CN112357960A - Preparation method and application of rare earth element neodymium-doped titanium niobate material - Google Patents
Preparation method and application of rare earth element neodymium-doped titanium niobate material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-performance rare earth element neodymium-doped titanium niobate material and application thereof in a lithium ion battery, wherein the preparation method of the titanium niobate material comprises the following steps: dissolving a titanium source compound and oxalic acid in an organic solvent, heating, stirring and dissolving the niobium source compound and the oxalic acid in distilled water, and dissolving a neodymium-containing compound in dilute hydrochloric acid; mixing the three solutions prepared in the step one, and preparing a rare earth element neodymium-doped titanium niobate material precursor by a heating, stirring and evaporating solvent method or a solvothermal method; and thirdly, carrying out heat treatment on the precursor obtained in the second step, and obtaining the rare earth element neodymium-doped titanium niobate material with better electrochemical performance after the heat treatment. According to the invention, the rare earth element neodymium is used for doping and modifying the titanium niobate material, so that the unit cell size is increased, and the lithium ion conduction rate of the material is improved, thereby further improving the electrochemical performance of the titanium niobate, and further promoting the application of the titanium niobate in a lithium ion secondary battery.
Description
Technical Field
The invention belongs to the field of energy storage materials, and particularly relates to a preparation method and application of a rare earth element neodymium-doped titanium niobate material.
Background
The lithium ion battery is a chemical power supply with higher energy density at present, and plays a vital role in the development of the future energy field, the negative electrode material is one of the important components of the lithium ion battery, the cost of the negative electrode material accounts for more than 25% of the total cost of the battery, and the performance of the negative electrode material directly influences the performance and the production cost of the lithium ion battery. The traditional carbon material has small potential for further research due to low safety problem, low energy density and the like, and silicon and tin materials with high specific capacity still have some problems to be solved, while the lithium titanate (Li) which is a zero-strain material still has some problems to be solved4Ti5O12) The application of (a) is also limited by its lower theoretical capacity (175mAh/g), so a negative electrode with higher theoretical capacity and better cycling stability and rate capability is soughtThe material has great promotion effect on the lithium ion secondary battery.
2011, Goodenough group assigned TiNb2O7(TNO) is used as a lithium ion battery cathode material, and therefore the lithium ion battery cathode material with great potential enters the visual field of various scholars, and 3 pairs of redox couples (Nb) exist in the electrochemical reaction of the TNO5+/Nb4+，Nb4+/Nb3+，Ti4+/Ti3+) Corresponding to 5 electron transfers, the lithium niobate lithium ion battery provides 387.6mAh/g theoretical specific capacity which is more than twice of that of lithium titanate, the average potential of the lithium niobate lithium ion battery is 1.6V, the decomposition of electrolyte can be effectively prevented, the safety of the electrolyte is improved, in addition, the lithium niobate lithium ion battery also has good circulation stability, but the lithium niobate lithium ion battery also has some defects, such as low lithium ion conductivity and the like, so that the research on how to improve the lithium ion conductivity of the material is carried out, the electrochemical performance of the material is further improved, and the lithium niobate lithium ion battery has important significance for promoting the commercial application of the titanium niobate material.
Disclosure of Invention
The invention provides a preparation method and application of a rare earth element neodymium-doped titanium niobate material in order to further improve the ionic conductivity of the titanium niobate material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a rare earth element neodymium-doped titanium niobate material comprises the following steps:
the method comprises the following steps: dissolving a titanium source compound and oxalic acid in an organic solvent, and controlling the molar ratio of Ti to oxalic acid to be 1: 3-5, the concentration of titanium ions is 0.01-0.2 mol/L;
step two: dissolving a niobium source compound and oxalic acid in distilled water, and controlling the molar ratio of Nb to oxalic acid to be 1: 5-7, stirring and dissolving at 60-90 ℃, wherein the concentration of Nb ions is 0.02-0.3 mol/L;
step three: dissolving a neodymium compound containing rare earth elements in dilute hydrochloric acid;
step four: mixing the solutions obtained in the first step, the second step and the third step, and controlling the molar ratio of Ti to Nd to be 0.995-0.96: 0.005-0.04, heating, stirring and evaporating the solvent to prepare a neodymium-doped titanium niobate material precursor;
step five: calcining the precursor in a high-temperature furnace at 800-1400 ℃ for 10-20 h in air atmosphere to obtain the rare earth element neodymium-doped TiNb2O7A material.
The application of the rare earth element neodymium-doped titanium niobate material prepared by the method is that the neodymium-doped titanium niobate material is applied to a lithium ion battery as a negative electrode active substance.
Compared with the prior art, the invention has the beneficial effects that: the neodymium-doped TiNb prepared by the invention2O7When the material is used as a lithium ion battery cathode material, the material has higher reversible capacity, first-time efficiency, excellent charge and discharge performance and safety performance, and the synthesis method is simple, the raw materials are cheap, and the material has a wider application prospect. According to the invention, the rare earth element neodymium is used for doping and modifying the titanium niobate material, so that the unit cell size is increased, and the lithium ion conduction rate of the material is improved, thereby further improving the electrochemical performance of the titanium niobate, and further promoting the application of the titanium niobate in a lithium ion secondary battery.
Drawings
FIG. 1 is a graph of the Nd-doped TiNb obtained in example 12O7Material and TiNb2O7A material XRD spectrogram;
FIG. 2 is a graph of the Nd-doped TiNb obtained in example 12O7Scanning electron micrographs of the material;
FIG. 3 shows the Nd-doped TiNb obtained in example 12O7Three-time charging and discharging curve chart of the material at 0.1C;
FIG. 4 shows the Nd-doped TiNb obtained in example 12O71C long cycle test curve of the material;
FIG. 5 shows the Nd-doped TiNb obtained in example 12O7Material and TiNb2O7Material alternating current impedance spectrogram;
FIG. 6 shows the Nd-doped TiNb obtained in example 12O7Material and TiNb2O7Material Zre and omega-1/2And (5) a relational graph.
Detailed Description
The technical solution of the present invention is further described below with reference to the drawings and the embodiments, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention
The first embodiment is as follows: the embodiment describes a method for preparing a rare earth element neodymium-doped titanium niobate material, which comprises the following steps:
the method comprises the following steps: dissolving a titanium source compound and oxalic acid in an organic solvent, and controlling the molar ratio of Ti to oxalic acid to be 1: 3-5, the concentration of titanium ions is 0.01-0.2 mol/L;
step two: dissolving a niobium source compound and oxalic acid in distilled water, and controlling the molar ratio of Nb to oxalic acid to be 1: 5-7, stirring and dissolving at 60-90 ℃, wherein the concentration of Nb ions is 0.02-0.3 mol/L;
step three: dissolving a neodymium compound containing rare earth elements in dilute hydrochloric acid;
step four: mixing the solutions obtained in the first step, the second step and the third step, and controlling the molar ratio of Ti to Nd to be 0.995-0.96: 0.005 to 0.04, Nd: ti: the Nb molar ratio is x: 1-x: 2, heating, stirring and evaporating the solvent to prepare a neodymium-doped titanium niobate material precursor; the solvent evaporation method has no requirement on the concentration of the solution, and can be completely dissolved.
Step five: calcining the precursor in a high-temperature furnace at 800-1400 ℃ for 10-20 h in air atmosphere to obtain the rare earth element neodymium-doped TiNb2O7A material.
The second embodiment is as follows: in the first step of the method for preparing a rare earth element neodymium-doped titanium niobate material, the titanium source compound should be soluble in a selected organic solvent and non-reactive with the selected organic solvent, and may be one of tetrabutyl titanate, titanium isopropoxide or titanium tetrachloride.
The third concrete implementation mode: in the preparation method of the rare earth element neodymium-doped titanium niobate material of the first embodiment, in the first step, the organic solvent is miscible with water, and the titanium source and the oxalic acid can be dissolved in the organic solvent, and is one or a mixture of several of absolute ethyl alcohol, acetone or acetonitrile.
The fourth concrete implementation mode: in a second step of the preparation method of the rare earth element neodymium-doped titanium niobate material of the first embodiment, the niobium source compound should be soluble in an oxalic acid solution or soluble in an oxalic acid solution under heating, and may be one of niobium oxalate hydrate, niobium acid or niobium ethoxide.
The fifth concrete implementation mode: in a third step of the preparation method of the rare earth element neodymium-doped titanium niobate material according to the first embodiment, the compound containing the rare earth element neodymium is one of neodymium oxide, neodymium trichloride or neodymium nitrate. The titanium source, niobium source and neodymium compound are selected to be soluble in the solvent, and the organic solvent is selected to be miscible with water and non-reactive with the selected titanium source, niobium source and neodymium compound.
The sixth specific implementation mode: in the fourth step of the preparation method of the rare earth element neodymium-doped titanium niobate material, the temperature of the heating, stirring and solvent evaporation method is 40-90 ℃, and the solvent is evaporated until crystals are separated out.
The seventh embodiment: in a fifth step of the method for preparing a rare earth element neodymium-doped titanium niobate material, the high-temperature furnace is one of a tube furnace, a box furnace or a muffle furnace.
The specific implementation mode is eight: in a specific embodiment, the preparation method of the neodymium-doped titanium niobate material is not limited, and can be replaced by a ball milling method or a solvothermal method. The ball milling method is to mix oxides of Ti, Nb and Nd elements in proportion and then to prepare the alloy by high-speed ball milling. The solvothermal method is to dissolve the elements according to a similar method of steps one to three, and then to prepare the element in a sealed high-pressure reaction kettle by controlling the temperature and time.
The specific implementation method nine: the preparation method of the rare earth element neodymium-doped titanium niobate material comprises the fourth step, wherein the temperature of the solvothermal method is 120-200 ℃ and the time is 5-24 hours.
The detailed implementation mode is ten: the application of the rare earth element neodymium-doped titanium niobate material prepared by the method in any one of the first to ninth embodiments is to use the neodymium-doped titanium niobate material as a negative electrode active material in a lithium ion battery, wherein the lithium ion battery is composed of a positive electrode sheet, a negative electrode sheet, a diaphragm, electrolyte, an aluminum shell or an aluminum-plastic film, the specific combination mode is according to a conventional combination mode in the field, and the negative electrode sheet comprises copper foil and negative electrode slurry.
The concrete implementation mode eleven: in the application of the rare earth element neodymium-doped titanium niobate material in the embodiment, in the lithium ion battery, the negative electrode slurry is composed of 70-95% of neodymium-doped titanium niobate material, 2-10% of conductive agent and 3-20% of binder by mass percentage. The conductive agent is one or a mixture of several of acetylene black, graphene, Ketjen black, carbon nanotubes or Super P.
Example 1:
dissolving 0.8451g of tetrabutyl titanate and 1.2474g of oxalic acid dihydrate in 20mL of anhydrous ethanol, wherein the concentration of the tetrabutyl titanate is 0.125mol/L, adding 8.53mg of neodymium oxide into 5mL of distilled water, dropwise adding 1mol/L of dilute hydrochloric acid until the neodymium oxide is completely dissolved, dissolving 0.9025g of niobic acid and 3.78g of oxalic acid dihydrate in 50mL of distilled water, heating and stirring for dissolving at 90 ℃, wherein the concentration of the niobic acid is 0.101mol/L, adding the dissolved tetrabutyl titanate oxalic acid solution and the neodymium oxide hydrochloric acid solution after the solution is clarified, continuously stirring at 90 ℃, evaporating the solvent to obtain a precursor, placing the precursor in a tubular furnace after the precursor is ground to be fine, and carrying out heat treatment at 900 ℃ for 15h in the air atmosphere to obtain neodymium-doped TiNb2O7A material.
The titanium niobate material obtained in the embodiment can be used as a negative electrode material to be applied to assembling a button lithium ion battery, wherein the negative electrode slurry is composed of 80% of the titanium niobate material, 10% of a conductive agent and 10% of a binder in percentage by mass. As can be seen from FIG. 1, this embodiment can be seenTo neodymium-doped TiNb2O7Peak position of material portion compared to undoped TiNb2O7The material slightly moves to a small angle direction, which shows that the doped TiNb is2O7The size of the crystal lattice increases. Theoretical calculation shows that after 1 percent of Nb is doped, TiNb2O7The unit cell parameters a, b, c and beta are changed from 2.0351nm, 0.3801nm and 1.1882nm to 2.0785nm, 0.3780nm and 1.2400nm, and the increase of a and c axes is favorable for the diffusion of lithium ions in crystal lattices. As can be seen from FIG. 2, the Nd-doped TiNb obtained in this example2O7The material is formed by aggregating small particles with the diameter of about 200 nm. As can be seen from fig. 3, the first discharge capacity and the reversible capacity of the neodymium-doped titanium niobate material obtained in the present embodiment are 278.6 mAh/g and 262.6mAh/g, respectively, and the first coulombic efficiency reaches 94.26%. As can be seen from fig. 4, the neodymium-doped titanium niobate material obtained in the present embodiment has a first reversible capacity of 237.2mAh/g at a rate of 1C, and has a capacity retention rate of 73% after 500 cycles according to the original reversible capacity of 173.2 mAh/g. As can be seen from FIG. 5, the neodymium-doped TiNb2O7The charge transfer resistance of the material is reduced, and the real part of the impedance and omega in the low-frequency region in the impedance diagram are compared-1/2Plotting, the obtained result is shown in FIG. 6, and the calculation according to FIG. 6 shows that the TiNb is doped with the neodymium2O7The lithium ion diffusion coefficients of the material and the undoped titanium niobate material are respectively 1.01 multiplied by 10-15And 7.06X 10-16cm2And/s shows that the Nd doping improves the diffusion coefficient of lithium ions in the titanium niobate material.
Example 2:
the present embodiment is different from embodiment 1 in that: the tetrabutyl titanate in example 1 was replaced with titanium isopropoxide.
Example 3:
the present embodiment is different from embodiment 1 in that: the niobic acid in example 1 was replaced with niobium oxalate hydrate.
Example 4:
preparing an Nd doped material by a solvothermal method: 0.1752g of tetrabutyl titanate and 0.2810g of NbCl5Dissolving in 50mL of absolute ethyl alcohol, and stirring for 1 hour to obtain a solution I; 4.2mg of Nd2O3Adding intoIn 10mL of absolute ethyl alcohol, performing ultrasonic dispersion for 1 hour to obtain a suspension II, and controlling the Nd: ti: the Nb molar ratio is x: 1-x: 2; then mixing the solution I and the suspension II, stirring for 30min, and then ultrasonically dispersing for 1 hour; and then transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 24 hours at 180 ℃ in a homogeneous reactor, cooling to room temperature after the reaction is finished, then carrying out centrifugal separation at a rotating speed of 6000 rpm to obtain a white precursor, washing with absolute ethyl alcohol and distilled water for three times, carrying out vacuum drying at 80 ℃ for 10 hours, grinding, and calcining at 900 ℃ for 6 hours in an air atmosphere to obtain Nd-doped titanium niobate.
Example 5:
preparing an Nd doped material by a ball milling method: using a planetary ball mill, the mixing ratio was determined according to Nd: ti: the Nb molar ratio is x: 1-x: 2 weighing Nd with corresponding mass2O3、TiO2And Nb2O5Adding the mixture into a ball milling tank, adding a corresponding amount of zirconium balls according to a ball-to-material ratio of 1:10, adding a proper amount of n-hexane as a dispersing agent, ball milling for 20 hours at a rotating speed of 350 r/min, after the ball milling is finished, vacuum drying the obtained material for 10 hours at 80 ℃, and calcining the obtained material for 24 hours at 1100 ℃ in an air atmosphere after grinding to obtain Nd-doped titanium niobate.
Claims (11)
1. A preparation method of a rare earth element neodymium-doped titanium niobate material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dissolving a titanium source compound and oxalic acid in an organic solvent, and controlling the molar ratio of Ti to oxalic acid to be 1: 3-5, the concentration of titanium ions is 0.01-0.2 mol/L;
step two: dissolving a niobium source compound and oxalic acid in distilled water, and controlling the molar ratio of Nb to oxalic acid to be 1: 5-7, stirring and dissolving at 60-90 ℃, wherein the concentration of Nb ions is 0.02-0.3 mol/L;
step three: dissolving a neodymium compound containing rare earth elements in dilute hydrochloric acid;
step four: mixing the solutions obtained in the first step, the second step and the third step, and controlling the molar ratio of Ti to Nd to be 0.995-0.96: 0.005-0.04, heating, stirring and evaporating the solvent to prepare a neodymium-doped titanium niobate material precursor;
step five: calcining the precursor in a high-temperature furnace at 800-1400 ℃ for 10-20 h in air atmosphere to obtain the rare earth element neodymium-doped TiNb2O7A material.
2. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: in the first step, the titanium source compound is one of tetrabutyl titanate, titanium isopropoxide or titanium tetrachloride.
3. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: in the first step, the organic solvent is one or a mixture of more of absolute ethyl alcohol, acetone or acetonitrile.
4. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: in the second step, the niobium source compound is one of niobium oxalate hydrate, niobic acid or niobium ethoxide.
5. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: in the third step, the compound containing rare earth element neodymium is one of neodymium oxide, neodymium trichloride or neodymium nitrate.
6. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: in the fourth step, the temperature of the solvent heating, stirring and evaporating method is 40-90 ℃, and the solvent is evaporated until crystals are separated out.
7. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: and in the fifth step, the high-temperature furnace is one of a tube furnace, a box furnace or a muffle furnace.
8. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 1, characterized in that: the preparation method of the neodymium-doped titanium niobate material is replaced by a ball milling method and a solvothermal method.
9. The method for preparing a rare earth element neodymium-doped titanium niobate material according to claim 8, characterized in that: in the fourth step, the temperature of the solvothermal method is 120-200 ℃ and the time is 5-24 hours.
10. The application of the rare earth element neodymium-doped titanium niobate material prepared by the method of any one of claims 1 to 9 is characterized in that: the neodymium-doped titanium niobate material is used as a negative active material and applied to a lithium ion battery.
11. The use of a rare earth element neodymium-doped titanium niobate material according to claim 10, wherein: in the lithium ion battery, the negative electrode slurry is composed of 70-95% of neodymium-doped titanium niobate material, 2-10% of conductive agent and 3-20% of binder by mass percentage.
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| CN115043430A (en) * | 2022-05-26 | 2022-09-13 | 哈尔滨工业大学 | Preparation method and application of praseodymium-doped porous spherical titanium niobate material |
| CN115124081A (en) * | 2022-08-03 | 2022-09-30 | 安徽工业大学 | Method for preparing lithium ion battery embedded negative electrode material and material obtained by method |
| CN115744986A (en) * | 2022-11-30 | 2023-03-07 | 哈尔滨理工大学 | Preparation of titanium niobium oxide lithium ion battery cathode material based on high oxidation state ion doping |
| CN115849446A (en) * | 2022-11-16 | 2023-03-28 | 山东科技大学 | Copper-doped titanium niobate microsphere negative electrode material and preparation method and application thereof |
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| CN115043430B (en) * | 2022-05-26 | 2024-02-09 | 哈尔滨工业大学 | Preparation method and application of praseodymium-doped porous spherical titanium niobate material |
| CN115124081A (en) * | 2022-08-03 | 2022-09-30 | 安徽工业大学 | Method for preparing lithium ion battery embedded negative electrode material and material obtained by method |
| CN115124081B (en) * | 2022-08-03 | 2023-12-12 | 安徽工业大学 | Method for preparing lithium ion battery embedded cathode material and material obtained by method |
| CN115849446A (en) * | 2022-11-16 | 2023-03-28 | 山东科技大学 | Copper-doped titanium niobate microsphere negative electrode material and preparation method and application thereof |
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