CN106450173A - Graphene oxide/lithium titanate composite negative electrode material for lithium-ion battery and preparation method of graphene oxide/lithium titanate composite negative electrode material - Google Patents
Graphene oxide/lithium titanate composite negative electrode material for lithium-ion battery and preparation method of graphene oxide/lithium titanate composite negative electrode material Download PDFInfo
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- CN106450173A CN106450173A CN201510487263.4A CN201510487263A CN106450173A CN 106450173 A CN106450173 A CN 106450173A CN 201510487263 A CN201510487263 A CN 201510487263A CN 106450173 A CN106450173 A CN 106450173A
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- lithium titanate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a graphene oxide/lithium titanate composite negative electrode material for a lithium-ion battery and a preparation method of the graphene oxide/lithium titanate composite negative electrode material. The composite negative electrode material is formed by compounding graphene oxide and lithium titanate; and the mass percentage of the graphene oxide is 1%-90% and the mass percentage of the lithium titanate is 10%-99%. The preparation method of the composite negative electrode material comprises the steps of slowly dropwise adding graphene oxide sol or a graphene oxide dispersion liquid to a suspension liquid of the lithium titanate, and achieving homogeneous compounding of the graphene oxide and the lithium titanate under the help of agitation or ultrasonic dispersion to obtain slurry of the graphene oxide composite negative electrode material. The slurry can directly coat to form an electrode slice after a conductive agent is added; and an adhesive is not needed. The composite negative electrode material disclosed by the invention has relatively high reversible specific capacity, cycle stability and excellent rate charge-discharge property.
Description
Technical field
The invention belongs to field of lithium ion battery, it is related to a kind of lithium ion battery negative material and preparation method thereof.
Background technology
As green high-capacity battery of new generation, lithium ion battery has that weight is little, energy density is high, has extended cycle life, work
Make the advantages such as voltage height, memory-less effect, non-environmental-pollution, be widely used to mobile phone, notebook computer, video camera etc.
In portable electric appts, it is also following electric automobile and the preferred electrical source of power of mixed type electric automobile, has wide
Application prospect.
Negative material is one of key components of lithium ion battery.Spinel type lithium titanate (Li4Ti5O12) because of tool
Good safety and cyclical stability is had to be expected to become the negative material of lithium-ion-power cell of new generation.But
Li4Ti5O12Electron conduction is poor, and when working under big multiplying power (high current) environment, capacity attenuation is rapid, seriously cuts
The weak energy density of battery and power density are it is impossible to the lasting high current meeting required by large-sized power battery is put
Electric energy power etc., therefore, the modification of lithium titanate, lithium titanate and other negative materials are compounded to form composite, are lithium titanates
The development trend of negative material.
Nanometer carbon material, due to having the micro structure of uniqueness, can be conducive to carrying by unique mechanism mass storage lithium ion
The charge/discharge capacity of high-lithium ion battery, cycle life and electric current density, thus become lithium ion battery negative material of new generation
Study hotspot.In recent years, the appearance of Graphene causes global research boom.Graphene is tight by monolayer carbon atom
The carbonaceous new material with two-dimension plane structure that closs packing becomes, is to build zero dimension fullerene, one-dimensional CNT, three-dimensional stone
The basic structural unit of ink.Graphene is not only the thinnest one kind (theoretic throat only has 0.35nm) in known materials, also gathers around
There is very high intensity (110GPa), and theoretical specific surface area is up to 2630m2/g.The unique atomic structure of Graphene gives it
The excellent properties of the aspects such as electricity, calorifics, mechanics, are with a wide range of applications in numerous areas.Graphene oxide is not only
Have the construction featuress of Graphene, and there is substantial amounts of oxygen-containing functional group, the hydrosol of high concentration can be formed, and and titanium
The other types of negative material such as sour lithium has the good compatibility.Compared with expensive Graphene, graphene oxide is cheap,
Raw material is easy to get, and preparation method is simple, and graphene oxide colloidal sol can play the effect of bonding agent, such that it is able to and metatitanic acid
The Material claddings such as lithium prepare the self-supporting electrode of adhesive-free.
Existing result of study (ShiY, Wen L, Li F, Cheng HM, Nanosized Li at present4Ti5O12/graphene
Hybrid materials with low polarization for high rate lithium ion batteries, J.Power Sources 2011,
196(20)：8610-8617) show, graphene/lithium titanate complex as lithium ion battery negative material, specific capacity under its 1C
Can reach 175mAh/g, its 20C specific capacity still has 130mAh/g, illustrate that graphene/lithium titanate composite negative pole has preferably
High rate performance.But, Graphene is due to its larger theoretical specific surface area (2630m2/ g), form solid electrolyte interface
A large amount of lithium ions can be consumed, simultaneously big specific surface area also makes it be easy to reunite, is difficult to after Lithium-ion embeding during film
Abjection, specific capacity significantly declines, and more disadvantageously Graphene does not have caking property, also needs during as composite negative pole material
Want 10% binding agent, such electrode active material only accounts for the 80% of electrode gross mass.
Content of the invention
The purpose of the present invention be develop a kind of there is more height ratio capacity have the lithium ion battery of high rate capability lithium titanate concurrently be combined
Negative material.
The object of the invention is realized by following process：Lithium titanate and graphene oxide are combined to prepare lithium titanate/graphene oxide multiple
Close negative material, using the substantial amounts of oxy radical of surface of graphene oxide carry out that reversible lithium storage improves composite negative pole material can
Inverse specific capacity, improves composite negative pole using the high connductivity characteristic after graphene oxide local conductive characteristic and electrochemical reduction
The high-rate charge-discharge capability of material.The present invention is by stirring the suspension of lithium titanate and graphene oxide dispersion or colloidal sol
Mix compound, prepare the composite cathode material for lithium ion cell without binding agent with height ratio capacity and high rate capability.
Graphene oxide colloidal sol used in the present invention or graphene oxide dispersion are made by the steps：With natural height
Pure crystalline flake graphite is raw material, using potassium permanganate and concentrated sulphuric acid as oxidant, successively after low, medium and high temperature reaction,
Add hydrogen peroxide, then with appropriate dilute hydrochloric acid and deionized water centrifuge washing, finally obtain graphene oxide colloidal sol.Take a small amount of
Colloidal sol add deionized water, ultrasonic after obtain graphene oxide dispersion.
Lithium titanate suspension used in the present invention is made by the steps：Add a certain amount of water or organic in a reservoir
Solvent, adds the lithium titanate of amount of calculation, fully dispersed after stirring, and obtains lithium titanate suspension.
Prepared graphene oxide-lithium titanate composite anode material in the present invention, wherein graphene oxide and the quality of lithium titanate
Percentage composition is than for 1-90%: 10-99%.
Lithium titanate used in the present invention is commercialization lithium titanate, modified lithium titanate and their derivant and its mixture.
Lithium titanate used in the present invention can be a diameter of 50-500 nanometer, 500-700 nanometer, 700-1000 nanometer, 1-5
Micron and the lithium titanate more than 5 microns.
Lithium titanate used in the present invention, its pattern is general spherical shape granule, spherical particle, bar-shaped or nanometer wire.
Graphene oxide prepared by the present invention is the graphene oxide of monolayer and the multilamellar graphene oxide of 2-10 layer, its powder
Body specific insulation is more than 103Ω .cm, oxygen content 10-50%.
Compared with the class graphene lithium ion battery composite negative pole material of document report, the maximum difference of the present invention is to employ
Nonconducting graphene oxide as compound substance, has only just obtained answering of graphene oxide and lithium titanate by simple step
Close negative material, and do not use any bonding agent in the process preparing electrode slice, the graphene oxide colloidal sol being added can
To play bonding effect, and obtain the electrode slice of self-supporting.Composite negative pole material prepared by the present invention is in different electric current densities
Under carry out charge and discharge cycles test, show excellent chemical property, after multiple charge and discharge cycles, still be able to protect
Hold higher specific capacity and efficiency.This negative material preparation process is simply easily operated, and raw material is cheap and easy to get, has industrialization to answer
Value.
Brief description
Fig. 1 is transmission electron microscope (TEM) photo of graphene oxide dispersion.
Fig. 2 is scanning electron microscope (SEM) photo of the lithium titanate anode material in embodiment 1.
Fig. 3 is scanning electron microscope (SEM) photo of the graphene oxide/lithium titanate composite anode material in embodiment 1.
Fig. 4 is transmission electron microscope (TEM) photo of the graphene oxide/lithium titanate composite anode material in embodiment 1.
Fig. 5 is composite negative pole material graphene oxide (GO) and lithium titanate (LTO) in embodiment 1, in different electric currents
The high rate performance comparison diagram of (1C, 2C, 5C, 10C, 20C, 1C) under density.
Fig. 6 is composite negative pole material graphene oxide (GO) and lithium titanate (LTO) in embodiment 2, in different electric currents
The high rate performance comparison diagram of (1C, 2C, 5C, 10C, 20C, 1C) under density.
Fig. 7 is composite negative pole material graphene oxide (GO) in embodiment 2 and lithium titanate (LTO) is close in 1C electric current
The cycle performance figure that the lower discharge and recharge of degree is 1300 times.
Fig. 8 is composite negative pole material in embodiment 3 under different electric current densities (1C, 2C, 5C, 10C, 20C, 1C)
High rate performance comparison diagram.
Fig. 9 is composite negative pole material graphene oxide (GO) and lithium titanate (LTO) in embodiment 4, in different electric currents
The high rate performance comparison diagram of (1C, 2C, 5C, 10C, 20C, 1C) under density.
Figure 10 is composite negative pole material graphene oxide (GO) and lithium titanate (LTO) in embodiment 5, in different electric currents
The high rate performance comparison diagram of (1C, 2C, 5C, 10C, 20C, 1C) under density.
Specific embodiment
The following is embodiments of the invention, and the invention is not limited in embodiment.
Embodiment 1
Weigh 5.0 grams of graphene oxide colloidal sols (as shown in Figure 1), its solid content is 1.71%, adds 50 ml deionized water,
Graphene oxide dispersion is obtained standby after ultrasonic.Weigh 0.425 gram of a diameter of 300 nanometers of lithium titanate powdery (as Fig. 2
Shown), add 50 milliliters of dehydrated alcohol, ultrasonic after to obtain lithium titanate suspension standby.Lithium titanate suspension is slowly added to
(instead add effect identical) in graphene oxide dispersion, constantly with magneton stirring during Deca, move it into reactor afterwards
In, at 70 DEG C, oil bath heating is evaporated 2 hours, makes most of ethanol and moisture evaporation, obtains graphene oxide/lithium titanate multiple
Close the slurry (as shown in Figure 3, Figure 4) of negative material, wherein graphene oxide and the weight/mass percentage composition ratio of lithium titanate is
17%: 83%.
The preparation of electrode and its test：
The preparation of electrode be by above-mentioned slurry by composite negative pole material and conductive black 9: 1 quality than mix homogeneously, in mortar
Homogeneous paste is made in middle grinding, is coated on 12 microns of thick bright Copper Foils as collector, after moisture evaporation is complete,
Roll electrode slice with roll squeezer, then be punched into the electrode slice of required diameter, in 105 DEG C of dryings 12 hours in vacuum drying oven,
After removing contained micro-moisture in electrode slice, it is transferred quickly in glove box.It is to electrode, Celgard 2400 with lithium metal
For barrier film, electrolyte is the 1mol/1LiPF containing 2%VC (vinylene carbonate)6, solvent is EC/DMC/EMC (body
Long-pending ratio is 1: 1: 1), assemble CR2032 type button cell.Respectively test electrode high rate performance (electric current density be 1C, 5C,
10C and 20C, wherein 1C are equal to 200mAh/g) and cycle performance (electric current density is 1C), test voltage scope is
0.6～3.0V or 0.8～3.0V.
The high rate performance of composite as shown in figure 5, under the electric current density of 1C graphene oxide/lithium titanate composite negative pole material
The embedding first lithium specific capacity of material, lithium titanate and graphene oxide is respectively：190th, 155 and 90mAh/g.Graphene oxide/
Lithium titanate composite anode material shows obvious advantage.Additionally, under the high current of 20C, graphene oxide/lithium titanate
Composite negative pole material still maintains the de- lithium specific capacity of 115mAh/g, and has preferable stability.Have passed through 1C, 5C,
After charge and discharge cycles test under 10C and 20C electric current density, again return to the electric current density of 1C, graphene oxide/titanium
The de- lithium specific capacity of sour lithium composite negative pole material still is able to return to initial value, embodies good structural stability.
Embodiment 2
The weight/mass percentage composition ratio of graphene oxide and lithium titanate is adjusted to 12%: 88%, other steps are with embodiment 1.Knot
Fruit as shown in fig. 6, when the weight/mass percentage composition ratio of graphene oxide and lithium titanate is from 17%: 83%, after being adjusted to 12%: 88%,
The specific capacity of embedding and removing first of composite negative pole material has all risen.And, have passed through 1C, 2C, 5C, 10C
After the charge and discharge cycles test under 20C electric current density, after again returning to the electric current density of 1C, answering in the present embodiment
Closing negative material still has the de- lithium specific capacity of 194mAh/g (12%: 88%) (graphene oxide consumption reduces, but compound
Negative material specific capacity does not have reduction), illustrate that in embodiment 1, graphene oxide does not play a role completely.
In embodiment 2, the charge-discharge performance of composite negative pole material is as shown in fig. 7, under the electric current density of 1C, graphite oxide
It is 190mAh/g that alkene/lithium titanate composite anode material circulates the de- lithium specific capacity after 1400 times, and specific capacity conservation rate is up to 96%
More than.
Embodiment 3
The weight/mass percentage composition ratio of graphene oxide and lithium titanate is adjusted to 9%: 91%, other steps are with embodiment 1.Result
As shown in figure 8, when the graphene oxide amount used by when composite negative pole material gradually decreases, the embedding first lithium of composite negative pole material
It is significantly improved with de- lithium specific capacity.The lamella that this is possibly due to graphene oxide easily stacks, and when equivalent is many, aoxidizes stone
It is stacked between black alkene lamella, be unfavorable for Lithium-ion embeding and abjection.But, when graphene oxide consumption reduces, LTO
Graphene oxide fully can be strutted, provide wider " passage " to lithium ion, easily deviate from after making Lithium-ion embeding, because
And it is higher to take off lithium specific capacity.
Embodiment 4
The weight/mass percentage composition ratio of graphene oxide and lithium titanate is adjusted to 5%: 95%, other steps are with embodiment 1.Result
As shown in figure 9, have passed through 1C, 5C, 10C and 20C charge and discharge cycles, after again returning to the electric current density of 1C, answer
The de- lithium specific capacity closing negative material still have 185mAh/g hence it is evident that higher than simple lithium titanate (155mAh/g) with simple
The capacity of graphene oxide (90mAh/g) even their superposition sum.
Embodiment 5
The weight/mass percentage composition ratio of graphene oxide and lithium titanate is adjusted to 3%: 97%, other steps are with embodiment 1.Result
As shown in Figure 10, its de- lithium specific capacity is significantly lower than the composite negative pole material in embodiment 4, but is above pure lithium titanate and oxygen
Graphite alkene.Illustrate that the appropriate interpolation of graphene oxide can provide more storage lithium spaces, significantly improve composite negative pole material
De- lithium specific capacity.
Claims (10)
1. a kind of lithium ion battery graphene/lithium titanate composite anode material, be composited by Graphene and lithium titanate it is characterised in that
Described Graphene is graphene oxide, and it is 10～50% that X- photoelectron spectroscopy tests its oxygen content.
2. composite negative pole material according to claim 1 is it is characterised in that described composite negative pole material is without using bonding agent, its
Slurry can be directly coated with into electrode slice.
3. composite negative pole material according to claim 1 is it is characterised in that in described composite negative pole material, graphene oxide with
The mass content percentage ratio of lithium titanate is 1-90%：10-99%.
4. composite negative pole material according to claim 1 it is characterised in that described graphene oxide be single-layer graphene oxide or
The multilamellar graphene oxide of person's 2-10 layer, and its powder body specific insulation is more than 103Ω·cm.
5. composite negative pole material according to claim 1 is it is characterised in that described lithium titanate is commercialization lithium titanate or modification
Lithium titanate and their derivant and its mixture afterwards.
6. composite negative pole material according to claim 5 is it is characterised in that described its powder body specific insulation of graphene oxide is big
In 103Ω·cm.
7. composite negative pole material according to claim 6 is it is characterised in that the pattern of described lithium titanate is general spherical shape granule, class
Spheroidal particle, bar-shaped or nanometer wire.
8. a kind of preparation method of composite negative pole material described in claim 1 is it is characterised in that comprise the following steps：1. use chemical oxidation
Method prepares graphene oxide colloidal sol or graphene oxide dispersion；2. the lithium titanate of amount of calculation is added in water or organic solvent
Fully dispersed, obtain lithium titanate suspension；3. the graphene oxide colloidal sol of amount of calculation or graphene oxide dispersion are slowly added to
To in lithium titanate suspension, also can instead add, stir or ultrasonic disperse is uniform；4. heating removes part moisture and organic molten
Agent, obtains graphene oxide/lithium titanate composite negative pole slurry.
9. preparation method according to claim 8 it is characterised in that described organic solvent be methanol, ethanol, benzene, chlorobenzene,
Or acetone.
10. preparation method according to claim 8 is it is characterised in that described dispersion is by the ultrasonic device with ultrasonic probe
Realize.
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Application publication date: 20170222 |