Li in embodiment 22FeSiO4Positive electrode
Cycle performance figure, cycle performance is preferable.
From performance as can be seen that the carbon graphite alkene/Li2FeSiO4Positive electrode not only reversible capacity with higher, and
And under the big multiplying power of 5C, there are higher reversible capacity and preferable cycle performance, clad has completely cut off positive electrode and electrolysis
Contact between liquid reduces the generation of side reaction, improves the chemical property of material, and the building of conductive network also makes
Obtaining material has lesser polarization.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within be also intended to include these modifications and variations.
Claims (6)
1. a kind of preparation method of graphene-based automobile-used anode material for lithium-ion batteries, which comprises the following steps:
Step 1, PVP glue is configured
It is stirred 0.5-2 hours after PVP, deionized water are mixed according to the ratio that weight ratio is 1:10-100, is configured to PVP glue
Liquid；
Step 2, graphene oxide mixed solution is prepared
By lithium salts, molysite according to elemental lithium: ferro element molar ratio be 2:1 ratio mixing after, obtain salt-mixture, by salt-mixture with
Water is uniformly mixed according to the ratio that weight ratio is 1:10-50, obtains mixing salt solution；Mixing salt solution is mixed with PVP glue
It stirs 1-6 hours afterwards, is then charged with graphene oxide dispersion, stirring obtains graphene oxide mixing after 1-6 hours
Solution；
Wherein, the weight ratio of graphene oxide and lithium salts is 0.5-1:1 in graphene oxide dispersion；
The weight ratio of the PVP and lithium salts is 1-15:1；
Step 3, carbon graphite alkene/Li is prepared2FeSiO4Presoma
Configuration concentration is the ethanol solution of the ethyl orthosilicate of 0.01-1g/mL；Then by the ethanol solution of ethyl orthosilicate and step
The mixing of graphene oxide mixed solution obtained in rapid 2, and stir 1-3 hours, obtain carbon graphite alkene/Li2FeSiO4Presoma
Solution；By carbon graphite alkene/Li2FeSiO4Precursor solution spray drying, obtains carbon graphite alkene/Li2FeSiO4Presoma；
Elemental lithium molar ratio is 1:2 in element silicon and the lithium salts in the ethyl orthosilicate；
Step 4, carbon graphite alkene/Li is prepared2FeSiO4Positive electrode:
Under reducing atmosphere, by carbon graphite alkene/Li2FeSiO4Presoma 450-900 DEG C sintering 6-24 hours, it is sintered
Sample furnace cooling to get arrive the carbon graphite alkene/Li2FeSiO4Positive electrode, the carbon graphite alkene/Li2FeSiO4Anode
Material is automobile-used anode material for lithium-ion batteries.
2. the preparation method of graphene-based automobile-used anode material for lithium-ion batteries according to claim 1, feature exist
In the lithium salts in the step 2 is anhydrous lithium hydroxide, lithium carbonate, one of lithium acetate.
3. the preparation method of graphene-based automobile-used anode material for lithium-ion batteries according to claim 1, feature exist
In the molysite in the step 2 is ferrous acetate, in ferrous oxalate, ferrous citrate, ferric acetate, ferric oxalate, ironic citrate
It is a kind of.
4. the preparation method of graphene-based automobile-used anode material for lithium-ion batteries according to claim 1, feature exist
In the reducing atmosphere in the step 4 is formed by the mixed gas of inert gas and reducibility gas, and inert gas accounts for mixing
The volume ratio of gas is 90%-99%, and remaining gas is reducibility gas；Inert gas is one of nitrogen and argon gas or more
Kind；Reducibility gas is one of hydrogen and carbon monoxide or a variety of.
5. the preparation method of graphene-based automobile-used anode material for lithium-ion batteries according to claim 1, feature exist
In spray drying condition in the step 3 are as follows: intake air temperature is 145-165 DEG C, and air outlet temperature is 90-110 DEG C.
6. the graphene-based automobile-used anode material for lithium-ion batteries that one kind is prepared method according to claim 1.
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| CN112510198A (en) * | 2020-12-16 | 2021-03-16 | 武汉大学 | Positive electrode active material, aqueous solution sodium ion battery and electronic device |
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