CN110459750B - Negative electrode material of lithium ion power battery and preparation method thereof - Google Patents
Negative electrode material of lithium ion power battery and preparation method thereof Download PDFInfo
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Abstract
The invention provides a lithium ion power battery cathode material and a preparation method thereof, wherein the method adopts a sol-gel method to prepare V and Cr co-doped lithium titanate, the doping is Ti ion 16d doped, and then spray drying method is adopted to granulate again, thus effectively improving the initial capacity, the circulation stability and the tap density of the lithium titanate.
Description
Technical Field
The invention relates to the technical field of lithium ion power battery negative electrode materials, in particular to a lithium ion power battery co-doped lithium titanate negative electrode material and a preparation method thereof.
Background
The lithium ion power battery has the advantages of long cycle life, high energy density and the like, is widely applied to the field of new energy automobiles, but the problems of weak endurance, poor safety and the like at present are always the technical direction of important research in the field of new energy.
Spinel lithium titanate is used as a negative electrode material of great interest, which has the following advantages: 1) Almost zero strain of lithium titanate before and after lithium intercalation; 2) The lithium intercalation potential is higher (1.55V), the generation of lithium dendrite can be effectively avoided, and the safety is higher; 3) Having a very flat voltage platform; 4) The chemical diffusion coefficient and the coulombic efficiency are high.
The 8a tetrahedral void occupied by lithium ions and the 16d octahedral void occupied by titanium ions exist in the spinel lithium titanate structure, when doping ions are selected, the doping ions which enter the occupied ion sites preferentially are generally considered, and if the doping ions enter the 16d octahedral void, the structure of the spinel is more favorable for stabilizing, so that the capacity and the cycle performance of the electrode material can be improved; if the lithium ions enter the 8a space, the lithium ions are extruded to 16d position, so that an inverse spinel structure is formed, and the capacity and the cycle performance of the obtained electrode material are reduced to different degrees.
Therefore, aiming at the defects of the prior art, the invention is based on improving the electrochemical performance of lithium titanate, and V and Cr elements are co-doped in the lithium titanate, so that the elements can enter the 16d position of Ti ions more easily, and the initial capacity and the cycle stability of the lithium titanate are effectively improved.
Disclosure of Invention
The invention provides a lithium ion power battery negative electrode material and a preparation method thereof, wherein the method adopts a sol-gel method to prepare co-doped lithium titanate, and then adopts a spray drying method to granulate again, thereby effectively improving the initial capacity and the cycling stability of the lithium titanate.
In order to achieve the above purpose, the invention provides a negative electrode material of a lithium ion power battery, wherein the negative electrode material is double-element co-doped lithium titanate, the double elements are transition metal elements, and the doping is Ti-site doping.
Further, the chemical structural formula is as follows: li (Li) 4 Ti 5-x-y V x Cr y O 12 Wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.3.
Further, the structural formula of the anode material is preferably Li 4 Ti 4.7 V 0.2 Cr 0.1 O 12 。
Further, the tap density of the anode material is 1.0-2.0g/cm 3 The average particle size is 50-800nm.
The invention also provides a preparation method of the lithium ion power battery anode material, which comprises the following steps:
a. weighing a certain amount of titanium source according to the molar ratio of n (Li) to n (Ti) to n (V) to n (Cr) =4 to (5-x-y) to x to y, dispersing in a solvent, and uniformly stirring and mixing to obtain a solution A; weighing a certain amount of lithium source, dissolving the lithium source in a solvent, and uniformly stirring to obtain a solution B; weighing a certain amount of vanadium source, dispersing the vanadium source in a solvent, and stirring and mixing uniformly to obtain a solution C; weighing a certain amount of chromium source, dispersing the chromium source in a solvent, and stirring and mixing the chromium source uniformly to obtain solution D, wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.3;
b. slowly adding the solution B into the solution A under the stirring action, then simultaneously adding the solutions C and D to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining at 400-600 ℃ under the protection atmosphere, keeping the temperature for 2-5h, then increasing the temperature to 700-900 ℃ for calcining, keeping the temperature for 3-8h, and cooling to room temperature to obtain co-doped lithium titanate;
c. weighing a certain amount of co-doped lithium titanate prepared in the step (b), adding deionized water to prepare slurry with the concentration of 0.1-0.3g/mL, performing ball milling, and performing spray drying on the slurry to obtain powder with uniform particle size, wherein the powder is Li 4 Ti 5-x-y V x Cr y O 12 。
Further, the lithium source is at least one of lithium acetate, lithium carbonate and lithium hydroxide, the titanium source is at least one of isopropyl titanate and butyl titanate, the vanadium source is at least one of sodium vanadate, potassium vanadate and ammonium metavanadate, the chromium source is at least one of chromium nitrate and chromium chloride, the solvent is deionized water, ethanol or acetone, the protective atmosphere is selected from nitrogen or argon, and the temperature rising rate during calcination in the step (b) is 5-8 ℃/min.
Further, the spray drying has an inlet temperature of 150-220 ℃, an outlet temperature of 80-100 ℃ and a pressure of 0.1-0.3MPa.
Further, the ball milling is dry ball milling, and the time is 1-5h.
In another aspect, the invention provides a lithium ion power battery negative electrode, which comprises a copper foil and a negative electrode slurry coated on the copper foil, wherein the negative electrode slurry comprises the lithium ion power battery negative electrode material.
In another aspect, the invention provides a lithium ion power battery, which comprises the negative electrode of the lithium ion power battery.
Compared with the prior art, the invention has the following advantages:
(1) The anode material prepared by the invention is Ti-site co-doped lithium titanate, V and Cr easily enter a 16d position of the Ti site for co-doping by adopting a sol-gel method, wherein V and Cr have synergistic effect, so that the initial capacity and the cycling stability of the obtained anode material are obviously improved.
(2) The invention adopts a spray drying method to granulate again, and the obtained particle size is more uniform, spherical, uniform in particle size and high in tap density after spray drying.
(3) The invention pre-ball-mills the slurry before spray drying, and simultaneously controls the concentration of the slurry, so that the tap density of the product is higher and the performance is better.
(4) The material has simple preparation process, excellent electrochemical performance and good application prospect.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following specific examples, which are given below as preferred embodiments of the present invention, and it should be noted that the content of the present invention is not limited to the following examples.
Example 1
Weighing 16.33g of butyl titanate according to the molar ratio of n (Li) to n (Ti) to n (V) to n (Cr) =4:4.8:0.1:0.1, dispersing the butyl titanate in 50mL of absolute ethyl alcohol, and uniformly stirring and mixing to obtain a solution A; weighing 2.64g of LiAc, dissolving the LiAc in 10mL of deionized water, and uniformly stirring to obtain a solution B; 0.184g of Na was weighed out 3 VO 4 Dissolving the mixture in 10mL of deionized water, and uniformly stirring and mixing to obtain a solution C; 0.238g of Cr (NO) was weighed out 3 ) 3 Dissolving the mixture in 10mL of deionized water, and stirring and mixing the mixture uniformly to obtain solution D.
Under the action of magnetic stirring, slowly adding the solution B into the solution A, then simultaneously adding the solutions C and D to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining the gel at 500 ℃ in nitrogen atmosphere, keeping the temperature for 3 hours at a heating rate of 5 ℃/min, then calcining the gel at 800 ℃, keeping the temperature for 5 hours, and cooling the gel to room temperature to obtain the co-doped lithium titanate.
Weighing 4g of prepared co-doped lithium titanate, dispersing in 20mL of deionized water to prepare slurry with the concentration of 0.2g/mL, ball milling for 2h, and spray drying the slurry, wherein the inlet temperature is 200 ℃, the outlet temperature is 90 ℃, and the pressure is 0.2MPa, so as to obtain powder with uniform particle size, namely Li 4 Ti 4.8 V 0.1 Cr 0.1 O 12 。
Example 2
15 is weighed according to the mol ratio of n (Li) to n (Ti) to n (V) to n (Cr) =4:4.7:0.2:0.1.99g of tetrabutyl titanate is dispersed in 50mL of absolute ethyl alcohol, and the solution A is obtained after stirring and mixing uniformly; weighing 2.64g of LiAc, dissolving the LiAc in 10mL of deionized water, and uniformly stirring to obtain a solution B; 0.368g of Na was weighed out 3 VO 4 Dissolving the mixture in 10mL of deionized water, and uniformly stirring and mixing to obtain a solution C; 0.238g of Cr (NO) was weighed out 3 ) 3 Dissolving the mixture in 10mL of deionized water, and stirring and mixing the mixture uniformly to obtain solution D.
Under the action of magnetic stirring, slowly adding the solution B into the solution A, then simultaneously adding the solutions C and D to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining the gel at 500 ℃ in nitrogen atmosphere, keeping the temperature for 3 hours at a heating rate of 5 ℃/min, then calcining the gel at 800 ℃, keeping the temperature for 5 hours, and cooling the gel to room temperature to obtain the co-doped lithium titanate.
Weighing 4g of prepared co-doped lithium titanate, dispersing in 20mL of deionized water to prepare slurry with the concentration of 0.2g/mL, ball milling for 2h, and spray drying the slurry, wherein the inlet temperature is 200 ℃, the outlet temperature is 90 ℃, and the pressure is 0.2MPa, so as to obtain powder with uniform particle size, namely Li 4 Ti 4.7 V 0.2 Cr 0.1 O 12 。
Example 3
15.65g of butyl titanate is weighed according to the molar ratio of n (Li) to n (Ti) to n (V) to n (Cr) =4:4.6:0.1:0.3 and dispersed in 50mL of absolute ethyl alcohol, and the solution A is obtained after stirring and mixing uniformly; weighing 2.64g of LiAc, dissolving the LiAc in 10mL of deionized water, and uniformly stirring to obtain a solution B; 0.184g of Na was weighed out 3 VO 4 Dissolving the mixture in 10mL of deionized water, and uniformly stirring and mixing to obtain a solution C; 0.714g of Cr (NO) was weighed out 3 ) 3 Dissolving the mixture in 10mL of deionized water, and stirring and mixing the mixture uniformly to obtain solution D.
Under the action of magnetic stirring, slowly adding the solution B into the solution A, then simultaneously adding the solutions C and D to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining the gel at 500 ℃ in nitrogen atmosphere, keeping the temperature for 3 hours at a heating rate of 5 ℃/min, then calcining the gel at 800 ℃, keeping the temperature for 5 hours, and cooling the gel to room temperature to obtain the co-doped lithium titanate.
Weighing 4g of prepared co-doped lithium titanate, dispersing in 20mL of deionized water to prepare slurry with the concentration of 0.2g/mL, ball milling for 2h, and spray drying the slurry, wherein the inlet temperature is 200 ℃, the outlet temperature is 90 ℃, and the pressure is 0.2MPa, so as to obtain powder with uniform particle size, namely Li 4 Ti 4.6 V 0.1 Cr 0.3 O 12 。
Comparative example 1
17g of butyl titanate is weighed according to the molar ratio of n (Li) to n (Ti) =4:5 and dispersed in 50mL of absolute ethyl alcohol, and the mixture is stirred and mixed uniformly to obtain solution A; 2.64g of LiAc was weighed and dissolved in 10mL of deionized water, and stirred well to give solution B. Under the action of magnetic stirring, slowly adding the solution B into the solution A to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining at 500 ℃ in nitrogen atmosphere for 3h at a heating rate of 5 ℃/min, then calcining at 800 ℃ for 5h, and cooling to room temperature to obtain spinel Li 4 Ti 5 O 12 。
By the above embodiment, the specific test procedure of the present invention is as follows: in a glove box protected by argon, the prepared composite material of each embodiment is used as a negative electrode material, a negative electrode is prepared through operations such as slurry preparation, coating, drying and the like, a lithium sheet is used as a counter electrode, celgard 2400 (PP/PE/PP) is used as a diaphragm, 1M lithium hexafluorophosphate is dissolved in EC and DMC to be used as electrolyte, and a button cell shell model CR2016 is used for assembling a lithium battery. Under the condition of 0.1C of charge and discharge rate, a CT-4008 multichannel battery tester manufactured by Shenzhen Xinwei company is adopted to test the battery under the condition of constant temperature (25 ℃) in a laboratory. The test data include average particle size, tap density, initial capacity, and capacity retention after 100 cycles of the resulting material.
The data are shown in Table 1.
As can be seen from Table 1, the co-doped Li prepared according to the present invention 4 Ti 5 O 12 The composite material has excellent performance in all aspects. While the electrochemical performance of comparative example 1 was somewhat inferior.
Variations and modifications to the above would be obvious to those of ordinary skill in the art in light of the foregoing description. Therefore, the invention is not limited to the specific embodiments disclosed and described above, but equivalent modifications and variations of the invention should be made within the scope of the claims of the present invention. In addition, although specific terms are used in the present specification, these terms are for convenience of description only and do not limit the present invention in any way.
Claims (3)
1. A lithium ion power battery negative electrode material is characterized in that the chemical structural formula of the negative electrode material is Li 4 Ti 4.7 V 0.2 Cr 0.1 O 12 The average particle diameter is 320nm, and the tap density is 1.51 g/cm 3 The initial capacity is 173mAh/g, and the capacity retention rate is 97.2%;
the preparation method of the lithium ion power battery anode material comprises the following steps:
according to the molar ratio n (Li): n (Ti): n (V): n (Cr) =4:4.7: 0.2:0.1, 15.99g of butyl titanate is weighed and dispersed in 50mL of absolute ethyl alcohol, and the mixture is stirred and mixed uniformly to obtain solution A; weighing 2.64g of LiAc, dissolving the LiAc in 10mL of deionized water, and uniformly stirring to obtain a solution B; 0.368g of Na was weighed out 3 VO 4 Dissolving the mixture in 10mL of deionized water, and uniformly stirring and mixing to obtain a solution C; 0.238g of Cr (NO) was weighed out 3 ) 3 Dissolving the mixture in 10mL of deionized water, and uniformly stirring and mixing to obtain a solution D;
under the action of magnetic stirring, slowly adding the solution B into the solution A, then simultaneously adding the solutions C and D to obtain transparent sol, continuously stirring until gel is formed, drying and grinding the obtained gel, calcining the gel at 500 ℃ in nitrogen atmosphere, keeping the temperature for 3 hours at a heating rate of 5 ℃/min, then calcining the gel at 800 ℃ for 5 hours, and cooling the gel to room temperature to obtain co-doped lithium titanate;
weighing 4g of prepared co-doped lithium titanate, dispersing in 20mL of deionized water to prepare slurry with the concentration of 0.2g/mL, ball milling for 2h, and spray drying the slurry, wherein the inlet temperature is 200 ℃, the outlet temperature is 90 ℃, and the pressure is 0.2MPa, so as to obtain powder with uniform particle size, namely Li 4 Ti 4.7 V 0.2 Cr 0.1 O 12 。
2. A lithium ion power battery negative electrode, which comprises a copper foil and a negative electrode slurry coated on the copper foil, wherein the negative electrode slurry comprises the lithium ion power battery negative electrode material according to claim 1.
3. A lithium-ion power battery comprising the lithium-ion power battery anode of claim 2.
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| CN102153137B (en) * | 2011-05-18 | 2013-06-05 | 中南大学 | Method for preparing spherical lithium titanate from inorganic titanium sources |
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| CN103400977B (en) * | 2013-08-19 | 2015-06-17 | 攀枝花学院 | Sol-gel method for preparing lithium titanate |
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