CN105958018A - Preparation method for vanadium-doped lithium titanate negative electrode material - Google Patents
Preparation method for vanadium-doped lithium titanate negative electrode material Download PDFInfo
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- CN105958018A CN105958018A CN201610306112.9A CN201610306112A CN105958018A CN 105958018 A CN105958018 A CN 105958018A CN 201610306112 A CN201610306112 A CN 201610306112A CN 105958018 A CN105958018 A CN 105958018A
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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
- H01M4/364—Composites as mixtures
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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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- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/626—Metals
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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 preparation method for a vanadium-doped lithium titanate negative electrode material. Titanium dioxide, a vanadium compound and a lithium compound water solution are mixed uniformly and subjected to a hydrothermal reaction at a temperature of 120 DEG C for 10h to obtain a precursor product; and the obtained precursor is dried and grinded, and then is subjected to heat treatment at a constant temperature of 650 DEG C for 4h to obtain the Li<4>Ti<5-x>V<x>O<12> material. The tap density of the Li<4>Ti<5-x>V<x>O<12> material prepared by the method reaches 1.35-1.8g/cm<3>; the material has an excellent electrochemical performance; the initial specific discharge capacity of the material reaches 171mAh/g under 0.2C current discharge; the average capacity attenuation rate in each cycle is less than 0.05%; the specific discharge capacity still can reach 145mAh/g under 10C rate; therefore, the vanadium-doped lithium titanate negative electrode material is an ideal negative electrode material of a high power lithium ion power battery; and in addition, the preparation method is simple, practical and low in cost and the vanadium-doped lithium titanate negative electrode material is suitable for industrialized production.
Description
Technical field
The invention belongs to lithium rechargeable battery Material Field, be specifically related to the lithium titanate anode material of a kind of vanadium that adulterates
Preparation method, can be as cathode material for lithium-ion power battery.
Background technology
Automobile industry is the pillar industry that national economy is important, is also the significant industry embodying national competitiveness.China
Become the first in the world automobile production and marketing state, the longest one period China's automobile volume of production and marketing also holding is quickly increased gesture
Head, it is contemplated that will reach 2.5 hundred million to the year two thousand twenty automobile pollution, by current automobile fuel ecomomy horizontal estimated, fuel oil for vehicles year
Consumption will break through 400,000,000 tons, and the energy security thus brought and environmental problem will be more prominent.Therefore, greatly develop energy-conservation with
New-energy automobile, accelerates the industrialization process of propulsion energy-saving and new-energy automobile, is to successfully manage the energy and environment challenge, it is achieved
The inevitable choice of Chinese Auto Industry sustainable development.Thus need to research and develop high-power, high-energy, long-life, height
Safety, low cost and eco-friendly electrokinetic cell.Lithium rechargeable battery have good cycle, energy density high,
The advantages such as voltage platform is high are it is considered to be most possibly used as the electrokinetic cell of electric automobile.The research of lithium-ion-power cell
Most important part in " 13 " Energy efficiency in planning and new-energy automobile major project with exploitation, become state key support and
Encourage the project of development, be also simultaneously the focus of whole world research and development, thus research and development high-performance, high security lithium from
Sub-electrokinetic cell is the most necessary.At present, the negative material of business-like lithium ion battery is mainly carbon negative pole material, but it is first
The characteristic that discharge and recharge irreversible capacity is higher, safety is low, cycle performance is poor, not being suitable for electric automobile etc. needs big electric current to fill
The equipment of electric discharge.It is long that lithium titanate has service life, and overcharging resisting is crossed and put the feature good with security performance, meets high-power discharge and recharge
Demand.
Pure spinelle Li4Ti5O12Electronics and the ionic conductivity of material are relatively low, and respectively 10-13 S·cm-1With 10-9~
10-13 cm2·s-1, therefore many researcheres adulterate vanadium to Li by conventional solid-state method4Ti5O12Improveing, the method is difficult to
Ensure that batch mixing is uniform, and resulting materials is more than under 800 DEG C of high temperature, could prepare more than 15 hours heat treatments, resulting materials electricity
Chemical property is poor.Therefore researchers are closed by methods such as sol-gel process, microemulsion method, solvent-thermal method, electrospray deposition
Become the material of containing transition metal lithium titanate.These methods can prepare the material of size tunable, but its complex steps, chemistry are anti-
Between Ying Shi longer and raw materials used environment is had pollution, be not easy to industrialized production.And by said method resulting materials
Particle diameter mostly is nanoscale, and the less energy density that result in battery of the tap density of nano material is relatively low, and nano material is bigger
Specific surface area make again reactivity higher, may result in material capacity in charge and discharge process and decline rapidly.China is specially
Profit CN 102328952 B reports a kind of method preparing spherical lithium titanate material, obtains pattern rule by the method
Spherical micron-sized lithium titanate material, but resulting materials battery capacity decay during high rate charge-discharge is very fast, due to
Resulting materials particle diameter is the least, and tap density is relatively low, is unfavorable for the raising of material energy densities.By patent CN 102328952
Method disclosed in B, it was predicted that use the TiO of big particle diameter2Raw material can obtain the lithium titanate material of big particle diameter, but due to lithium titanate self
Low conductivity cause Li under its big particle diameter+Can not quickly embed in positive electrode so that it is can not large-scale application.
Summary of the invention
The present invention is primarily to solve the pure low electronics of spinel lithium titanate material and low ionic conductivity, and passes through
The shortcoming that liquid phase method gained lithium titanate material particle diameter is less, complex steps, cost are high, it is provided that a kind of the most former by using
Material, the lithium titanate anode material of synthesizing blender vanadium under short period and lower temperature, chemical formula is Li4Ti5-xVxO12
(0.01≤x≤0.30), resulting materials has tap density height, specific discharge capacity height, high rate performance excellent characteristics.
For realizing above-mentioned technical purpose, the present invention is accomplished by:
A kind of preparation method of the lithium titanate anode material of the vanadium that adulterates, the lithium titanate material of doping vanadium prepared by the method be lithium from
Sub-secondary battery cathode material, containing v element in the Li4Ti5-xVxO12 material of synthesis, its content is 0.01 ~ 0.3 mol%.
The preparation method of the lithium titanate anode material of a kind of vanadium that adulterates, comprises the steps:
1) preparation lithium concentration is the lithium compound aqueous solution of 0.5 ~ 5 mol/L；
2) press thing mass ratio in Li4Ti5-xVxO12, take x=0.01 ~ 0.30, by titanium dioxide, vfanadium compound and lithium compound
Aqueous solution is uniform, in 120 DEG C of hydro-thermal reactions 10 hours, obtains precursor product；
3) gained presoma being dried and ground 30 ~ 90 minutes, then 650 DEG C of constant temp. heatings process 4 hours, obtain Li4Ti5-
XVxO12 material.
Further, high temperature products obtained therefrom is cooled down, pulverizes, sieves, obtain finished product doping vanadium lithium titanate material.
In above-mentioned preparation method, lithium salt compound described in step 1) is Lithium hydrate, lithium carbonate or lithium nitrate lithium compound
In one or more, preferably lithium nitrate.
Above-mentioned steps 2) described vfanadium compound is the one in ammonium metavanadate, vanadyl oxalate or vanadic anhydride compound,
The number of vanadium doping amount determines the size of resulting materials particle diameter, preferably ammonium metavanadate.
Above-mentioned steps 2) described titanium dioxide and lithium compound and vfanadium compound mixed material in the material of Li/ (V+Ti)
The ratio of amount be that 4:5 is preferable, the doping of vanadium be the doping of 0.01 ~ 0.3 mol%, preferably vanadium be 0.01 ~ 0.25 mol%,
The preferably doping of vanadium is 0.05 ~ 0.2 mol%, it is contemplated that the volatility of lithium compound under hot conditions, can suitably increase lithiumation
The consumption of compound but no more than 4 wt%, the consumption preferably increasing lithium compound is 2 ~ 3%.
Above-mentioned steps 3) atmosphere of high-temperature process is not particularly limited, can be air atmosphere or inert atmosphere, directly exist
In air, sintering enormously simplify process conditions.
The invention have the advantages that
1. utilize common raw material, through less step, it is not necessary to long-time high-temperature process can synthesize the lithium titanate of doping vanadium
Material.
2. the tap density of the Li4Ti5-xVxO12 material prepared by reaches 1.35 ~ 1.8g/cm3.This material is penetrated through X-
Line powder diffractometer (XRD) is detected as pure spinel structure, exists mutually without other non-spinelle impurity；Scanned ultramicroscope
(SEM) detection, the particle diameter of this Li4Ti5-xVxO12 material is gradually increased with the increase of vanadium doping amount, and tap density increases the most therewith
Greatly.
3. the Li4Ti5-xVxO12 material prepared by has excellent chemical property, including cycle performance and high magnification
Flash-over characteristic, is preferable high power lithium ion power battery negative material.Under 0.2C current discharge, discharge specific volume first
Amount is more than 170mAh/g, and average every circulation primary capacity attenuation rate is less than 0.5 ‰；Still have with 10C multiplying power discharging specific capacity
145mAh/g。
4. the present invention prepares the method simple practical of lithium titanate Li4Ti5-xVxO12 material of doping vanadium, and low cost is suitable
Close industrial-scale production.
Accompanying drawing explanation
Fig. 1 is embodiment 1(120 DEG C hydrothermal temperature) and 1(100 DEG C of hydrothermal temperature of comparative example) synthesize
The X-ray powder diagram of Li4Ti4.95V0.05O12 material.
Fig. 2 is embodiment 1(120 DEG C hydrothermal temperature) and 1(100 DEG C of hydrothermal temperature of comparative example) synthesize
The specific discharge capacity circulation figure of Li4Ti4.95V0.05O12 material.
Detailed description of the invention
Below by embodiment, technical scheme is further described in detail.
Embodiment 1
1. the synthesis of Li4Ti4.95V0.05O12 material
Compound concentration is the lithium hydroxide aqueous solution of 5 mol/L.39.5 grams of Detitanium-ore-type titanium dioxide are weighed according to stoichiometric proportion
Titanium and 0.585 gram of ammonium metavanadate are in hydrothermal reaction kettle, and the lithium hydroxide aqueous solution measuring 0.08 liter of preparation afterwards is anti-in hydro-thermal
Answer in still, be uniformly mixed in the baking oven being placed on 120 DEG C reaction 10 hours.Hydro-thermal reaction products therefrom is taken out, is dried
And transfer in alumina crucible.Being placed in Muffle furnace by crucible, be warming up to 650 DEG C with the speed of 6 DEG C/min, constant temperature 6 is little
Time, stop heating, in stove, naturally cool to room temperature, obtain Li4Ti4.95V0.05O12 material product.Test through XRD, show
Material is the product of single spinel structure, as shown in Figure 1；Observing through SEM, product particle smooth surface, densification, in spinelle
Type, the tap density of material is 1.35 g/cm3。
2. the chemical property of Li4Ti4.95V0.05O12 material
By the Li4Ti4.95V0.05O12 synthesized, acetylene black and electrically conductive graphite, binding agent polyvinylidene fluoride PVDF by quality
Than 90:4:6(wherein acetylene black and electrically conductive graphite and account for the 4% of total proportion) mix homogeneously, be coated on aluminium foil, dried cutting
Become pole piece.By electrolyte LiPF6The mixing that salt is dissolved in the ethylene carbonate (EC)/dimethyl carbonate (DMC) that volume ratio is 1:1 is molten
Liquid is formed the electrolyte that concentration is 1 mol/L, with lithium metal for electrode, assembles in the vacuum glove box of full argon
Become R2032 button cell, carry out electrochemical property test.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity reaches 171mAh/g, and average every circulation primary capacity attenuation rate is less than 0.5 ‰；With 10C multiplying power discharging specific capacity
Still having 145mAh/g, electrochemical property test the results are shown in Table 1.
Embodiment 2
1. the synthesis of Li4Ti4.9V0.1O12 material
Compound concentration is the lithium hydroxide aqueous solution of 5 mol/L.39.1 grams of Detitanium-ore-type titanium dioxide are weighed according to stoichiometric proportion
Titanium and 1.17 grams of ammonium metavanadates, in hydrothermal reaction kettle, measure the lithium hydroxide aqueous solution of 0.08 liter of preparation afterwards in hydro-thermal reaction
In still, it is uniformly mixed in the baking oven being placed on 120 DEG C reaction 10 hours.Hydro-thermal reaction products therefrom is taken out, is dried also
Transfer in alumina crucible.Crucible is placed in Muffle furnace, is warming up to 650 DEG C with the speed of 6 DEG C/min, constant temperature 6 hours,
Stop heating, in stove, naturally cool to room temperature, obtain Li4Ti4.9V0.1O12 material product.Test through XRD, show material
Product for single spinel structure；Observing through SEM, product particle smooth surface, densification, in spinel-type；The jolt ramming of material
Density is 1.5 g/cm3。
2. the chemical property of Li4Ti4.9V0.1O12 material
According to the condition assembled battery that embodiment 1 is identical.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity is 165mAh/g, and average every circulation primary capacity attenuation rate, less than 0.8 ‰, with 10C multiplying power discharging specific capacity is
142mAh/g。
Embodiment 3
1. the synthesis of Li4Ti4.85V0.15O12 material
Compound concentration is the lithium hydroxide aqueous solution of 5 mol/L.38.7 grams of Detitanium-ore-type titanium dioxide are weighed according to stoichiometric proportion
Titanium and 1.75 grams of ammonium metavanadates, in hydrothermal reaction kettle, measure the lithium hydroxide aqueous solution of 0.08 liter of preparation afterwards in hydro-thermal reaction
In still, it is uniformly mixed in the baking oven being placed on 120 DEG C reaction 10 hours.Hydro-thermal reaction products therefrom is taken out, is dried also
Transfer in alumina crucible.Crucible is placed in Muffle furnace, is warming up to 650 DEG C with the speed of 6 DEG C/min, constant temperature 6 hours,
Stop heating, in stove, naturally cool to room temperature, obtain Li4Ti4.85V0.15O12 material product.Test through XRD, show material
Material is the product of single spinel structure, and the tap density of material is 1.63 g/cm3。
2. the chemical property of Li4Ti4.85V0.15O12 material
According to the condition assembled battery that embodiment 1 is identical.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity is 149mAh/g, and average every circulation primary capacity attenuation rate, less than 1 ‰, with 10C multiplying power discharging specific capacity is
122mAh/g。
Embodiment 4
1. the synthesis of Li4Ti4.8V0.2O12 material
Compound concentration is the lithium hydroxide aqueous solution of 5 mol/L.38.3 grams of Detitanium-ore-type titanium dioxide are weighed according to stoichiometric proportion
Titanium and 2.34 grams of ammonium metavanadates, in hydrothermal reaction kettle, measure the lithium hydroxide aqueous solution of 0.08 liter of preparation afterwards in hydro-thermal reaction
In still, it is uniformly mixed in the baking oven being placed on 120 DEG C reaction 10 hours.Hydro-thermal reaction products therefrom is taken out, is dried also
Transfer in alumina crucible.Crucible is placed in Muffle furnace, is warming up to 650 DEG C with the speed of 6 DEG C/min, constant temperature 6 hours,
Stop heating, in stove, naturally cool to room temperature, obtain Li4Ti4.8V0.2O12 material product.Test through XRD, show material
For the product of single spinel structure, the tap density of material is 1.8 g/cm3。
2. the chemical property of Li4Ti4.8V0.2O12 material
According to the condition assembled battery that embodiment 1 is identical.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity is 138mAh/g, and average every circulation primary capacity attenuation rate, less than 1 ‰, with 10C multiplying power discharging specific capacity is
113mAh/g。
Comparative example 1
1. the synthesis of Li4Ti4.95V0.05O12 material
Substitute the heat treatment time of 120 DEG C with the hydrothermal temperatures of 100 DEG C, other condition is same as in Example 1.Survey through XRD
Examination, shows that material is containing V2O5The Li4Ti4.95V0.05O12 material of the single spinel structure of impurity phase, the jolt ramming of material
Density is 1.3g/cm3。
2. the chemical property of Li4Ti4.95V0.05O12 material
According to the condition assembled battery that embodiment 1 is identical.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity is 145mAh/g, and average every circulation primary capacity attenuation rate is less than 1%.
Comparative example 2
1. the synthesis of Li4Ti4.95V0.05O12 material
Substitute the heat treatment temperature of 650 DEG C with the heat treatment temperatures of 800 DEG C, other condition is same as in Example 1.Survey through XRD
Examination, shows that material is containing V2O5And TiO2The Li4Ti4.95V0.05O12 of the spinel structure of impurity phase, the vibration density of material
Degree is 1.2 g/cm3。
2. the chemical property of Li4Ti4.95V0.05O12 material
According to the condition assembled battery that embodiment 1 is identical.Charging/discharging voltage is 1.0 ~ 2.5V, under 0.2C current discharge, first
Specific discharge capacity is 140mAh/g, and average every circulation primary capacity attenuation rate is about 2%.
Claims (8)
1. the lithium titanate anode material preparation method of the vanadium that adulterates, it is characterised in that in the Li4Ti5-xVxO12 material of synthesis
It is 0.01 ~ 0.3 mol% that vanadium contains.
The lithium titanate anode material preparation method of a kind of vanadium that adulterates the most as claimed in claim 1, comprises the steps:
Preparation lithium concentration is the lithium compound aqueous solution of 0.5 ~ 5 mol/L；
By thing mass ratio in Li4Ti5-xVxO12, take x=0.01 ~ 0.3, by titanium dioxide, vfanadium compound and lithium compound water
Solution mix homogeneously, in 120 DEG C of hydro-thermal reactions 10 hours, obtains precursor product；
Being dried by gained presoma and ball milling 30 ~ 90 minutes, then 650 DEG C of high-temperature heat treatment 4 hours, obtain Li4Ti5-
XVxO12 material.
3. preparation method as claimed in claim 2, it is characterised in that lithium compound described in step 1) is inorganic lithium compound,
One or more mixing in Lithium hydrate, lithium carbonate or lithium nitrate lithium compound.
4. preparation method as claimed in claim 2, it is characterised in that step 2) described vfanadium compound is ammonium metavanadate, oxalic acid
One in vanadyl or vanadic anhydride vfanadium compound, the number of vanadium doping amount determines the size of resulting materials particle diameter.
5. preparation method as claimed in claim 2, it is characterised in that step 2) described titanium dioxide, lithium compound and vanadium
In the mixed material of compound, the ratio of the amount of the material of Li/ (V+Ti) is 4:5, and the doping of vanadium is 0.01 ~ 0.3 mol%, can be suitable
Increase lithium compound consumption but no more than 4 wt%, the consumption preferably increasing lithium compound is 2 ~ 3%.
6. preparation method as claimed in claim 2, it is characterised in that the doping of described vanadium is 0.05 ~ 0.25 mol%；Examine
Consider to the volatility of lithium compound under hot conditions, can suitably increase the consumption of lithium compound but no more than 4 wt%, preferably increase
The consumption adding lithium compound is 2 ~ 3%.
7. preparation method as claimed in claim 2, it is characterised in that the doping of described vanadium is 0.1 ~ 0.2 mol%, it is considered to
The volatility of lithium compound under hot conditions, can suitably increase the consumption of lithium compound but no more than 4 wt%, preferably increase
The consumption of lithium compound is 2 ~ 3%.
8. preparation method as claimed in claim 2, it is characterised in that in step 3), high-temperature heat treatment is carried out in atmosphere.
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Cited By (3)
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| CN110323433A (en) * | 2019-07-10 | 2019-10-11 | 银隆新能源股份有限公司 | A kind of lithium titanate composite material and preparation method thereof, lithium ion battery and preparation method thereof |
| CN110323436A (en) * | 2019-07-11 | 2019-10-11 | 银隆新能源股份有限公司 | The electrode slice and preparation method thereof and lithium ion battery of lithium titanate composite material and preparation method thereof, lithium ion battery |
| CN110459750A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of cathode material of lithium-ion power battery and preparation method thereof |
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| CN110323436A (en) * | 2019-07-11 | 2019-10-11 | 银隆新能源股份有限公司 | The electrode slice and preparation method thereof and lithium ion battery of lithium titanate composite material and preparation method thereof, lithium ion battery |
| CN110323436B (en) * | 2019-07-11 | 2023-04-11 | 银隆新能源股份有限公司 | Lithium titanate composite material and preparation method thereof, electrode plate of lithium ion battery and preparation method thereof, and lithium ion battery |
| CN110459750A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of cathode material of lithium-ion power battery and preparation method thereof |
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Application publication date: 20160921 |