CN110911666A - Method for synthesizing nitrogen-containing carbon-coated titanium niobate material for negative electrode of lithium battery - Google Patents
Method for synthesizing nitrogen-containing carbon-coated titanium niobate material for negative electrode of lithium battery Download PDFInfo
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Abstract
The invention relates to a method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a lithium battery cathode, which comprises the following operations: mixing TiNb2O7And putting PVP (polyvinyl pyrrolidone) and the alcohol solvent into the alcohol solvent to prepare solution A, mixing the zinc nitrate alcohol solution and the 2-methylimidazole alcohol solution to react to obtain solution B, mixing the A, B solutions to perform a coating reaction, recovering a precipitate after the coating reaction is finished, purifying to obtain an intermediate product A, calcining the intermediate product A, and calcining to obtain the nitrogen-containing carbon-coated titanium niobate material. TiNb by selecting high nitrogen content metal organic frame compound pair2O7Coating to form nitrogen-containing carbon packetCoated titanium niobate composite material. On one hand, the porous structure is beneficial to the insertion and extraction of lithium ions, and the volume expansion effect can be effectively relieved; on the other hand, the nitrogen-containing carbon in the sample can improve the conductivity of the electrode material, thereby realizing the requirements of quick charge and discharge and prolonging the service life, and making up for the lower conductivity and the lower lithium ion diffusion coefficient of the titanium niobate. In addition, when the carbon material containing nitrogen is used as the composite material substrate, the lithium storage capacity of the electrode material can be additionally improved.
Description
Technical Field
The invention relates to the field of synthesis of lithium battery materials, in particular to a method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a lithium battery cathode.
Background
With the increasing social demand for battery-type energy, the traditional graphite material battery can not meet the requirements. Therefore, it is necessary to research a next-generation new material having high specific capacity, excellent rate property, long cycle stability and excellent safety, which is expected to replace a graphite electrode. Among the potential materials, titanium niobate (TiNb) with unique structure2O7) The material completely exposes the head corner, because of the structural characteristics, at least four lithium ions can be inserted, and the lattice parameter, the unit cell volume and the lattice volume change are very small, so that the material is very suitable for lithium ion extraction, and the material brings excellent lithium transmission performance and good working stability for the TNO material. On the way of the development and popularization of TNO material lithium batteries, the defects of poor conductivity and low capacity are the key of the TNO material lithium batteries, and the problems need to be solved urgently.
The titanium niobate has the characteristics of high theoretical specific capacity of 388 mAh/g, high working potential (1.0-2.0V), excellent charge and discharge capacity, no SEI film and the like, and is considered to be one of potential negative electrode materials of secondary lithium batteries. However, the lower conductivity and the lower lithium ion diffusion coefficient of the titanium niobate influence the release of the capacity of the active material in the negative electrode material; the solid phase method is generally adopted, the particle size is larger, and the lithium ion transmission and electrochemical reaction areas are smaller; the raw materials niobium source and titanium source are easy to hydrolyze, and the controllability of the chemical reaction process is not high; the working potential is higher and the matched high-potential anode material is lacked. Therefore, a conductive phase, bulk phase doping and nano-structure of the material can be formed on the surface of the titanium niobate, so that the surface area is increased while the conductivity is improved, the electronic conductivity and the ion transmission rate are improved, and better electrochemical properties are obtained.
Disclosure of Invention
The invention aims to provide a method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a lithium battery negative electrode.
The technical scheme adopted by the invention is as follows.
A method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a negative electrode of a lithium battery comprises the following operations: mixing TiNb2O7And putting PVP (polyvinyl pyrrolidone) and the alcohol solvent into the alcohol solvent to prepare solution A, mixing the zinc nitrate alcohol solution and the 2-methylimidazole alcohol solution to react to obtain solution B, mixing the A, B solutions to perform a coating reaction, recovering a precipitate after the coating reaction is finished, purifying to obtain an intermediate product A, calcining the intermediate product A, and calcining to obtain the nitrogen-containing carbon-coated titanium niobate material.
Further, TiNb2O7The method comprises the following steps: dissolving TBOT and DETA in an alcohol solvent to obtain a solution C, uniformly mixing niobium chloride alcohol solution and the solution C, carrying out heat preservation reaction, recovering a precipitate after the heat preservation reaction is finished, carrying out purification treatment to obtain an intermediate product B, calcining the intermediate product B, and preparing the spherical TiNb after the calcining treatment is finished2O7。
Specifically, the method comprises the following steps: TiNb in solution A2O7The mass ratio to PVP was 4: 3.
The molar ratio of the zinc nitrate to the 2-methylimidazole in the solution B is 1: 2.8.
The molar ratio of TBOT to DETA in solution C was 3.17: 1.
And (3) adding the niobium chloride alcoholic solution and the solution C according to the molar ratio of TBOT to niobium pentachloride of 1:1.6 carrying out a mixing reaction.
The temperature for calcining the intermediate product A is 800 ℃, the calcining treatment is carried out for 3h, and the calcining treatment is carried out in the nitrogen atmosphere.
The temperature of calcining the intermediate product B is 700 ℃, the calcining treatment is carried out for 2h, and the calcining treatment is carried out in the oxygen-enriched atmosphere.
The detailed scheme is as follows: 0.200g of TiNb2O7Adding the mixture into a conical flask containing 40ml of methanol, adding 0.150g of PVP powder to obtain solution A, dissolving 0.302g of zinc nitrate hexahydrate in 15ml of methanol, simultaneously dissolving 0.232g of 2-methylimidazole in 15ml of methanol, then adding the 2-methylimidazole solution into the zinc nitrate solution, reacting for 30 minutes to obtain solution B, adding the solution A into the solution B, stirring and reacting for 6 hours, standing for 12 hours, centrifuging to obtain a white precipitate, repeatedly washing with methanol, washing off unreacted 2-methylimidazole, drying in vacuum to obtain an intermediate product A, transferring the intermediate product A into a muffle furnace, and calcining to obtain the nitrogen-containing carbon-coated titanium niobate material.
Dissolving 0.380g of niobium pentachloride in 10ml of ethanol, performing ultrasonic oscillation for 20min to prepare a niobium chloride alcoholic solution, dissolving 0.300g of tetrabutyl titanate and DETA in 20ml of isopropanol, performing ultrasonic oscillation for 20min to prepare a solution C, mixing the niobium chloride alcoholic solution and the solution C, placing the mixture in a stainless steel reaction kettle with a polytetrafluoroethylene lining, stirring for 1 hour, sealing the reaction kettle, placing the reaction kettle in an oven for reaction at 200 ℃ for 12 hours to obtain an intermediate product B, drying the intermediate product B in a vacuum environment, transferring the intermediate product B into a muffle furnace, and performing calcination treatment in an air atmosphere to obtain the spherical TiNb2O7。
The invention has the technical effects that:
selecting high nitrogen content metal organic frame compound pair TiNb2O7Coating to form the nitrogen-containing carbon-coated titanium niobate composite material. On one hand, the porous structure is beneficial to the insertion and extraction of lithium ions, and the volume expansion effect can be effectively relieved; on the other hand, the nitrogen-containing carbon in the sample can improve the conductivity of the electrode material, thereby realizing the requirements of quick charge and discharge and prolonging the service life, and making up for the lower conductivity and the lower lithium ion diffusion coefficient of the titanium niobate. In addition, when the carbon material containing nitrogen is used as the composite material substrate, the lithium storage capacity of the electrode material can be additionally improved.
In addition, the technical proposal adopts NbCl through a solvothermal method5TBOT is taken as a raw material, DETA is taken as a surfactant, the pH value of the solution is adjusted, the reaction rate of the hydrolysis reaction of niobium ethoxide and TBOT is slowed down, and the spherical porous TiNb is successfully prepared2O7The nanometer material is prepared, a metal organic framework material ZIF-8 is successfully grown around the titanium niobate material, and central ion zinc ions and organic ligands of the ZIF-8 are volatilized through high-temperature calcination, so that the nitrogen-containing carbon-coated titanium niobate material is obtained, and the process is novel. Nitrogen-containing carbon-coated TiNb2O7Electrode negative electrode material, and pure TiNb2O7Compared with the negative electrode material, the specific capacity of the battery is greatly improved, and the conductivity of the battery is also greatly improved. The invention has simple synthetic process and is used for synthesizing the porous TiNb with fixed morphology2O7The material and its carbon-coated composite provide a new path.
Drawings
FIG. 1 is a schematic view of a preparation process.
FIG. 2 is an X-ray diffraction pattern of the synthesized titanium niobate material.
FIG. 3 is an XRD pattern of the synthesized TNO/N-C material.
FIG. 4 is a scanning electron micrograph of the synthesized sample: a. pure TiNb2O74500 times magnified scanning electron micrograph of the crystal; b. pure TiNb2O7A scanning electron microscope image of local magnification of the crystal; c. scanning electron microscope images of the synthesized TNO @ N-C material; d. and (3) a local magnified scanning electron microscope image of the synthesized TNO @ N-C material.
FIG. 5 is a mapping image of an EDS energy spectrum scan: a) the surface scanning range of the TNO/N-C material b) a Ti element distribution diagram; c) a distribution diagram of Nb element; d) c element distribution diagram.
FIG. 6 is TiNb2O7Powder image.
FIG. 7 is TiNb2O7N-C powder image.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the following description is given in conjunction with the accompanying examples. It is to be understood that the following text is merely illustrative of one or more specific embodiments of the invention and does not strictly limit the scope of the invention as specifically claimed.
The reagents and procedures used in the present invention are understood in accordance with the conventional concepts of the art, unless otherwise specified.
Example 1 titanium niobate TiNb2O7Synthesis of (2)
The titanium source is tetrabutyl titanate (C)16H36O4Ti) 0.300g, tetrabutyl titanate and DETA (300 um) dissolved in 20ml of isopropanol and then sonicated for 20 min. 0.380g of NbCl5Dissolving in 10ml ethanol, ultrasonically oscillating for 20min to obtain niobium ethoxide, mixing the two solutions in a polytetrafluoroethylene reactor, stirring with magnetons for 1 h (300 r/min), sealing the reaction kettle, and placing in an oven for heat preservation at 200 ℃ for 12h to obtain a light yellow precipitate. Washing with ethanol for several times, centrifuging to obtain dried product, calcining the dried product in muffle furnace at 700 deg.C (temperature increase rate of 5 deg.C/min) for 2 hr to obtain 0.325g of pale yellow TiNb powder2O7(FIG. 6).
Example 2 TiNb2O7Synthesis method of/N-C composite material
0.200g of the product obtained in example 1 was put into a conical flask containing 40ml of methanol, 0.150g of PVP powder was added, a magneton was placed, the bottle mouth was sealed with a sealing film, and the product was activated for 12 hours by magnetic stirring (300 r/min) and was used. Dissolving 0.302g of zinc nitrate hexahydrate in 15ml of methanol, simultaneously dissolving 0.232g of 2-methylimidazole in 15ml of methanol, then adding the 2-methylimidazole solution into the zinc nitrate solution, adding the activated PVP suspension of titanium niobate into the zinc nitrate solution when the reaction is carried out for 30 minutes, stirring at a low speed for reaction for 6 hours, standing for 12 hours, centrifuging to obtain white precipitate, repeatedly washing for 3 times by using methanol, washing out unreacted 2-methylimidazole, drying in vacuum, transferring into a muffle furnace, calcining for 3 hours at 800 ℃ (the heating rate of 4 ℃/min) in a nitrogen thermal environment, wherein the product is grey powder TiNb2O7N-C (FIG. 7). The operation flow is shown in fig. 1.
Example 3
The products obtained in examples 1-2 were tested, and the results are shown in Table 1 and FIGS. 2-5.
As can be seen from the X-ray diffraction pattern (FIG. 2), the XRD pattern of the prepared pale yellow powder sample prepared in example 1 substantially coincides with the simulated XRD pattern of the crystal data of the standard substance, and the position and shape of the diffraction peak substantially coincide with those of TiNb2O7The standard cards are completely consistent, which shows that the molecular formula of the titanium niobate of the prepared material is TiNb2O7。
As can be seen from FIG. 3, TiNb synthesized by the present invention2O7N-C with pure TiNb2O7Compared with the crystal by XRD, the TNO/N-C material is a carbon material containing nitrogen formed by growing a layer of ZIF-8 metal organic framework material on the surface of titanium niobate and carrying out high-temperature heat treatment on the titanium niobate. As the nitrogen-containing carbon presents a steamed bread peak near 26 degrees, the XRD peaks of the two materials are superimposed. With pure TiNb2O7Compared with TNO/N-C material, the XRD peak height of the TNO/N-C material is reduced sharply to a certain extent at about 26 degrees. The results fully show that the composite material does not contain a diffraction peak of ZIF-8 crystal any more, and only contains TiNb2O7And a nitrogen-containing carbon phase.
The TEM image (FIG. 4) shows that the sample obtained by the present invention, pure TiNb2O7The crystals are regularly spherical, the particle sizes are different, and the average size is about 3 microns. From the b diagram, it can be seen that TiNb2O7The crystal is spherical and has smooth surface. When in TiNb2O7After a layer of nitrogen-containing carbon material is wrapped around the crystal, as shown in figure c, the sphere is wrapped around by nitrogen-containing carbon, and an irregular porous surface structure is shown, which indicates that TiNb is coated on the surface of the TiNb2O7A layer of nitrogen-containing carbon material was successfully coated around the crystals.
As is clear from FIG. 5 and Table 1, TiNb obtained by the present invention2O7The sample, the wrapped single crystal was analyzed and tested by an energy spectrometer (EDS) of an electron scanning microscope. Single nitrogen-containing carbon-coated TiNb2O7The results of crystal surface scanning showed that the TNO/N-C material contained Ti, Nb, C and O (corresponding to 5(b), 5(C) and 5(d), respectively). Also, the elemental weight and atomic distribution analyzed by the EDS spectrometer illustrate this result, see table 1. Wherein the carbon element is 16.85 percent, and the zinc element in the ZIF-8 is not shown, which indicates that the zinc can be completely volatilized at 800 ℃ by the ZIF-8 crystal and is completely decomposed into nitrogen-containing carbon.
TABLE 1 EDS spectrometer analysis of elemental weight and atomic distribution
| Element(s) | Weight (%) | Atom (%) |
| C K | 7.91 | 16.85 |
| O K | 37.16 | 59.39 |
| N K | 9.88 | 9.00 |
| Ti K | 10.09 | 5.14 |
| Nb L | 34.96 | 9.62 |
| Total amount of | 100.00 | 100.00 |
In order to improve the specific capacity and conductivity of titanium niobate by utilizing the fast-charging material, namely titanium niobate in the field of lithium ion batteries, porous nitrogen-containing MOF material is grown around the titanium niobate material, and ZIF-8 around the titanium niobate is decomposed into nitrogen-containing carbon through heat treatment under certain conditions, so that the nitrogen-containing carbon-coated titanium niobate porous composite material is formed. Preparing spherical porous TiNb by solvothermal method2O7Nano material, then using carbon nitrogen to wrap said nano material to improve TiNb2O7The nano material and untreated materials in the same batch are respectively assembled into a battery to carry out a series of characterization and performance comparison, the influence of the structure of the anode material of the lithium battery on the battery performance is revealed, the porous structure is clarified to be beneficial to the insertion and extraction of lithium ions, and the TiNb is improved2O7The specific capacity of the electrode material and the conductivity thereof are improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.
Claims (10)
1. A method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a negative electrode of a lithium battery comprises the following operations: mixing TiNb2O7And putting PVP (polyvinyl pyrrolidone) and the alcohol solvent into the alcohol solvent to prepare solution A, mixing the zinc nitrate alcohol solution and the 2-methylimidazole alcohol solution to react to obtain solution B, mixing the A, B solutions to perform a coating reaction, recovering a precipitate after the coating reaction is finished, purifying to obtain an intermediate product A, calcining the intermediate product A, and calcining to obtain the nitrogen-containing carbon-coated titanium niobate material.
2. The method of claim 1, wherein the TiNb is added to the titanium niobate-coated material to form a negative electrode for a lithium battery2O7The method comprises the following steps: dissolving TBOT and DETA in an alcohol solvent to obtain a solution C, uniformly mixing niobium chloride alcohol solution and the solution C, carrying out heat preservation reaction, recovering a precipitate after the heat preservation reaction is finished, carrying out purification treatment to obtain an intermediate product B, calcining the intermediate product B, and preparing the spherical TiNb after the calcining treatment is finished2O7。
3. The method of claim 1, wherein the TiNb solution is TiNb2O7The mass ratio to PVP was 4: 3.
4. The method for synthesizing the nitrogen-containing carbon-coated titanium niobate material for a negative electrode of a lithium battery as claimed in claim 1, wherein the molar ratio of zinc nitrate to 2-methylimidazole in the solution B is 1: 2.8.
5. The method for synthesizing the nitrogen-containing carbon-coated titanium niobate material for the negative electrode of the lithium battery as claimed in claim 2, wherein the molar ratio of TBOT to DETA in the C solution is 3.17: 1.
6. The method for synthesizing the nitrogen-containing carbon-coated titanium niobate material for the negative electrode of the lithium battery as claimed in claim 2, wherein the niobium chloride alcoholic solution and the solution C are subjected to a mixing reaction in a molar ratio of TBOT to niobium pentachloride of 1: 1.6.
7. The method for synthesizing a nitrogen-containing carbon-coated titanium niobate material for a negative electrode of a lithium battery as claimed in claim 1, wherein the temperature at which the intermediate product a is subjected to the calcination treatment is 800 ℃ for 3 hours, and the calcination treatment is performed in a nitrogen atmosphere.
8. The method for synthesizing the nitrogen-containing carbon-coated titanium niobate material for a negative electrode of a lithium battery as claimed in claim 2, wherein the temperature of the calcination treatment of the intermediate product B is 700 ℃ and the calcination treatment is carried out for 2 hours, and the calcination treatment is carried out in an oxygen-rich atmosphere.
9. The method of claim 1, wherein 0.200g of TiNb is added2O7Adding the mixture into a conical flask containing 40ml of methanol, adding 0.150g of PVP powder to obtain solution A, dissolving 0.302g of zinc nitrate hexahydrate in 15ml of methanol, simultaneously dissolving 0.232g of 2-methylimidazole in 15ml of methanol, then adding the 2-methylimidazole solution into the zinc nitrate solution, reacting for 30 minutes to obtain solution B, adding the solution A into the solution B, stirring and reacting for 6 hours, standing for 12 hours, centrifuging to obtain a white precipitate, repeatedly washing with methanol, washing off unreacted 2-methylimidazole, drying in vacuum to obtain an intermediate product A, transferring the intermediate product A into a muffle furnace, and calcining to obtain the nitrogen-containing carbon-coated titanium niobate material.
10. The method for synthesizing the nitrogen-containing carbon-coated titanium niobate material for the negative electrode of the lithium battery as claimed in claim 9, wherein the method comprises the steps of dissolving 0.380g of niobium pentachloride in 10ml of ethanol, performing ultrasonic oscillation for 20min to obtain a niobium chloride alcoholic solution, dissolving 0.300g of tetrabutyl titanate and DETA in 20ml of isopropanol, performing ultrasonic oscillation for 20min to obtain a solution C, mixing the niobium chloride alcoholic solution and the solution C, placing the mixture in a stainless steel reaction kettle with a polytetrafluoroethylene lining, stirring for 1 hour, sealing the reaction kettle, placing the reaction kettle in an oven at 200 ℃ for reaction for 12h to obtain an intermediate product B, drying the intermediate product B in a vacuum environment, transferring the reaction kettle into a muffle furnace, and performing calcination treatment in an air atmosphere to obtain the spherical TiNb material2O7。
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