CN109950525B - Hair belly-shaped Nb2O5Preparation method of lithium ion battery electrode material - Google Patents
Hair belly-shaped Nb2O5Preparation method of lithium ion battery electrode material Download PDFInfo
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Abstract
Hair belly-shaped Nb2O5Firstly, adding analytically pure niobium oxalate hydrate into distilled water to obtain A; then adding glucose into distilled water to obtain B; mixing A and B to obtain a mixed solution C; carrying out hydrothermal reaction on the mixed solution C in a homogeneous reaction instrument, and cooling to room temperature to obtain a precipitate; drying the obtained precipitate in a vacuum drying oven to obtain a precursor D; adding the precursor D into distilled water to obtain a solution E; adding melamine into oleic acid to obtain a solution F; mixing the solution E and the solution F, carrying out a secondary hydrothermal reaction, naturally cooling to room temperature, and then precipitating; freeze drying the precipitate to obtain MAODU-shaped Nb2O5An electrode material for lithium ion batteries. The invention adopts a secondary hydrothermal method to prepare the morel-shaped Nb with better crystallinity and uniform distribution2O5The nano material adopts different oleic acid addition amounts as a carbon source and a surfactant, can be beneficial to regulating and controlling the structure and the appearance of the prepared material, and has the advantages of simple process and low cost.
Description
Technical Field
The invention belongs to the technical field of battery materials, relates to a preparation method of a lithium ion battery cathode material, and particularly relates to a mao-bellied Nb2O5A preparation method of an electrode material of a lithium ion battery.
Background
Due to the development and progress of science and technology, the primary energy sources such as coal, petroleum, natural gas and the like are in crisis, and the development of new energy sources is widely concerned. As a device for realizing mutual conversion between electric energy and chemical energy, a lithium ion battery has been widely used in modern life as a clean energy source as the quantity and quality of electronic products for civil use have been improved.
Currently, many transition metal oxides have been developed on the market as electrode materials for lithium ion batteries, most of which undergo alloying and conversion reactions with a large volume expansion, while Nb is used as a material for lithium ion batteries2O5As one of the transition metal oxides, it undergoes intercalation [ Augustyn V, Come J, Lowe M, et al+intercalation pseudocapacitance.Nature Materials,2013,12(6): 518-522]And the volume expansion is smaller. Griffith et al [ Griffith K, Forse A, Griffin J, et. high-rate interaction with out nanostructing in metastable Nb2O5bronzephases.Journal of the American Chemical Society,2016,138(28):8888-8899]Four kinds of Nb with different crystal forms are prepared by a calcination method2O5There are TT phase, T phase, B phase and H phase. Literature [ Zeng G, Wang H, GuoJ, et al2O5/C nanocomposites as a high performance anode forlithium ion battery. Chinese Chemical Letters,2017,28(4):755-758]A T phase Nb2O5Has pseudocapacitance behavior due to its interplanar spacing of (001)
While the diameter of the lithium ion is only
So that lithium ions are inserted into or extracted from T-Nb2O5The (001) plane of (a) is relatively easy. However, intercalated Nb2O5Meanwhile, the conductive film also has some defects, such as lower conductivity, which has been paid attention to by many researchers, and the conductivity of the conductive film is improved by changing the morphology, regulating the nanocrystallization, and carrying out compounding and doping on the conductive film.
The existing method does not improve Nb to a great extent2O5The conductivity of the material is improved, so that the specific discharge capacity of the material as the negative electrode material of the lithium ion battery is improved. And the existing preparation method processComplicated and tedious and high-cost, therefore, the development of the Nb preparation with low cost and short reaction period2O5The electrode method has great research significance.
Disclosure of Invention
The invention aims to provide a morel-shaped Nb with low preparation cost and special sample appearance2O5The preparation method of the electrode material of the lithium ion battery can prepare the morchella-shaped Nb with uniform dispersion and stable structure2O5The electrode material of the lithium ion battery has high specific discharge capacity.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) firstly, adding 0.60-1.0 g of analytically pure niobium oxalate hydrate into 30ml of distilled water, and uniformly stirring to obtain a transparent solution A;
2) then adding 1.2-2.0 g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction in a homogeneous phase reactor at 120-160 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven to obtain a precursor D;
6) adding 1.0-1.8 g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a suspension E;
7) adding 0.2-0.6 g of melamine into 30-60 ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the suspension E and the solution F, uniformly stirring, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction at 160-200 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven to obtain morel-shaped Nb2O5An electrode material for lithium ion batteries.
The ultrasonic dispersion time in the step 3) is 20-60 min.
The filling ratio of the mixed solution C in the step 4) added into the reaction kettle is 30-60%.
The hydrothermal reaction time in the step 4) is 12-24 h.
And 5) drying the vacuum drying oven at the drying temperature of 60-80 ℃.
The hydrothermal reaction time in the step 8) is 12-24 h.
The freeze drying temperature in the step 9) is-40 to-30 ℃, and the drying time is 8 to 12 hours.
The invention adopts a secondary hydrothermal method to prepare the morel-shaped Nb with better crystallinity and uniform distribution2O5The nano material adopts different oleic acid addition amounts as a carbon source and a surfactant, can be beneficial to regulating and controlling the structure and the appearance of the prepared material, and has the advantages of simple process and low cost.
Drawings
FIG. 1 shows a morel-like Nb prepared in example 1 of the present invention2O5XRD pattern of electrode material of lithium ion battery.
FIG. 2 shows a morel-like Nb prepared in example 1 of the present invention2O5SEM photographs of the lithium ion battery electrode material.
FIG. 3 shows a morel-like Nb prepared in example 1 of the present invention2O5And (3) a cycle performance picture of the lithium ion battery electrode material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
1) firstly, 0.6g of analytically pure niobium oxalate hydrate is added into 30ml of distilled water and stirred uniformly to obtain a transparent solution A;
2) then adding 1.2g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then performing ultrasonic dispersion for 20min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to the filling ratio of 30%, sealing, carrying out hydrothermal reaction in a homogeneous reactor at 120 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven at 70 ℃ to obtain a precursor D;
6) adding 1.8g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a solution E;
7) adding 0.6g of melamine into 60ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the solution E and the solution F, stirring uniformly, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction at 160 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven at-40 deg.C for 8h to obtain MAODU-shaped Nb2O5An electrode material for lithium ion batteries.
FIG. 1 shows that T-Nb is successfully prepared by the present invention2O5. The diffraction peaks corresponding to the (001), (180), (181), (002), (380) and (202) crystal planes can be seen, indicating that the sample is pure T-Nb2O5。
As can be seen from FIG. 2, the prepared morel-like Nb2O5The dispersion is uniform, and a plurality of small rods can be clearly seen to grow on the sheet and are shaped like a tripe.
FIG. 3 shows a morel-like Nb prepared in example 12O5Cycle performance pictures (current density 100 mA/g) of nanomaterials. The specific capacity of the product reaches 375mAh/g under the current density of 100mA/g, and Nb is obtained after 40 cycles2O5The specific capacity of the electrode also has a tendency to rise. Therefore, it is prepared from Nb2O5When the material is used as a negative electrode material of a lithium ion battery, the material shows high specific discharge capacity and good reversibility.
Example 2:
1) firstly, 0.7g of analytically pure niobium oxalate hydrate is added into 30ml of distilled water and stirred uniformly to obtain a transparent solution A;
2) then adding 1.4g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion for 30min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to 50% of filling ratio, sealing, carrying out hydrothermal reaction for 15h at 150 ℃ in a homogeneous phase reactor, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven at 60 ℃ to obtain a precursor D;
6) adding 1.6g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a solution E;
7) adding 0.5g of melamine into 50ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the solution E and the solution F, stirring uniformly, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction at 170 ℃ for 21h, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven at-30 ℃ for 12h to obtain morel-shaped Nb2O5An electrode material for lithium ion batteries.
Example 3:
1) firstly, 0.8g of analytically pure niobium oxalate hydrate is added into 30ml of distilled water and stirred uniformly to obtain a transparent solution A;
2) then adding 1.6g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion for 40min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to the filling ratio of 60%, sealing, carrying out hydrothermal reaction in a homogeneous reactor at 16 ℃ for 12 hours, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven at 80 ℃ to obtain a precursor D;
6) adding 1.4g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a solution E;
7) adding 0.4g of melamine into 45ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the solution E and the solution F, stirring uniformly, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction at 180 ℃ for 18h, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven at-35 deg.C for 10h to obtain MAODU-shaped Nb2O5An electrode material for lithium ion batteries.
Example 4:
1) firstly, 0.9g of analytically pure niobium oxalate hydrate is added into 30ml of distilled water and stirred uniformly to obtain a transparent solution A;
2) then adding 1.8g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion for 50min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to the filling ratio of 40%, sealing, carrying out hydrothermal reaction in a homogeneous reactor at 130 ℃ for 20 hours, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven at 65 ℃ to obtain a precursor D;
6) adding 1.2g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a solution E;
7) adding 0.3g of melamine into 40ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the solution E and the solution F, stirring uniformly, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction for 15h at 190 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven at-40 deg.C for 11h to obtain MAODU-shaped Nb2O5An electrode material for lithium ion batteries.
Example 5:
1) firstly, adding 1.0g of analytically pure niobium oxalate hydrate into 30ml of distilled water, and uniformly stirring to obtain a transparent solution A;
2) then adding 2.0g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion for 60min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to 50% of filling ratio, sealing, carrying out hydrothermal reaction in a homogeneous reactor at 140 ℃ for 18h, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven at 75 ℃ to obtain a precursor D;
6) adding 1.0g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a solution E;
7) adding 0.2g of melamine into 30ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the solution E and the solution F, stirring uniformly, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction for 12 hours at 200 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven at-30 ℃ for 9h to obtain morel-shaped Nb2O5An electrode material for lithium ion batteries.
Claims (7)
1. Hair belly-shaped Nb2O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps:
1) firstly, adding 0.60-1.0 g of analytically pure niobium oxalate hydrate into 30ml of distilled water, and uniformly stirring to obtain a transparent solution A;
2) then adding 1.2-2.0 g of glucose into 30ml of distilled water, and uniformly stirring to obtain a transparent solution B;
3) mixing the solution A and the solution B, and then carrying out ultrasonic dispersion to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction in a homogeneous phase reactor at 120-160 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, and drying in a vacuum drying oven to obtain a precursor D;
6) adding 1.0-1.8 g of the precursor D into 30ml of distilled water, and uniformly stirring to obtain a suspension E;
7) adding 0.2-0.6 g of melamine into 30-60 ml of oleic acid, and uniformly stirring to obtain a solution F;
8) mixing the suspension E and the solution F, uniformly stirring, adding into an inner reaction kettle, carrying out secondary hydrothermal reaction at 160-200 ℃, naturally cooling to room temperature after the reaction is finished, and precipitating;
9) washing the precipitate obtained in the step 8) with water and alcohol respectively, and drying in a freeze drying oven to obtain morel-shaped Nb2O5An electrode material for lithium ion batteries.
2. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: the ultrasonic dispersion time in the step 3) is 20-60 min.
3. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: the filling ratio of the mixed solution C in the step 4) added into the reaction kettle is 30-60%.
4. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: the hydrothermal reaction time in the step 4) is 12-24 h.
5. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: and 5) drying the vacuum drying oven at the drying temperature of 60-80 ℃.
6. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: the hydrothermal reaction time of the step 8) is 12-24h。
7. Hair belly-like Nb according to claim 12O5The preparation method of the lithium ion battery electrode material is characterized by comprising the following steps: the freeze drying temperature in the step 9) is-40 to-30 ℃, and the drying time is 8 to 12 hours.
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| 五氧化二钒电极材料的研究新进展;林源 等;《无机盐工业》;20121010;第57-60页 * |
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