CN111463419B - Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof - Google Patents
Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of lithium ion batteries, and provides a silicon-based @ titanium niobium oxide core-shell structure cathode material and a preparation method thereof, wherein a titanium source and a niobium source are used as coating layer raw materials, the titanium source and the niobium source are prepared into a nano suspension through a sand mill, and then nano-micron-sized silicon-based particles are uniformly dispersed in the suspension; and then granulating by a low-temperature rapid drying technology, and finally forging at a specific high temperature to obtain the silicon-based negative electrode material coated with the nano titanium niobium oxide, which has good particle appearance and uniform particle size distribution. The titanium niobium oxide is used as a coating layer, and on one hand, the titanium niobium oxide has higher capacity; on the other hand, the coating layer can inhibit the volume expansion of the silicon-based material caused in lithium ion deintercalation, and can prevent silicon-based particles from directly contacting with electrolyte, thereby being beneficial to forming a stable SEI film and improving the first effect, the multiplying power and the cycling stability of the material; the method is environment-friendly, pollution-free, simple and easy to implement and can be industrialized.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a silicon-based @ titanium niobium oxide core-shell structure negative electrode material formed by coating silicon-based particles with a titanium niobium oxide and a preparation method thereof.
Background
With the emergence of energy problems, green energy lithium ion batteries applied to electric vehicles and energy storage are urgently needed. The traditional graphite cathode (with specific capacity of 372mAh/g) battery can hardly meet the requirement of the current electric vehicle with long endurance mileage. Therefore, a series of high-capacity negative electrode materials are widely researched, wherein the Si-based material has higher application prospect in the field of lithium ion battery negative electrodes due to higher capacity (Si theoretical capacity is 4200mAh/g, SiO theoretical capacity is 2600mAh/g) and low lithium potential (0.1V vs Li/Li +).
However, the Si-based negative electrode material has the defects of poor conductivity, low first coulombic efficiency and easy decay of cycle performance; the requirements of practical application are still difficult to achieve. The titanium niobium oxide has high lithium storage capacity (the theoretical capacity is 390mAh/g), the crystal structure of the titanium niobium oxide is very beneficial to the insertion and the separation of lithium ions, lithium dendrites are not easy to form, and a discharge platform is stable, so the titanium niobium oxide is very suitable to be used as a coating material of silicon-based negative electrode particles; the volume expansion of the silicon material caused in the lithium ion extraction can be inhibited, the direct contact between the silicon material and electrolyte can be avoided, the stable SEI film formation is facilitated, and the silicon material is very suitable for being used as a coating layer of the silicon-based material.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon-based @ titanium niobium oxide core-shell structure cathode material, and the prepared silicon-based @ titanium niobium oxide core-shell structure cathode material overcomes the defects of the existing silicon-based cathode material in conductivity, first coulombic efficiency and cycle performance, so that the requirements of practical application can be met.
The invention also aims to provide a silicon-based @ titanium niobium oxide core-shell structure cathode material which takes a titanium source and a niobium source as coating raw materials and uniformly coats the surface of silicon-based particles.
A preparation method of a silicon-based @ titanium niobium oxide core-shell structured negative electrode material is characterized in that a titanium source and a niobium source are used as coating raw materials and are uniformly coated on the surface of silicon-based particles to obtain the silicon-based negative electrode material coated by nano titanium niobium oxide.
The method sequentially comprises the following steps:
step 1: weighing raw materials of a titanium source and a niobium source according to a molar ratio of 1:1.9-2.0, preparing a mixed solution with deionized water, and dispersing and stirring, wherein the mass ratio of the titanium source to the niobium source to the deionized water is 1: 5-20;
step 2: transferring the mixed solution obtained in the step 1 into a sand mill dispersion tank for ball milling, testing the particle size of the slurry in the ball milling process, and stopping ball milling until the particle sizes of the titanium source and the niobium source are within the range of 70-90nm to obtain a nano suspension;
and step 3: adding a silicon-based material into the nano suspension obtained in the step 2, ball-milling for 2-10min, and then leading out the suspension containing the silicon-based raw material, wherein the mass ratio of the silicon-based material to the titanium source is 90-95: 10;
and 4, step 4: carrying out low-temperature spray drying on the suspension containing the silicon-based raw material obtained in the step 3 to obtain a precursor of the silicon-based titanium niobium oxide negative electrode material;
and 5: putting the silicon-based titanium niobium oxide precursor obtained in the step (4) into an atmosphere protection furnace for forging treatment to obtain the silicon-based @ titanium niobium oxide core-shell structure cathode material; the forging treatment process comprises the following steps: raising the temperature to 1000-1200 ℃ at the temperature rise rate of 20-50 ℃/min under the inert atmosphere, and preserving the temperature for 10-30 min; then quickly reducing the temperature to 750 ℃ and 900 ℃, and preserving the temperature for 30-90 min.
In the step 1, the titanium source is any one of titanium dioxide, metatitanic acid, butyl titanate, tetraisopropyl titanate, titanium tetrachloride or titanium trichloride, and the niobium source is niobium pentoxide or niobium ethoxide.
Wherein, in the step 1, the dispersion stirring time is 10-60min, and the stirring speed is 200-600 r/min.
Wherein, in the step 2, the ball milling time is 30-300 min.
Wherein, in the step 3, the added silicon-based material is si or sio with the grain size range of 0.1um-50 um.
Wherein, in the step 4, the low-temperature spray drying temperature is 40-70 ℃, the feeding amount is 50-100ml/min, and the air inlet pressure is 4-8 MPa.
In the step 5, the inert atmosphere comprises one or more of argon, hydrogen-argon mixed gas and nitrogen.
The invention provides a preparation method of a silicon-based @ titanium niobium oxide core-shell structure cathode material, which comprises the steps of taking a titanium source and a niobium source as coating layer raw materials, preparing a nano suspension through a sand mill, and uniformly dispersing nano-micron-sized silicon-based particles in the suspension; the nanometer suspension containing the titanium source and the niobium source is automatically arranged and recombined on the surface of the silicon-based particles due to larger surface adsorption force; and then granulating by a rapid drying technology, and forging at high temperature by a certain procedure to obtain the silicon-based negative electrode material coated by the nano titanium niobium oxide, which has good particle appearance and uniform particle size distribution.
The preparation method of the silicon-based @ titanium niobium oxide core-shell structure cathode material provided by the invention has the following beneficial effects due to the adoption of the scheme:
(1) according to the invention, a titanium source and a niobium source are subjected to nano treatment to prepare a suspension, so that the titanium source and the niobium source are uniformly mixed, and the surface of a silicon-based particle is automatically coated by utilizing the surface adsorption force of the nano particle; on the other hand, the contact area of the titanium source and the niobium source is increased, and the high-temperature solid phase reaction time required by the synthesis of the titanium niobium oxide is reduced.
(2) The titanium niobium oxide is used as the silicon-based particle coating layer, so that the titanium niobium oxide has high capacity on one hand; on the other hand, the coating layer can inhibit the volume expansion of the silicon-based material caused in lithium ion extraction, and can prevent the silicon-based material from directly contacting with electrolyte, so that a stable SEI film can be formed, and the coating layer has important significance on the first effect, the multiplying power and the cycling stability of the material.
(3) The invention uses low-temperature rapid spray drying, the drying temperature is lower, and the capacity reduction caused by the oxidation of the silicon-based material is avoided.
(4) The specific forging process used in the invention not only ensures the synthesis of the titanium niobium oxide of the surface coating layer, but also can control the excessive disproportionation of the silicon-based particles.
(5) The preparation method adopted by the invention is environment-friendly, pollution-free, simple and easy to realize, and can be industrialized.
Drawings
Fig. 1 is an SEM image of the SiO @ titanium niobium oxide anode material prepared in example 1.
Fig. 2 is an SEM image of the SiO negative electrode material prepared in comparative example 1.
Fig. 3 shows the rate capability of the SiO @ ti niobium oxide anode material prepared in example 1 and the SiO anode material of comparative example 1. The ordinate is specific capacity, unit is: milliampere hours gram-1 (mAhg-1), and the abscissa represents the number of charge and discharge cycles.
Fig. 4 is a graph of the cycle performance and coulombic efficiency at 1C for the SiO @ titanium niobium oxide anode material prepared in example 1 and the SiO anode material of comparative example 1. The abscissa is the cycle number in units of: the left ordinate is the charge capacity in units of: mAhg-1, with coulombic efficiency on the right ordinate in units of: % of the total weight of the composition.
Detailed Description
The technical solutions provided in the present application will be further described with reference to the following specific embodiments and accompanying drawings. The advantages and features of the present application will become more apparent in conjunction with the following description.
It should be noted that the embodiments of the present application have a better implementation and are not intended to limit the present application in any way. The technical features or combinations of technical features described in the embodiments of the present application should not be considered as being isolated, and they may be combined with each other to achieve a better technical effect. The scope of the preferred embodiments of this application may also include additional implementations, and this should be understood by those skilled in the art to which the embodiments of this application pertain.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Comparative example 1
(1) Transferring 200ml of deionized water to a sand mill dispersing tank, adding 130g of sio with the particle size of 5um, and leading out the mixture after ball milling for 2 min;
(2) drying with a low-temperature spray dryer at 50 deg.C for air inlet and 100ml/min for feeding; the air inlet pressure is 6 MPa; obtaining a sio dry material;
(5) forging the sio dried material: heating to 1100 deg.C at a heating rate of 50 deg.C/min under the protection of argon, and maintaining for 30 min; then quickly cooling to 800 ℃, and preserving heat for 30 min; and cooling to room temperature to obtain the sio cathode material.
Example 1
(1) 1.53g of titanium dioxide was placed in a dispersion tank, and 9.78g of niobium pentoxide (in a molar ratio of the titanium source to the niobium source of 1:1.92) was added; 200ml of deionized water, and dispersing and stirring for 30 min;
(2) transferring the mixed solution to a sand mill dispersing tank, carrying out ball milling for 60min, and taking the slurry to carry out particle size testing, wherein the particle size is 79 nm;
(3) weighing 130g of sio with the particle size of 5um, adding the sio into the sand mill dispersion tank, continuing ball milling for 2min, and then guiding out the mixture;
(4) drying with a low-temperature spray dryer at an air inlet temperature of 50 deg.C and a feeding amount of 50 ml/min; the air inlet pressure is 6 MPa; obtaining a sio-TiNb oxide precursor;
(5) forging the sio-TiNb oxide precursor: heating to 1100 deg.C at a heating rate of 50 deg.C/min under the protection of argon, and maintaining for 30 min; then quickly cooling to 800 ℃, and preserving heat for 30 min; and (4) cooling to room temperature to obtain the sio @ titanium niobium oxide cathode material.
The sio @ titanium niobium oxide anode material prepared according to the steps has the average particle size of 4.8um, the specific surface area of about 4.8m2/g and the tap density of 1.15 g/ml.
FIG. 1 shows an SEM image of the sio @ TiNb oxide anode material of example 1, with an enlarged view of selected areas in the image at the top right, and with the nano TiNb oxide coating clearly visible.
FIG. 2 is an SEM image of the SiO negative electrode material of comparative example 1, and it can be seen from the enlarged view (upper right corner) of the selected area in the figure that the uncoated SiO surface is dense and has clear edges and corners, which are not favorable for electrolyte infiltration.
The nano titanium niobium oxide obtained in the invention is mainly TiNb2O7, so that the sio @ titanium niobium oxide negative electrode material not only shows high first efficiency of 80.9% (figure 3, the first reversible capacity of 0.1C reaches 994.6mAhg < -1 >), but also has better multiplying power performance, and the capacity can still reach 855mAhg < -1 > (figure 3) at the current of 5A/g; while the first effect of the sio material without being coated by the nano titanium niobium oxide is only 67%, and the capacity under the current of 5Ag-1 is only 615.6mAhg-1 (figure 3).
The prepared SiO @ titanium niobium oxide material is used as a lithium ion battery negative electrode material, is mixed with CMC + PAA (binder) and conductive carbon black (conductive agent) according to the mass ratio of 6:2:2 to prepare slurry, is coated on copper foil to prepare a pole piece, and is dried in a vacuum oven at 75 ℃ for 10 hours to prepare the pole piece with the diameter of 12 mm. A button cell is assembled in a glove box by using a polypropylene membrane (PE) diaphragm and adopting a 1.0mol/L lithium hexafluorophosphate (LiPF6), Ethylene Carbonate (EC), diethyl carbonate (DEC) (the volume ratio is 1:1) and 10% Fluoroacetate (FEC) mixed solution as electrolyte by taking a metal lithium sheet as a counter electrode. The electrochemical performance test is carried out by adopting a blue CT2001A type battery tester, the charge-discharge cut-off voltage is 0.005V-2V (vs Li +/Li), and the test temperature is 25 ℃.
The electrical property test shows that the material is charged and discharged for the first time as shown in figure 3, the charging and discharging current is 100mAhg < -1 > (0.1C), the first reversible capacity of the sio @ titanium niobium oxide negative electrode material can reach 994.6mAhg < -1 >, the first coulombic efficiency is as high as 80.9 percent (figure 4), and the first charging and discharging of the general sio material is high (1621 mAhg < -1 > in a comparative example 1), but the first efficiency is low and is only 67 percent (figure 4). As shown in FIG. 4, the specific capacity of the sio @ Ti niobium oxide negative electrode material can still reach 911.7mAh g < -1 > after 250 weeks under the current of 1Ag < -1 > (1C), the capacity retention rate is 92.6 percent, the specific capacity of the comparative sample sio is only 603.2mAh g < -1 >, the retention rate is 61.7 percent, and the attenuation is fast. Therefore, the material of the invention not only realizes the first efficiency improvement, but also can keep higher capacity retention rate.
Example 2
(1) Putting 1.82g of metatitanic acid into a dispersion tank, and adding 9.49g of niobium pentoxide (according to the molar ratio of the titanium source to the niobium source being 1: 1.92); 200ml of deionized water, and dispersing and stirring for 30 min;
(2) transferring the mixed solution to a sand mill dispersing tank, carrying out ball milling for 60min, and taking the slurry to carry out particle size test, wherein the particle size is 80 nm;
(3) weighing 130g of sio with the particle size of 5um, adding the sio into the sand mill dispersion tank, continuing ball milling for 2min, and then guiding out the mixture;
(4) drying with a low-temperature spray dryer at an air inlet temperature of 50 deg.C and a feeding amount of 50 ml/min; the air inlet pressure is 6 MPa; obtaining a sio-TiNb oxide precursor;
(5) forging the sio-TiNb oxide precursor: heating to 1100 deg.C at a heating rate of 50 deg.C/min under the protection of argon, and maintaining for 30 min; then quickly cooling to 800 ℃, and preserving heat for 30 min; and (4) cooling to room temperature to obtain the sio @ titanium niobium oxide cathode material.
Example 3
(1) Putting 1.4g of metatitanic acid into a dispersion tank, and adding 7.3g of niobium pentoxide (according to the molar ratio of the titanium source to the niobium source being 1: 1.92); 150ml of deionized water, and dispersing and stirring for 30 min;
(2) transferring the mixed solution to a sand mill dispersing tank, performing ball milling for 50min, and taking slurry for particle size testing, wherein the particle size is 85 nm;
(3) weighing 100g of si with the particle size of 200nm, adding the si into the sand mill dispersion tank, continuing ball milling for 2min, and then guiding out the mixture;
(4) drying with a low-temperature spray dryer at an air inlet temperature of 50 deg.C and a feeding amount of 50 ml/min; the air inlet pressure is 6 MPa; obtaining a si-titanium niobium oxide precursor;
(5) forging the si-titanium niobium oxide precursor: heating to 1100 deg.C at a heating rate of 50 deg.C/min under the protection of argon, and maintaining for 30 min; then quickly cooling to 800 ℃, and preserving heat for 30 min; and (4) cooling to room temperature to obtain the si @ titanium niobium oxide cathode material.
The above description is only illustrative of the preferred embodiments of the present application and is not intended to limit the scope of the present application in any way. Any changes or modifications made by those skilled in the art based on the above disclosure should be considered as equivalent effective embodiments, and all the changes or modifications should fall within the protection scope of the technical solution of the present application.
Claims (8)
1. A preparation method of a silicon-based @ titanium niobium oxide core-shell structure anode material is characterized by comprising the following steps of: the method comprises the steps of uniformly coating a titanium source and a niobium source serving as coating raw materials on the surface of silicon-based particles to obtain a silicon-based negative electrode material coated by nano titanium-niobium oxide; the method sequentially comprises the following steps:
step 1: weighing raw materials of a titanium source and a niobium source according to a molar ratio of 1:1.9-2.0, preparing a mixed solution with deionized water, and dispersing and stirring, wherein the mass ratio of the titanium source to the niobium source to the deionized water is 1: 5-20;
step 2: transferring the mixed solution obtained in the step 1 into a sand mill dispersion tank for ball milling, testing the particle size of the slurry in the ball milling process, and stopping ball milling until the particle sizes of the titanium source and the niobium source are within the range of 70-90nm to obtain a nano suspension;
and step 3: adding a silicon-based material into the nano suspension obtained in the step 2, ball-milling for 2-10min, and then leading out the suspension containing the silicon-based raw material, wherein the mass ratio of the silicon-based material to the titanium source is 90-95: 10;
and 4, step 4: carrying out low-temperature spray drying on the suspension containing the silicon-based raw material obtained in the step 3 to obtain a precursor of the silicon-based titanium niobium oxide negative electrode material; the low-temperature spray drying temperature is 40-70 ℃, the feeding amount is 50-100ml/min, and the air inlet pressure is 4-8 MPa;
and 5: putting the silicon-based titanium niobium oxide precursor obtained in the step (4) into an atmosphere protection furnace for forging treatment to obtain the silicon-based @ titanium niobium oxide core-shell structure cathode material; the forging treatment process comprises the following steps: raising the temperature to 1000-1200 ℃ at the temperature rise rate of 20-50 ℃/min under the inert atmosphere, and preserving the temperature for 10-30 min; then quickly reducing the temperature to 750 ℃ and 900 ℃, and preserving the temperature for 30-90 min.
2. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 1, the titanium source is any one of titanium dioxide, metatitanic acid, butyl titanate, tetraisopropyl titanate, titanium tetrachloride or titanium trichloride.
3. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 1, the niobium source is niobium pentoxide or niobium ethoxide.
4. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 1, the dispersing and stirring time is 10-60min, and the stirring speed is 200-600 r/min.
5. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 2, the ball milling time is 30-300 min.
6. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 3, the added silicon-based material is si or sio with the particle size range of 0.1-50 um.
7. The preparation method of the silicon-based @ titanium niobium oxide core-shell structured anode material as claimed in claim 1, wherein: in the step 5, the inert atmosphere comprises one or more of argon, hydrogen-argon mixed gas and nitrogen.
8. A silicon-based @ titanium niobium oxide core-shell structure anode material is characterized in that: the silicon-based anode material coated with the nano titanium niobium oxide is obtained by uniformly coating a titanium source and a niobium source serving as coating raw materials on the surface of silicon-based particles, and the anode material with the silicon-based @ titanium niobium oxide core-shell structure is prepared by the method of any one of claims 1 to 7.
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| CN112086629B (en) * | 2020-09-08 | 2022-05-06 | 合肥国轩高科动力能源有限公司 | Si @ C/ZnNb2O6Preparation method and application of negative electrode composite material |
| CN112467097A (en) * | 2020-10-30 | 2021-03-09 | 安普瑞斯（南京）有限公司 | Negative electrode material, preparation method thereof, electrode and secondary battery |
| CN112467099B (en) * | 2020-10-31 | 2022-04-05 | 浙江锋锂新能源科技有限公司 | TiNb2O7Method for producing a material |
| TWI743017B (en) | 2021-05-10 | 2021-10-11 | 台灣中油股份有限公司 | Lithium titanate/titanium niobate core-shell composite material and preparation method thereof |
| CN114914414A (en) * | 2022-04-24 | 2022-08-16 | 安徽工业大学 | Preparation method of silicon/titanium-niobium oxide composite anode material of lithium ion battery |
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