CN110627114B - Modified lithium titanate negative electrode material and preparation method thereof - Google Patents
Modified lithium titanate negative electrode material and preparation method thereof Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- 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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Abstract
The invention provides a modified lithium titanate negative electrode material and a preparation method thereof, the method adopts a direct molten salt method of a low-temperature co-molten lithium source, the low-temperature co-molten lithium source is a mixed lithium source comprising lithium acetate and at least one of lithium carbonate, lithium hydroxide and lithium chloride, the combination provides a good liquid phase environment for reaction, increases the ion diffusion rate, and in addition, nano-scale carbon powder and Cr are simultaneously doped, and the functions of the nano-scale carbon powder and the Cr enable the modified lithium titanate to have better conductivity, better reversible cyclicity and better rate discharge performance.
Description
Technical Field
The invention relates to the technical field of negative electrode materials of lithium ion power batteries, in particular to a modified lithium titanate negative electrode material of a lithium ion power battery and a preparation method thereof.
Background
The lithium ion power battery has the advantages of long cycle life, high energy density and the like, and is widely applied to the field of new energy automobiles, but the problems of weak cruising ability, poor safety and the like are always the technical direction of more important research in the field of new energy.
Spinel lithium titanate is used as a negative electrode material which is in particular concerned, and has the following advantages: 1) the lithium titanate has almost zero strain before and after lithium is deintercalated; 2) the lithium intercalation potential is higher (1.55V), the generation of lithium dendrite can be effectively avoided, and the safety is higher; 3) has a very flat voltage plateau; 4) the chemical diffusion coefficient and the coulombic efficiency are high.
The modification is usually carried out by mixing conductive carbon, and the addition of carbon has various functions, such as being used as a reducing agent, so that the reaction of lithium is more complete, and the particle size of the product can be reduced. Such as carbon coating and carbon doping, can effectively improve the conductivity and high rate performance of the material.
The Cr element is a common doping element, and easily enters 16d octahedral space occupation of Ti, so that the structure of the spinel is more favorably stabilized, and the capacity and the cycle performance of the electrode material can be improved. Based on the fact that the electrochemical performance of the lithium titanate is improved, the lithium titanate is doped with carbon powder and Cr elements, so that the conductivity, high rate performance, initial capacity and cycling stability of the lithium titanate are effectively improved.
Disclosure of Invention
The invention provides a modified lithium titanate negative electrode material and a preparation method thereof, wherein a direct molten salt method of a low-temperature co-molten lithium source is adopted, nano-scale carbon powder and Cr are simultaneously doped in the method, and the modified lithium titanate has better conductivity, reversible cyclicity and rate discharge performance under the action of the nano-scale carbon powder and the Cr.
In order to achieve the above object, the invention provides a modified lithium titanate negative electrode material, which is carbon powder and transition metal element co-doped lithium titanate, wherein the transition metal element is Ti-site doped.
Further, the chemical structural formula is as follows: li4Ti5-xCrxO12and/C, wherein x is more than 0 and less than or equal to 0.3.
Further, the carbon powder is preferably nano-scale graphite powder, and the average particle size of the carbon powder is 5-50 nm.
Further, the doping amount of the nano graphite powder is 5-20wt%, wherein the doping amount is that the graphite powder accounts for the Li modified lithium titanate4Ti5-xCrxO12In percentage by mass.
Further, the anode material is preferably Li4Ti4.7Cr0.3O12C, the doping amount of C is 5 wt%, or Li4Ti4.8Cr0.2O12C, the doping amount of C is 10 wt%, or Li4Ti4.9Cr0.1O12C, the doping amount of C is 20wt%, or Li4Ti4.95Cr0.05O12C, the doping amount of C is 15 wt%.
The invention also provides a preparation method of the modified lithium titanate negative electrode material, the codoped lithium titanate is prepared by adopting a direct molten salt method of a low-temperature eutectic lithium source, and the preparation method specifically comprises the following steps:
a. weighing a certain amount of nano-scale graphite powder, dispersing the nano-scale graphite powder into concentrated nitric acid, heating and refluxing, centrifugally separating, washing with water, and drying in a vacuum drying oven for later use;
b. weighing certain amounts of low-temperature co-melting lithium source, titanium source and chromium source according to the molar ratio of n (Li) to n (Ti) to n (Cr) to 4 to (5-x) to x, uniformly mixing the weighed compounds, adding the graphite powder treated in the step (a), and carrying out ball milling on the obtained mixture, wherein the low-temperature co-melting lithium source is a mixed lithium source comprising lithium acetate and at least one selected from lithium carbonate, lithium hydroxide and lithium chloride, and x is more than 0 and less than or equal to 0.3;
c. taking out the product after ball milling in the step (b), placing the product in a tubular furnace for two-stage calcination, firstly heating the furnace to 500 ℃ for 2-5h, then heating to 1000 ℃ for calcination, and cooling to room temperature to obtain co-doped lithium titanate, which is marked as Li4Ti5-xCrxO12/C；
Further, the average particle size of the nano graphite powder is 5-50nm, the titanium source is selected from anatase titanium dioxide, the chromium source is selected from any one of chromium oxide and chromium tetraoxide, the atmosphere during calcination is selected from air or nitrogen, and the temperature rise rate during calcination is 5-8 ℃/min.
Furthermore, the doping amount of the nano graphite powder is 5-20wt%, and the mass percentage of lithium acetate in the low-temperature eutectic lithium source is 50-80 wt%.
Further, the heating reflux in the step (a) is carried out in 6M nitric acid solution at 70-90 ℃ for 12-24 h.
The invention also provides a lithium ion power battery cathode, which comprises a copper foil and cathode slurry coated on the copper foil, wherein the cathode slurry comprises the modified lithium titanate cathode material.
The invention also provides a lithium ion power battery, which comprises the lithium ion power battery negative electrode.
Compared with the prior art, the invention has the following advantages:
(1) the modified lithium titanate negative electrode material prepared by the invention is doped with nanoscale carbon powder and Cr at the same time, the carbon powder is doped and is different from coating, the completeness of reaction conversion can be effectively promoted after a small amount of carbon powder is doped, the crystallization of the product is better, and the spinel structure of lithium titanate is not influenced after detection. Meanwhile, Cr is doped on the 16d position of Ti, and the modified lithium titanate has better conductivity, reversible cyclicity and rate discharge performance under the action of the Cr and the Cr.
(2) The low-temperature eutectic lithium source is a mixed lithium source comprising lithium acetate and at least one of lithium carbonate, lithium hydroxide and lithium chloride, and the combination provides a good liquid phase environment for the reaction, increases the ion diffusion rate, and improves the reaction rate and the completion degree.
(3) 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 is further illustrated below by reference to specific examples, which are set forth to illustrate preferred embodiments of the present invention, and it should be understood that the present invention is not limited to the following examples.
Example 1
Weighing 0.5g of nano-scale graphite powder, dispersing the graphite powder into 6M concentrated nitric acid, heating and refluxing for 12 hours at 80 ℃, centrifugally separating, washing with water, and drying in a vacuum drying oven for later use.
7.92g of LiAc.2H are weighed in the molar ratio n (Li) to n (Ti) to n (Cr) 4: 4.7: 0.32O and 3.26g of LiOH H2O, 14.59g of TiO2And 0.88g of Cr2O3After mixing evenly, adding the pretreated graphite powder, and carrying out ball milling on the obtained mixture for 8 h. Then taking out the ball-milled product, placing the ball-milled product in a tubular furnace for two-stage calcination, firstly heating the furnace to 400 ℃ for calcination, keeping the temperature for 3h, then heating to 900 ℃ for calcination, keeping the temperature for 5h, cooling to room temperature to obtain co-doped lithium titanate, and marking the co-doped lithium titanate as Li4Ti4.7Cr0.3O12C, wherein the doping amount of C is 5 wt%.
Example 2
Weighing 1g of nano-scale graphite powder, dispersing the nano-scale graphite powder into 6M concentrated nitric acid, heating and refluxing for 12 hours at 80 ℃, carrying out centrifugal separation, washing with water, and drying in a vacuum drying oven for later use.
7.92g of LiAc.2H are weighed in the molar ratio n (Li) to n (Ti) to n (Cr) of 4: 4.8: 0.22O and 3.26g of LiOH H2O, 14.9g of TiO2And 0.59g of Cr2O3After mixing evenly, adding the pretreated graphite powder, and carrying out ball milling on the obtained mixture for 8 h. Then taking out the ball-milled product, placing the ball-milled product in a tubular furnace for two-stage calcination, firstly heating the furnace to 400 ℃ for calcination, keeping the temperature for 3h, then heating to 900 ℃ for calcination, keeping the temperature for 5h, cooling to room temperature to obtain co-doped lithium titanate, and marking the co-doped lithium titanate as Li4Ti4.8Cr0.2O12C, wherein the doping amount of C is 10 wt%.
Example 3
Weighing 2g of nano-scale graphite powder, dispersing the nano-scale graphite powder into 6M concentrated nitric acid, heating and refluxing for 12 hours at 80 ℃, carrying out centrifugal separation, washing with water, and drying in a vacuum drying oven for later use.
7.92g of LiAc.2H are weighed in the molar ratio n (Li) to n (Ti) to n (Cr) 4: 4.9: 0.12O and 3.26g of LiOH H2O, 15.21g of TiO2And 0.29g of Cr2O3After mixing evenly, adding the pretreated graphite powder, and carrying out ball milling on the obtained mixture for 8 h. Then taking out the ball-milled product, placing the ball-milled product in a tubular furnace for two-stage calcination, firstly heating the furnace to 400 ℃ for calcination, keeping the temperature for 3h, then heating to 900 ℃ for calcination, keeping the temperature for 5h, cooling to room temperature to obtain co-doped lithium titanate, and marking the co-doped lithium titanate as Li4Ti4.9Cr0.1O12C, wherein the doping amount of C is 20 wt%.
Example 4
Weighing 1.5g of nano-scale graphite powder, dispersing the graphite powder into 6M concentrated nitric acid, heating and refluxing for 12 hours at 80 ℃, centrifugally separating, washing with water, and drying in a vacuum drying oven for later use.
7.92g of LiAc.2H are weighed in the molar ratio n (Li) to n (Ti) to n (Cr) 4: 4.95: 0.052O and 3.26g of LiOH H2O, 15.36g of TiO2And 0.15g of Cr2O3After mixing evenly, adding the pretreated graphite powder, and carrying out ball milling on the obtained mixture for 8 h. Then taking out the ball-milled product, placing the ball-milled product in a tubular furnace for two-stage calcination, firstly heating the furnace to 400 ℃ for calcination, keeping the temperature for 3h, then heating to 900 ℃ for calcination, keeping the temperature for 5h, cooling to room temperature to obtain co-doped lithium titanate, and marking the co-doped lithium titanate as Li4Ti4.95Cr0.05O12C, wherein the doping amount of C is 15 wt%.
Comparative example 1
7.92g of LiAc.2H are weighed in a molar ratio of n (Li) to n (Ti) of 4: 52O and 3.26g of LiOH H2O, 15.52g TiO2After mixing well, the resulting mixture was ball milled for 8 h. And then taking out the ball-milled product, placing the ball-milled product in a tubular furnace for two-stage calcination, firstly heating the furnace to 400 ℃ for calcination, keeping the temperature for 3h, then heating to 900 ℃ for calcination, keeping the temperature for 5h, and cooling to room temperature to obtain the spinel lithium titanate.
Through the above embodiment, the specific test process of the present invention is as follows: in an argon-protected glove box, the prepared composite material of each embodiment is used as a negative electrode material, the negative electrode is prepared by operations of 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 the button type battery shell is CR2016 to be assembled into a lithium battery. Under the condition that the charge and discharge rate is 0.1C, the battery is tested by adopting a CT-4008 multi-channel battery tester produced by Shenzhen Xinwei company under the indoor constant temperature condition (25 ℃). The test data included the average particle size, tap density, initial capacity and capacity retention after 100 cycles of the prepared material.
The data are shown in table 1.
| Examples | Structural formula (I) | The doping amount of C is wt% | Initial capacity mAh/g | Capacity retention ratio% |
| Example 1 | Li4Ti4.7Cr0.3O12/C | 5 | 169 | 98.3 |
| Example 2 | Li4Ti4.8Cr0.2O12/C | 10 | 167 | 97.7 |
| Example 3 | Li4Ti4.9Cr0.1O12/C | 20 | 165 | 97.5 |
| Comparative example 1 | Li4Ti4.95Cr0.05O12/C | 15 | 163 | 96.2 |
| Comparative example 2 | Li4Ti5O12 | - | 123 | 75.3 |
As can be seen from Table 1, co-doped Li prepared by the present invention4Ti5O12The composite material has excellent performance in all aspects. Whereas comparative example 1 was somewhat inferior in electrochemical performance.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which are disclosed and described in the above specification. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some equivalent modifications and variations of the present invention should be covered by the protection scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (1)
1. The preparation method of the modified lithium titanate negative electrode material is characterized in that the codoped lithium titanate is prepared by adopting a direct molten salt method of a low-temperature eutectic lithium source, and specifically comprises the following steps:
a. weighing nano-scale graphite powder, wherein the average particle size of the nano-scale graphite powder is 5-50nm, the doping amount of the nano-scale graphite powder is 5-20wt%, dispersing the nano-scale graphite powder into concentrated nitric acid, heating and refluxing, centrifugally separating, washing with water, and drying in a vacuum drying oven for later use;
b. according to the molar ratio n (Li): n (Ti): n (Cr) =4 (5-x): x, respectively weighing a low-temperature co-melting lithium source, a titanium source and a chromium source, uniformly mixing the weighed compounds, then adding the nano-scale graphite powder treated in the step (a), and carrying out ball milling on the obtained mixture, wherein the low-temperature co-melting lithium source is a mixed lithium source which comprises lithium acetate and at least one of lithium carbonate, lithium hydroxide and lithium chloride, and x is more than 0 and less than or equal to 0.3;
c. taking out the product after ball milling in the step (b), placing the product in a tubular furnace for two-stage calcination, firstly heating the furnace to 500 ℃ for 2-5h, then heating to 1000 ℃ for calcination, and cooling to room temperature to obtain co-doped lithium titanate, which is marked as Li4Ti5-xCrxO12/C；
Wherein, the titanium source in the step (b) is selected from anatase titanium dioxide, the chromium source is selected from any one of chromium sesquioxide and chromium sesquioxide, the atmosphere in the calcination in the step (c) is selected from air or nitrogen, and the temperature rising rate in the calcination is 5-8 ℃/min;
the mass percent of lithium acetate in the low-temperature eutectic lithium source in the step (b) is 50-80 wt%;
in the step (a), the heating reflux is carried out for 12-24h in 6M nitric acid solution at 70-90 ℃;
the chemical structural formula of the co-doped lithium titanate is selected from Li4Ti4.7Cr0.3O12/C、Li4Ti4.8Cr0.2O12C and Li4Ti4.9Cr0.1O12Any one of the components/C, wherein x is more than 0 and less than or equal to 0.3.
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| CN1622368A (en) * | 2004-12-17 | 2005-06-01 | 清华大学 | Preparation method of spherical Li4Ti5O12 as lithium ion cell cathode material |
| CN1677740A (en) * | 2004-03-31 | 2005-10-05 | 株式会社东芝 | Nonaqueous electrolyte |
| CN101000960A (en) * | 2006-12-29 | 2007-07-18 | 深圳市贝特瑞电子材料有限公司 | Composite lithium titanate electrode material and preparation method thereof |
| CN102468485A (en) * | 2010-11-04 | 2012-05-23 | 海洋王照明科技股份有限公司 | Lithium titanate composite material, preparation method thereof, and application thereof |
| US10008723B1 (en) * | 2016-05-17 | 2018-06-26 | Nanotek Instruments, Inc. | Chemical-free production of graphene-wrapped electrode active material particles for battery applications |
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| US9428396B2 (en) * | 2011-04-28 | 2016-08-30 | Ishihara Sangyo Kaisha, Ltd | Method for producing lithium titanate precursor, method for producing lithium titanate, lithium titanate, electrode active material, and electricity storage device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1677740A (en) * | 2004-03-31 | 2005-10-05 | 株式会社东芝 | Nonaqueous electrolyte |
| CN1622368A (en) * | 2004-12-17 | 2005-06-01 | 清华大学 | Preparation method of spherical Li4Ti5O12 as lithium ion cell cathode material |
| CN101000960A (en) * | 2006-12-29 | 2007-07-18 | 深圳市贝特瑞电子材料有限公司 | Composite lithium titanate electrode material and preparation method thereof |
| CN102468485A (en) * | 2010-11-04 | 2012-05-23 | 海洋王照明科技股份有限公司 | Lithium titanate composite material, preparation method thereof, and application thereof |
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