CN107394192A - A kind of hollow micron spherical lithium titanate cathode material and preparation method thereof - Google Patents
A kind of hollow micron spherical lithium titanate cathode material and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of hollow micron spherical lithium titanate cathode material and preparation method, the hollow micron spherical lithium titanate cathode material, i.e. metal oxide is coated on lithium titanate anode material surface and formed, and wherein the amount of metal oxide and lithium titanate anode material calculates the metal in i.e. metal oxide in mass ratio：Lithium titanate anode material is 0.2 5：100.Its preparation method calculates in mass ratio, lithium titanate：Metal dust：Dispersant is 1：0.002‑0.05：0.01 10 ratio uniformly dries lithium titanate, metal dust and dispersant afterwards, after obtained presoma is warming up to 300 700 DEG C and the 10h of constant temperature 2 under the conditions of air or oxygen with 2 10 DEG C/min speed, room temperature is naturally cooled to, produces specific capacity and the excellent hollow micron spherical lithium titanate cathode material of fast charging and discharging performance.
Description
Technical field
The invention belongs to technical field of lithium ion battery electrode, more particularly to a kind of hollow micron spherical lithium titanate
Negative material and preparation method thereof.
Background technology
Lithium ion battery has energy density height, operating voltage height, long-life, memory-less effect and advantages of environment protection
It is applied to the field such as mobile communication, notebook computer, camera, portable instrument, and various countries are studied energetically
The preferred supporting power supply of electric automobile, space power system, turn into the first choice of fungible energy source.
And advanced electrode material turns into the core technology that current lithium ion battery updates.The lithium of commercialization at present from
Sub- cell negative electrode material uses various carbon materials mostly, but carbon material has the following disadvantages：The current potential of carbon material and lithium metal
Current potential is very close to when over-charging of battery, lithium metal may separate out in carbon electrodes and form Li dendrite, so as to cause short circuit；
First charge-discharge efficiency is low；Reacted with electrolyte；In the presence of obvious voltage delay.Compared with Carbon anode, lithium titanate conduct
Lithium ion battery negative material has obvious advantage：There is the lattice constant in charge and discharge process hardly to change for it
Characteristic, repeated charge crystal structure are less likely to occur to change, and cycle performance is excellent；Its intercalation potential height (1.55VvsLi/Li
+), the precipitation for causing lithium metal is not easy, anti-over-charging performance is good；Lithium ion diffusion coefficient (2 × 10-8cm2/s) is higher than Carbon anode by one
The individual order of magnitude.Become the lithium ion battery negative material of new generation of most development and application potentiality.
But the poorly conductive (intrinsic conductivity 10-9S/cm) of prior art lithium titanate material, fast charging and discharging performance is not
It can bring into play well, it is therefore desirable to material is optimized, improves its chemical property.International ceramic magazine
(Ceramics International) 39 (2013) 2695-2698, for raw material, passes through water with LiOHH2O and Ti (OC4H9) 4
Hot method has synthesized Li4Ti5O12 microballoons, and specific capacity of the material under 1C multiplying powers is 152.7mAh/g, the specific capacity under 5C multiplying powers
For 122mAh/g.The product purity height of hydro-thermal method preparation, uniformity is good, heat treatment temperature is relatively low, but the method is generally with organic carbon
Source is raw material, and production cost is high, is not easy to industrial production.
Battery magazine 5 (2011) 243-246 passes through two step Solid phase synthesis using Li2CO3, TiO2 and activated carbon as raw material
Activated carbon modified spinel lithium titanate, the activated carbon of addition inhibit the growth of particle, and the material is in 2C multiplying powers, specific volume
Measure as 134.7mAh/g, during 5C multiplying powers, specific capacity 103.5mAh/g.Method preparation technology is simple, and production cost is relatively low, is easy to
Industrialized production is realized, but the electrochemistry of material can meet the needs of commercialization.
The content of the invention
An object of the present invention is to solve the poorly conductive of above-mentioned lithium titanate material and fast charging and discharging performance
The technical problems such as difference and a kind of hollow micron spherical lithium titanate cathode material is provided, the hollow micron spherical lithium titanate cathode material
Electrochemical performance.
The second object of the present invention is to provide a kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material,
The preparation method has production cost low, and preparation process is simple, be suitable for industrial scale production etc. the characteristics of.
Technical scheme
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide are coated on the surface of lithium titanate anode material
And formed, calculate in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 0.2-5:100,
Described metal oxide is Cun1Om1, Fen2Om2, Crn3Om3, Con4Om4 or Nin5Om5；
M1 in described Cun1Om1:N1 value is 1-2；
M2 in described Fen2Om2:N2 value is 0.66-1；
M3 in described Crn3Om3:N3 value is 0.66-1；
M4 in described Con4Om4:N4 value is 0.66-1；
M5 in described Nin5Om5:N5 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.002-0.05：0.01-10 ratio
Example, lithium titanate, metal dust and dispersant is uniform, then dry, obtain presoma；
Described dispersant is water, polyethylene glycol, methanol, ethanol, acetone, ethoxylated dodecyl alcohol, triton x-100
One or both of composition described above mixture, preferably ethanol, acetone, ethoxylated dodecyl alcohol or triton x-100；
(2), the presoma obtained by step (1) is warming up under air or oxygen atmospheric condition with 2-10 DEG C/min speed
After 300-700 DEG C and constant temperature 2-10h, room temperature is naturally cooled to, produces hollow micron spherical lithium titanate cathode material.
Beneficial effects of the present invention
The mistake of a kind of hollow micron spherical lithium titanate cathode material of the present invention, metal dust and lithium titanate material in mixing
Cheng Zhong, the presence of metal dust advantageously reduce lithium titanate particle degree and effectively suppress the reunion between lithium titanate particle, be advantageous to
The performance of lithium titanate anode material chemical property.
Further, a kind of hollow micron spherical lithium titanate cathode material of the invention, because metal dust is in high-temperature process
The metal oxide generated afterwards is also common lithium ion battery negative material, and its specific capacity is more than the specific capacity of lithium titanate,
When hollow micron spherical lithium titanate cathode material carries out discharge and recharge ,-engaged column lithium can also be taken off, improves its discharge and recharge specific volume
Amount, experience is several times after recharge-discharge activation process, and the excellent electron electric conductivity for the mixed valence metal oxide being stabilized is more
The defects of having mended lithium titanate anode material electron conduction difference.
Further, a kind of hollow micron spherical lithium titanate cathode material of the invention, due to raw material Cu, Fe used, Cr,
The metal oxide sources such as Co, Ni enrich, and preparation technology is simple, therefore, a kind of hollow spherical metatitanic acid of micron of the invention
The preparation method of lithium titanate cathode material has production cost low, and preparation process is simple, the features such as being suitable for industrial-scale production.
Brief description of the drawings
The SEM figures of pure phase lithium titanate anode material used in Fig. 1 a, embodiment 1；
Fig. 1 b, the gained of embodiment 1 hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Crn3Om3 claddings
The SEM figures of negative material；
The spherical lithium titanate anode of hollow micron of pure phase lithium titanate material and the gained of embodiment 1 used in Fig. 2, embodiment 1
The Li4Ti5O12 negative materials of material, i.e. Crn3Om3 cladding, the cycle performance curve under different multiplying；
The spherical lithium titanate anode of hollow micron of pure phase lithium titanate material and the gained of embodiment 1 used in Fig. 3, embodiment 1
The Li4Ti5O12 negative materials of material, i.e. Crn3Om3 cladding, the first charge-discharge curve map under 2C multiplying powers.
Embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not intended to limit the present invention.
Electrochemical property test：
By pure phase lithium titanate and the hollow micron spherical lithium titanate cathode material synthesized using the inventive method respectively with leading
Electrical carbon is black and binding agent polyvinylidene fluoride (PVDF) in mass ratio 80:10:10 is well mixed, is coated on copper foil, is cut out after drying
Electrode slice is cut into, 24h is dried in vacuo in 100 DEG C.
Using lithium metal as to electrode；
Electrolyte LiPF6 salt is dissolved in mass ratio as 1：1：1 ethylene carbonate (EC)/dimethyl carbonate (DMC)/carbon
The concentration that LiPF6 salt is formed in the mixed solution of sour methyl ethyl ester (EMC) is 1mol/L electrolyte；
Button cell is assembled into argon gas glove box.
Electrochemical property test is carried out using the blue electric CT2001A types cell tester in Wuhan, charging/discharging voltage scope is
1.0V-2.5V(vs.Li+/Li)。
Embodiment 1
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 0.2:100；
Described metal oxide is Crn3Om3；
M3 in described Crn3Om3:N3 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.002：0.01 ratio, by 1g titaniums
The aqueous dispersant that sour lithium, 0.002g chromium metal dust and 1ml concentration are 1% is well mixed, and is dried, is obtained presoma；
Described dispersant is ethoxylated dodecyl alcohol；
(2) presoma obtained by step (1), is warming up to 700 DEG C and constant temperature with 2 DEG C/min speed in air atmosphere
2h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, produced hollow micron spherical lithium titanate and bear
The Li4Ti5O12 negative materials of pole material, i.e. Crn3Om3 cladding.
Above-mentioned raw material lithium titanate used is that pure phase lithium titanate anode material is scanned by Japanese JEOL companies SU-1500 types
Electron microscope (SEM) is observed its surface topography under 20KV, and the SEM figures of gained as shown in Figure 1a, can from Fig. 1 a
To find out that pure phase lithium titanate particle is larger, there is certain reunion in size from 200nm to 1um；
The hollow micron spherical lithium titanate cathode material of the gained of above-described embodiment 1, the i.e. Li4Ti5O12 of Crn3Om3 claddings
The SEM figures of negative material as shown in Figure 1 b, can be seen that Li4Ti5O12 negative materials by metal oxide from Fig. 1 b
After Crn3Om3 claddings, particle diameter diminishes, and particle size distribution tends to uniform, and the size of particle is between 100-300nm.Further
By Fig. 1 a and Fig. 1 b contrast, also show hollow micron spherical lithium titanate cathode material can effectively suppress lithium titanate anode
The reunion of material, increase the dispersiveness of lithium titanate anode material.
Raw material lithium titanate used in above-described embodiment 1 is the hollow micro- of pure phase lithium titanate anode material and the gained of embodiment 1
Rice spherical lithium titanate cathode material, i.e. the Li4Ti5O12 negative materials of Crn3Om3 claddings, the cycle performance under different multiplying
As shown in Figure 2, Li4Ti5O12 is pure phase lithium titanate anode material to curve in Fig. 2, and Crn3Om3 claddings Li4Ti5O12 is embodiment
The hollow micron spherical lithium titanate cathode material of 1 gained, the i.e. Li4Ti5O12 negative materials of Crn3Om3 claddings, can from Fig. 2
To find out the first discharge specific capacity of pure phase lithium titanate anode material as 164.3mAh/g, during 2C multiplying powers, specific discharge capacity is
Specific discharge capacity is 59.5mAh/g when 98.7mAh/g, 5C multiplying power, and the Li4Ti5O12 negative materials of Crn3Om3 claddings are first
Specific discharge capacity is 182.2mAh/g, and during 2C multiplying powers, specific discharge capacity is during specific discharge capacity 150.5mAh/g, 5C multiplying power
140.6mAh/g, be indicated above the hollow micron spherical lithium titanate cathode material of the gained of embodiment 1, i.e. Crn3Om3 claddings
The specific capacity performance and fast charging and discharging performance of Li4Ti5O12 negative materials have obtained obvious improvement.
Raw material lithium titanate used in above-described embodiment 1 is the hollow micro- of pure phase lithium titanate anode material and the gained of embodiment 1
Rice spherical lithium titanate cathode material, i.e. the Li4Ti5O12 negative materials of Crn3Om3 claddings, the first charge-discharge under 2C multiplying powers
For curve map as shown in figure 3, Li4Ti5O12 is pure phase lithium titanate anode material in Fig. 3, Crn3Om3 cladding Li4Ti5O12 are implementation
The hollow micron spherical lithium titanate cathode material of the gained of example 1, i.e. the Li4Ti5O12 negative materials of Crn3Om3 claddings, from Fig. 3
It can be seen that under 2C multiplying powers, the charging platform of pure phase lithium titanate anode material is left in 1.48V in 1.62V or so, discharge platform
The right side, the charging platform of the Li4Ti5O12 negative materials of voltage difference 0.14V, Crn3Om3 cladding is in 1.59V or so, discharge platform
In 1.52V or so, voltage difference 0.07V, after being indicated above Crn3Om3 claddings, Li4Ti5O12 voltage difference is obviously reduced,
Polarization phenomena are smaller, i.e. the hollow micron spherical lithium titanate cathode material of the gained of embodiment 1, i.e. Crn3Om3 claddings
The electronic conductivity of Li4Ti5O12 negative materials is improved.
Embodiment 2
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 1:100；
Described metal oxide is Crn3Om3, wherein m3:N3 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.01：0.05 ratio, by 1g metatitanic acids
The aqueous dispersant that lithium, 0.01g chromium metal dust and 5ml concentration are 1% is well mixed, and is dried, is obtained presoma；
Described dispersant is ethoxylated dodecyl alcohol；
(2) presoma obtained by step (1), is warming up to 700 DEG C and constant temperature under oxygen atmosphere with 10 DEG C/min speed
10h, then naturally cool to room temperature, produce hollow micron spherical lithium titanate cathode material, i.e. Crn3Om3 claddings
Li4Ti5O12 negative materials.
Embodiment 3
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 2:100；
Described metal oxide is Fen2Om2；
M2 in described Fen2Om2:N2 value is 0.66-1；
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.02：0.08 ratio, by 1g metatitanic acids
The aqueous dispersant that lithium, 0.02g iron metal powders and 8ml concentration are 1% is well mixed, and is dried, is obtained presoma；
Described dispersant is triton x-100；
(2) presoma obtained by step (1), is warming up to 300 DEG C and constant temperature with 5 DEG C/min speed in air atmosphere
2h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Fen2Om2 claddings
Negative material.
Embodiment 4
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 5:100；
Described metal oxide is Fen2Om2；
M3 in described Fen2Om2:N3 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.05：0.8 ratio, by 1g metatitanic acids
Lithium, 0.05g iron metal powders and 1ml dispersants are uniform, drying, obtain presoma；
Described dispersant is acetone；
(2) presoma obtained by step (1), is warming up to 400 DEG C and constant temperature under oxygen atmosphere with 3 DEG C/min speed
2h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Fen2Om2 claddings
Negative material.
Embodiment 5
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 1.5:100；
Described metal oxide is Con4Om4；
M4 in described Con4Om4:N4 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.015：4 ratio, by 1g metatitanic acids
Lithium, 0.015g cobalt metal powders and 5ml dispersants are uniform, drying, obtain presoma；
Described dispersant is ethanol；
(2) presoma obtained by step (1), is warming up to 500 DEG C and constant temperature with 2 DEG C/min speed in air atmosphere
6h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Con4Om4 claddings
Negative material.
Embodiment 6
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 2:100；
Described metal oxide is Con4Om4；
M4 in described Con4Om4:N4 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.02：10 ratio, by 1g metatitanic acids
Lithium, 0.02g cobalt metal powders and 12.5ml dispersants are uniform, drying, obtain presoma；
Described dispersant is ethanol；
(2) presoma obtained by step (1), is warming up to 600 DEG C and constant temperature under oxygen atmosphere with 6 DEG C/min speed
10h, then naturally cool to room temperature, produce hollow micron spherical lithium titanate cathode material, i.e. Con4Om4 claddings
Li4Ti5O12 negative materials.
Embodiment 7
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 4:100；
Described metal oxide is Cun1Om1；
M1 in described Cun1Om1:N1 value is 1-2.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.04：1.6 ratio, by 1g metatitanic acids
Lithium, 0.04g copper metals powder and 2ml dispersants are uniform, drying, obtain presoma；
Described dispersant is acetone；
(2) presoma obtained by step (1), is warming up to 500 DEG C and constant temperature under oxygen atmosphere with 6 DEG C/min speed
2h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Cun1Om1 claddings
Negative material.
Embodiment 8
A kind of hollow micron spherical lithium titanate cathode material, i.e. metal oxide be coated on lithium titanate anode material surface and
Formed, calculated in mass ratio, the quality of the metal in metal oxide：Lithium titanate anode material is 2:100；
Described metal oxide is Nin5Om5；
M5 in described Nin5Om5:N5 value is 0.66-1.
A kind of preparation method of above-mentioned hollow micron spherical lithium titanate cathode material, specifically comprises the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.02：0.15 ratio, by 1g metatitanic acids
The aqueous dispersant that lithium, 0.02g nickel metal powders and 15ml concentration are 1% is well mixed, and is dried, is obtained presoma；
Described dispersant is ethoxylated dodecyl alcohol；
(2) presoma obtained by step (1), is warming up to 700 DEG C and constant temperature under oxygen atmosphere with 8 DEG C/min speed
6h, room temperature is then naturally cooled to, produce hollow micron spherical lithium titanate cathode material, the i.e. Li4Ti5O12 of Nin5Om5 claddings
Negative material.
In summary, obtained by a kind of preparation method of the lithium titanate anode material of metal oxide coating modification of the invention
Metal oxide coat lithium titanate anode material compared with pure phase lithium titanate material, its specific capacity performance and fast charging and discharging
Obvious improvement can be obtained, and its preparation technology is simple, the characteristics of being suitable for industrial-scale production.
Above said content is only the basic explanation under present inventive concept, and is appointed according to what technical scheme was done
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (1)
1. a kind of preparation method of hollow micron spherical lithium titanate cathode material, the spherical lithium titanate anode material of described hollow micron
Material, i.e., metal oxide is coated on lithium titanate anode material surface and formed, described metal oxide be Cun1Om1,
Fen2Om2, Crn3Om3, Con4Om4 or Nin5Om5；
M1 in described Cun1Om1:N1 value is 1-2；
M2 in described Fen2Om2:N2 value is 0.66-1；
M3 in described Crn3Om3:N3 value is 0.66-1；
M4 in described Con4Om4:N4 value is 0.66-1；
M5 in described Nin5Om5:N5 value is 0.66-1；
The amount of metal oxide and lithium titanate anode material is in mass ratio in described hollow micron spherical lithium titanate cathode material
Calculate, i.e. metal in metal oxide：Lithium titanate anode material is 0.2-5：100；
It is characterized in that specifically comprise the following steps：
(1), calculate in mass ratio, i.e. lithium titanate：Metal dust：Dispersant is 1：0.002-0.05：0.01-10 ratio, will
Lithium titanate, metal dust and dispersant are uniform, then dry, and obtain presoma；
Described dispersant is in water, polyethylene glycol, methanol, ethanol, acetone, ethoxylated dodecyl alcohol, triton x-100
The mixture of one or more composition；
(2) presoma obtained by step (1), is warming up to 300- under air or oxygen atmospheric condition with 2-10 DEG C/min speed
After 700 DEG C and constant temperature 2-10h, room temperature is naturally cooled to, produces hollow micron spherical lithium titanate cathode material.
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| CN104109218A (en) * | 2013-04-22 | 2014-10-22 | 昭和电工株式会社 | (meth)acrylate-based polymer, composition comprising same and use thereof |
| CN104733699A (en) * | 2015-03-20 | 2015-06-24 | 常州大学 | Method for preparing molybdenum dioxide coated lithium titanate negative electrode material |
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| CN104109218A (en) * | 2013-04-22 | 2014-10-22 | 昭和电工株式会社 | (meth)acrylate-based polymer, composition comprising same and use thereof |
| CN103337616A (en) * | 2013-06-28 | 2013-10-02 | 上海电力学院 | Metal oxide coated lithium titanate negative pole material and preparation method thereof |
| CN104733699A (en) * | 2015-03-20 | 2015-06-24 | 常州大学 | Method for preparing molybdenum dioxide coated lithium titanate negative electrode material |
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