CN109987628B - Nb with nanowire structure2O5Preparation method of lithium ion battery anode material - Google Patents
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Abstract
Nb with nanowire structure2O5The preparation method of the lithium ion battery anode material comprises the steps of firstly adding niobium pentachloride into acetone to obtain a solution A; sequentially adding citric acid and deionized water into the solution A to obtain a mixed solution B; adjusting the pH value of the mixed solution B to 2-6 to obtain a mixed solution C; adding the mixed solution C into a reaction kettle for hydrothermal reaction, naturally cooling to room temperature, and precipitating; washing the obtained precipitate with water and alcohol respectively, and drying in vacuum to obtain a product D; sintering the product D in a high-temperature atmosphere furnace under the protection of argon, and then cooling the product with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material. The invention adopts a method of combining solvothermal treatment and heat treatment to prepare the nanowire-shaped Nb with better crystallinity and uniform distribution2O5. Different solvent volumes and sintering temperatures are adopted, so that the structure and the appearance of the prepared material can be favorably regulated and controlled, the process is simple, and the cost is low.
Description
Technical Field
The invention belongs to the technical field of battery materials, relates to a method for preparing a lithium ion battery anode material, and particularly relates to Nb with a nanowire structure2O5A preparation method of a lithium ion battery anode material.
Background
Due to the crisis of primary energy sources such as coal, oil and natural gas, the application of new energy sources is receiving global attention, and lithium ion batteries, as a clean energy source, have been applied to modern life on a large scale due to their superior performance.
The literature describes many transition metal oxides as electrode materials for lithium ion batteries, e.g. Co3O4[Deng X,Zhu S,He Fang,et al.Three-dimensionally hierarchical Co3O4/carbon composites with high pseudocapacitance contribution for enhancing lithium storage.Electrochimica Acta, 2018,283:1269-1276]，MnO[Kong X,Wang Y,Lin J,et al.Twin-nanoplate assembled hierarchical Ni/MnO porous microspheres as advancedanode materials for lithium-ion batteries.Electrochimica Acta,2018,259:419-426]，Fe3O4[Xu S,Hessel C,Ren H,et al. α-Fe2O3multi-shelled hollow microspheres for lithium ion battery anodes with superior capacity and charge retention.Energy&Environmental Science,2014,7(2):632-637]And the like, has rich resources and low price, and has the main advantage of high theoretical capacity. However, when used as an electrode material of a lithium ion battery, such transition metal oxides as these have a large volume expansion during charge and discharge, and Nb is2O5As one of transition metal oxides, there are advantages such as high operating voltage, no memory effect, and rapid charge and discharge, and relatively small volume expansion, and thus, they have attracted much attention as electrode materials for lithium ion batteries.
At present, a plurality of researchers prepare Nb with various morphologies2O5However, the preparation method is complex and high in preparation cost on the whole, and the obtained sample is not novel enough in appearance and is similar or different, so that the development of the method with low cost and simple preparation methodAnd has novel Nb with unique appearance2O5Has great development space.
Disclosure of Invention
The invention aims to provide Nb with a nanowire structure2O5A preparation method of a lithium ion battery anode material. The electrode prepared by the preparation method of the invention has good dispersibility, uniformity and stability.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) firstly, adding 0.50-1.5 g of analytically pure niobium pentachloride into 10-50 ml of acetone, uniformly stirring, and then performing ultrasonic dispersion to obtain a transparent solution A;
2) then, 0.2-1.0 g of citric acid is added into the transparent solution A, and 10-50 ml of deionized water is added into the solution A and uniformly mixed to obtain a mixed solution B;
3) adjusting the pH value of the mixed solution B to 2-6, and then performing ultrasonic dispersion to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction at the temperature of 120-200 ℃ 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 to obtain a product D;
6) heating the product D from room temperature to 500-900 ℃ in a high-temperature atmosphere furnace at a heating rate of 10 ℃/min under the protection of argon, treating for 2-4 h, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material.
The ultrasonic dispersion time in the step 1) is 20-60 min.
And 3) regulating the pH value of the mixed solution B to be 2-6 by adopting 2-4 mol/L hydrochloric acid.
The ultrasonic dispersion time in the step 3) is 60-120 min.
The filling ratio of the mixed liquid C added into the reaction kettle in the step 4) is 30-60%.
The hydrothermal reaction time in the step 4) is 120-360 min.
The vacuum drying temperature in the step 5) is 60-80 ℃, and the drying time is 1-3 h.
The invention adopts a method of combining solvothermal treatment and heat treatment to prepare the nanowire-shaped Nb with better crystallinity and uniform distribution2O5. Different solvent volumes and sintering temperatures are adopted, so that the structure and the appearance of the prepared material can be favorably regulated and controlled, the process is simple, and the cost is low.
FIG. 1 is a nanowire-structured Nb prepared in example 1 of the present invention2O5An XRD spectrum of the lithium ion battery anode material.
FIG. 2 is a nanowire-structured Nb prepared in example 1 of the present invention2O5And (3) SEM pictures of the lithium ion battery cathode material.
FIG. 3 is a nanowire-structured Nb prepared in example 1 of the present invention2O5A picture of the rate capability of the lithium ion battery anode material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
1) firstly, adding 0.5g of analytically pure niobium pentachloride into 10ml of acetone, uniformly stirring, and then carrying out ultrasonic dispersion for 30min to obtain a transparent solution A;
2) then 0.2g of citric acid is added into the transparent solution A, and 50ml of deionized water is added into the solution A and uniformly mixed to obtain mixed solution B;
3) regulating the pH value of the mixed solution B to 2 by using 2mol/L hydrochloric acid, and then performing ultrasonic dispersion for 120min 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 360min, 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 ℃ for 3 hours to obtain a product D;
6) heating the product D from room temperature to 900 ℃ for 2h in a high-temperature atmosphere furnace at the heating rate of 10 ℃/min under the protection of argon, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5Lithium ionA battery positive electrode material.
It can be seen from FIG. 1 that the invention successfully produces Nb2O5. In the figure Nb2O5The diffraction peaks of (A) correspond to T-Nb at 22.7 °, 28.4 °, 36.7 °, 46.2 °, 50.9 ° and 55.3 ° respectively2O5The (001), (180), (181), (002), (380) and (202) crystal planes of (A) and (B), except that no impurity peaks were observed at other positions, indicating that the purity of the sample was good.
As can be seen from FIG. 2, Nb is produced2O5Presents a nanowire structure and is uniformly dispersed.
FIG. 3 shows that the specific capacities of the products were 150, 110, 80, 50, 40, 30 and 10mAh/g at current densities of 50mA/g, 100mA/g, 200mA/g, 500mA/g, 1000mA/g, 2000mA/g and 5000mA/g, respectively; and when the current density returns to 50mA/g again, the specific capacity of the product can return to 150mAh/g, so that the nanowire-shaped Nb can be seen2O5The electrode material has good specific capacity reversibility and good rate capability.
Example 2:
1) firstly, adding 0.75g of analytically pure niobium pentachloride into 20ml of acetone, uniformly stirring, and then carrying out ultrasonic dispersion for 50min to obtain a transparent solution A;
2) then 0.4g of citric acid is added into the transparent solution A, and 40ml of deionized water is added into the solution A and uniformly mixed to obtain mixed solution B;
3) regulating the pH value of the mixed solution B to 3 by using 2.5mol/L hydrochloric acid, and then performing ultrasonic dispersion for 105min 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 140 ℃ for 300min, 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 ℃ for 2.5h to obtain a product D;
6) heating the product D from room temperature to 800 ℃ in a high-temperature atmosphere furnace at the heating rate of 10 ℃/min under the protection of argon, treating for 2.5h, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material.
Example 3:
1) firstly, adding 1g of analytically pure niobium pentachloride into 30ml of acetone, uniformly stirring, and then carrying out ultrasonic dispersion for 60min to obtain a transparent solution A;
2) then 0.6g of citric acid is added into the transparent solution A, and 30ml of deionized water is added into the solution A and uniformly mixed to obtain mixed solution B;
3) regulating the pH value of the mixed solution B to 4 by using 3mol/L hydrochloric acid, and then performing ultrasonic dispersion for 90min 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 160 ℃ for 240min, 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 ℃ for 2h to obtain a product D;
6) heating the product D from room temperature to 700 ℃ in a high-temperature atmosphere furnace at the heating rate of 10 ℃/min under the protection of argon for 3 hours, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material.
Example 4:
1) firstly, adding 1.25g of analytically pure niobium pentachloride into 40ml of acetone, uniformly stirring, and then carrying out ultrasonic dispersion for 20min to obtain a transparent solution A;
2) then 0.8g of citric acid is added into the transparent solution A, and 20ml of deionized water is added into the solution A and uniformly mixed to obtain mixed solution B;
3) regulating the pH value of the mixed solution B to 5 by using 3.5mol/L hydrochloric acid, and then performing ultrasonic dispersion for 75min 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 180 ℃ for 180min, 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 ℃ for 1.5h to obtain a product D;
6) placing the product D in a high-temperature atmosphere furnace, and argonHeating from room temperature to 600 deg.C under gas protection at a heating rate of 10 deg.C/min for 3.5h, and cooling in furnace to obtain Nb with nanowire structure2O5A lithium ion battery anode material.
Example 5:
1) firstly, adding 1.5g of analytically pure niobium pentachloride into 50ml of acetone, uniformly stirring, and then carrying out ultrasonic dispersion for 40min to obtain a transparent solution A;
2) then adding 1.0g of citric acid into the transparent solution A, adding 10ml of deionized water into the solution A, and uniformly mixing to obtain a mixed solution B;
3) regulating the pH value of the mixed solution B to 6 by using 4mol/L hydrochloric acid, and then performing ultrasonic dispersion for 60min to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle according to the filling ratio of 50%, sealing, carrying out hydrothermal reaction in a homogeneous reactor at 200 ℃ for 120min, 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 the precipitate in a vacuum drying oven at the temperature of 80 ℃ for 1h to obtain a product D;
6) heating the product D from room temperature to 500 ℃ in a high-temperature atmosphere furnace at the heating rate of 10 ℃/min under the protection of argon, treating for 4h, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material.
Claims (7)
1. Nb with nanowire structure2O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps:
1) firstly, adding 0.50-1.5 g of analytically pure niobium pentachloride into 10-50 ml of acetone, uniformly stirring, and then performing ultrasonic dispersion to obtain a transparent solution A;
2) then, 0.2-1.0 g of citric acid is added into the transparent solution A, and 10-50 ml of deionized water is added into the solution A and uniformly mixed to obtain a mixed solution B;
3) adjusting the pH value of the mixed solution B to 2-6, and then performing ultrasonic dispersion to obtain a mixed solution C;
4) adding the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction at the temperature of 120-200 ℃ 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 to obtain a product D;
6) heating the product D from room temperature to 500-900 ℃ in a high-temperature atmosphere furnace at a heating rate of 10 ℃/min under the protection of argon, treating for 2-4 h, and then cooling along with the furnace to obtain the Nb with the nanowire structure2O5A lithium ion battery anode material.
2. Nb of the nanowire structure of claim 12O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps: the ultrasonic dispersion time in the step 1) is 20-60 min.
3. Nb of the nanowire structure of claim 12O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps: and 3) regulating the pH value of the mixed solution B to be 2-6 by adopting 2-4 mol/L hydrochloric acid.
4. Nb of the nanowire structure of claim 12O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps: the ultrasonic dispersion time in the step 3) is 60-120 min.
5. Nb of the nanowire structure of claim 12O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps: the filling ratio of the mixed liquid C added into the reaction kettle in the step 4) is 30-60%.
6. Nb of the nanowire structure of claim 12O5The preparation method of the lithium ion battery anode material is characterized by comprising the following steps: the hydrothermal reaction time in the step 4) is 120-360 min.
7. Nb of the nanowire structure of claim 12O5Positive electrode of lithium ion batteryThe preparation method of the material is characterized by comprising the following steps: the vacuum drying temperature in the step 5) is 60-80 ℃, and the drying time is 1-3 h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025255A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical Nb2O5 electrode material and preparation method thereof |
| CN107369829A (en) * | 2017-06-30 | 2017-11-21 | 陕西科技大学 | A kind of preparation method of lithium ion battery Mao Danzhuan niobium oxide electrode materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025255A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical Nb2O5 electrode material and preparation method thereof |
| CN107369829A (en) * | 2017-06-30 | 2017-11-21 | 陕西科技大学 | A kind of preparation method of lithium ion battery Mao Danzhuan niobium oxide electrode materials |
Non-Patent Citations (3)
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| Highly Ordered Single Crystalline Nanowire Array Assembled Three-Dimensional Nb3O7(OH) and Nb2O5 Superstructures for Energy Storage and Conversion Applications;Haimin Zhang et al.;《ACS Nano》;20151118;第10卷;第507-514页 * |
| Nb2O5纳米线/碳纤维制备及Cr(VI)吸附降解研究;王学凯等;《非金属矿》;20170930;第40卷(第5期);第82-85页 * |
| 用作锂离子电池正极材料的不同晶型五氧化二铌的制备及其电化学性能;黄剑锋等;《陕西科技大学学报》;20190228;第37卷(第1期);第89-95页 * |
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