CN111137923B - Preparation method of prismatic tantalum oxide nano material - Google Patents
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- CN111137923B CN111137923B CN202010009427.3A CN202010009427A CN111137923B CN 111137923 B CN111137923 B CN 111137923B CN 202010009427 A CN202010009427 A CN 202010009427A CN 111137923 B CN111137923 B CN 111137923B
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Abstract
The present invention provides a prismatic Ta 2 O 5 A preparation process of nano materials, belonging to the technical field of nano material preparation; in particular to (NH) 4 ) 2 Ta 2 O 3 F 6 A method of heat treatment of the precursor. The method is characterized in that: with (NH) 4 ) 2 Ta 2 O 3 F 6 Taking the material as a precursor, heating to 750-1500 ℃ at a heating rate of 1-10 ℃/min in an inert atmosphere, preserving heat for 0.5-5 hours, and cooling to prepare the Ta 2 O 5 And (4) nanorods. Ta prepared according to the invention 2 O 5 The material has the advantages of high length-diameter ratio, radial electron transport, high dielectric constant, good thermal stability, good chemical stability and the like. Simultaneously has the following advantages: the synthesis method is simple, the selected raw materials are easy to obtain, the experimental equipment is simple, the experimental period is short, and the process flow is easy to control. Prepared prismatic Ta 2 O 5 The material has good application prospect in the field of energy storage.
Description
Technical Field
The invention relates to a Ta 2 O 5 A process for preparing nano-rods, which belongs to the technical field of micron material preparation; in particular to 4 ) 2 Ta 2 O 3 F 6 A heat treatment method of a precursor.
Background
Electrochemical energy storage is used as a key supporting technology, and the future development prospect is extremely wide. The current world's constant energy consumption has led researchers to a wide research interest in energy storage technology, particularly electrochemical energy storage, especially lithium ion batteries, sodium ion batteries and potassium ion batteries with high energy density but relatively low power density. For the field of energy storage applications, there is still a pressing need for electrode architectures with high energy, high power, large capacity and good stability.
Ta 2 O 5 Belonging to an orthorhombic structure, wherein a =0.6180nm, b =4.0290nm, c =0.3888nm, α = β = γ =90 °. As an n-type wide bandgap semiconductor, the bandgap width is about 4.0eV, and the semiconductor has excellent dielectric and photoelectric properties. Ta 2 O 5 The material has high dielectric constant, good thermal stability and chemical stability, and has been widely applied in the field of photocatalytic hydrogen production. Further, Ta 2 O 5 Has high theoretical capacity of lithium (482 mAh -1 ) Far higher than the graphite electrode (the lithium capacity is 372 mAh.g) which is applied at present -1 ) (ii) a In addition, at Ta 2 O 5 The potential of lithium ions of the electrode for lithium intercalation and lithium deintercalation is 0.8-1.0V, so that the high working potential can effectively avoid potential safety hazards caused by the deposition of simple substance lithium on the surface of the cathode in the charging and discharging processes; the above characteristics promote Ta 2 O 5 The material becomes a potential cathode material in the field of energy storage. Pan et al, in the article "structural distributed Ta 2 O 5 A structurally disordered Ta is prepared in aerogel for high-rate and high-type Li-ion and Na-ion storage through surface redox prosthesis 2 O 5 Aerogel, 3D porous form aerogel have higher specific surface area, interconnect's passageway and layering porosity, are favorable to quick ion transmission, have strengthened pseudo-capacitance performance. Ta 2 O 5 The lithium storage and sodium storage show excellent performance; for example, at a current density of 5000 mA/g, the lithium storage amount and the sodium storage amount of the material are respectively 97 mAh/g and 43.7 mAh/g; also shows excellent cycling stability, and the lithium storage capacity of the material is not obviously reduced after 2000 cycles at the current density of 5000 mA/g.
Xia et al in the article "Oxygen-deficiency Ta 2 O 5 Preparing amorphous Ta on a Ta sheet substrate by a cathodic oxidation method and heat treatment 2 O 5 A nanoporous membrane. ResultsIndicating that the film had a surface area of about 480mAh.g -1 High lithium storage capacity of (2); and exhibits excellent cycling stability at a rate of 5C over 8000 cycles. This 3D nanoporous self-supporting Ta 2 O 5 Thin film electrodes provide a large reaction area and promote ion diffusion, and are well suited for fast and sustainable lithium ion storage.
Yuxin et al, supra Structure Ta 2 O 5 mesocrystals derived from (NH 4 ) 2 Ta 2 O 3 F 6 (NH) prepared by steam hydrolysis in mesocrystals with effective photocatalytic activity 4 ) 2 Ta 2 O 3 F 6 Calcining the nano-rod in air at 750-900 ℃ for 3 hours to successfully prepare the mesomorphic Ta 2 O 5 A nanosheet; the maximum photocatalytic hydrogen production rate is 11268.241 mu mol g -1 h -1 。
Ammonium fluorotantalate ((NH) 4 ) 2 Ta 2 O 3 F 6 ) Pnma space group, orthorhombic structure, where a =10.43 a, b =5.64 a, c =14.84 a, α = β = γ =90 °. Six O or F atoms surround one Ta atom. Ta (O, F) 6 The octahedral structures are connected to form a double sawtooth-shaped chain structure parallel to the b axis, and ammonium ions are positioned between the chains. Wherein the Ta element is Ta 5+ Exist in the form of (1). As a wide-band-gap semiconductor material, the band gap width is 4.40eV, the material has excellent photocatalytic performance, and the photocatalytic hydrogen production rate reaches 3341.39 mu mol g -1 h -1 。
The (NH) prepared by the hydrothermal method has high purity, no impurity and uniform appearance 4 ) 2 Ta 2 O 3 F 6 The rod-shaped material is taken as a precursor, and the prismatic Ta with high length-diameter ratio, radial electron transmission, high dielectric constant, good thermal stability and chemical stability can be prepared after heat treatment in an inert atmosphere 2 O 5 A nanomaterial; can be used as a cathode material with great potential and applied to the field of energy storage.
Disclosure of Invention
The object of the present invention is to provide a prismatic Ta 2 O 5 The preparation process of the nanometer material also provides a (NH) 4 ) 2 Ta 2 O 3 F 6 A heat treatment method of the material.
The technical scheme is as follows:
(1) preparation of (NH) 4 ) 2 Ta 2 O 3 F 6 The method of the material is as follows: the method is characterized in that metal tantalum powder, hydrofluoric acid with the mass fraction of 40%, analytically pure acetic acid, urea and deionized water are used as raw materials. The method comprises the following steps: (1) hydrofluoric acid and metal tantalum powder are mixed according to a molar ratio (3-12): 1, mixing, and fully stirring until the metal tantalum powder is dissolved; (2) deionized water and glacial acetic acid are mixed according to the volume ratio (0.17-6): 1, uniformly mixing; gradually dripping the acetic acid solution into the mixed solution obtained in the step (1) to obtain a milky mixed solution; (3) according to the molar ratio of (0.25-2) urea to metal tantalum powder: 1, weighing urea, adding the urea into the milky white solution system obtained in the step (2), and uniformly stirring. (4) Transferring the solution system into a lining of a hydrothermal reaction kettle, screwing down the reaction kettle, transferring the reaction kettle into a drying oven, heating to 160-210 ℃, and reacting for 3-48 hours; (5) after the reaction is finished, naturally cooling the reaction kettle to room temperature, then centrifugally separating the product to obtain white precipitate, repeatedly washing the white precipitate with ethanol and water, centrifuging until the filtrate is neutral, and finally drying to obtain white (NH) 4 ) 2 Ta 2 O 3 F 6 A material.
(2) By heat treatment (NH) 4 ) 2 Ta 2 O 3 F 6 Precursor preparation of Ta 2 O 5 The method of the nano-rod is as follows: prepared by hydrothermal method (NH4) 2 Ta 2 O 3 F 6 Taking the material as a precursor, and heating to 750-1500 ℃ at a heating rate of 1-10 ℃/min in an inert atmosphere (argon, oxygen-free atmosphere); and preserving heat for 30 minutes to 5 hours, and cooling to obtain Ta 2 O 5 A nanorod material.
The invention has the following advantages: synthetic Ta 2 O 5 The nano material has high specific surface area, high purity and uniform appearance;simple preparation method, easily obtained raw materials, simple experimental equipment, short experimental period, easy control of process flow and the like.
The working principle of the invention is as follows: (NH) 4 ) 2 Ta 2 O 3 F 6 Thermal decomposition to form Ta in high temperature inert atmosphere 2 O 5 While producing the F-containing compound and ammonia gas.
Drawings
FIG. 1 is a prismatic Ta prepared in example 1 2 O 5 XRD spectrum of the nano material.
FIG. 2 is a prismatic Ta prepared in example 1 2 O 5 SEM pictures of nanomaterials.
FIG. 3 is a prismatic Ta prepared in example 2 2 O 5 XRD spectrum of the nano material.
FIG. 4 is a prismatic Ta prepared in example 2 2 O 5 SEM pictures of nanomaterials.
FIG. 5 is a prismatic Ta prepared in example 3 2 O 5 XRD spectrum of the nano material.
FIG. 6 is a prismatic Ta prepared in example 4 2 O 5 XRD spectrogram of the nanometer material.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
Example 1:
ta is obtained in this embodiment 2 O 5 The preparation process of the nano-rod comprises the following steps: (NH) to be prepared by a hydrothermal method 4 ) 2 Ta 2 O 3 F 6 The nano material is taken as a precursor, and is heated to 800 ℃ at the heating rate of 5 ℃/min for 2 hours under the atmosphere of argon (inert atmosphere, oxygen-free); cooling with the furnace to obtain prismatic Ta 2 O 5 A nano-material.
(NH) used in this example 4 ) 2 Ta 2 O 3 F 6 The preparation method of the precursor comprises the following steps:the method takes metal tantalum powder, hydrofluoric acid with the mass fraction of 40%, analytically pure acetic acid, urea and deionized water as raw materials. The method comprises the following steps: (1) hydrofluoric acid and metal tantalum powder are mixed according to a molar ratio (3-12): 1, mixing, and fully stirring until the metal tantalum powder is dissolved; (2) deionized water and glacial acetic acid are mixed according to the volume ratio (0.17-6): 1, uniformly mixing; gradually dripping the acetic acid solution into the mixed solution obtained in the step (1) to obtain a milky mixed solution; (3) according to the molar ratio of (0.25-2) urea to metal tantalum powder: 1, weighing urea, adding the urea into the milky white solution system obtained in the step (2), and uniformly stirring. (4) Transferring the solution system into a lining of a hydrothermal reaction kettle, screwing down the reaction kettle, transferring the reaction kettle into a drying oven, heating to 160-210 ℃, and reacting for 3-48 hours; (5) after the reaction is finished, naturally cooling the reaction kettle to room temperature, then centrifugally separating the product to obtain white precipitate, repeatedly washing the white precipitate with ethanol and water, centrifuging until the filtrate is neutral, and finally drying to obtain white (NH) 4 ) 2 Ta 2 O 3 F 6 A material.
The prepared prismatic Ta 2 O 5 The powder was subjected to X-ray diffraction phase analysis (XRD), and the XRD pattern obtained was as shown in FIG. 1. Its main characteristic peak can be combined with Ta 2 O 5 (JCPDS Card number 79-1375) shows that calcination (NH) was performed at 800 ℃ under an argon atmosphere 4 ) 2 Ta 2 O 3 F 6 Precursor is insulated for 2h, thus successfully preparing orthorhombic Ta 2 O 5 . In addition, the diffraction peak of XRD is very sharp, which indicates that the sample is single-phase, high-purity and has almost no other crystal impurity phase.
FIG. 2 is Ta prepared 2 O 5 Scanning Electron Microscope (SEM) images of the material. The results show that Ta produced 2 O 5 The material has a prismatic structure, the length is about 2-4 mu m, and the width is about 250-550 nm; the length-diameter ratio can reach 4-16. FIG. 2(b) shows a prismatic Ta 2 O 5 The edges and corners of the nano material are clear, and the surface is relatively smooth and compact.
Example 2:
this implementationExample (NH) to be prepared by hydrothermal method in contrast to example 1 4 ) 2 Ta 2 O 3 F 6 The powder is used as a precursor; under the condition of argon (inert atmosphere, oxygen-free) atmosphere, raising the temperature to 1000 ℃ at the temperature rise rate of 5 ℃/min, and preserving the heat for 2 hours; cooling with the furnace to obtain prismatic Ta 2 O 5 A nanomaterial; the rest is the same as in example 1.
The prepared prismatic Ta 2 O 5 The powder was subjected to X-ray diffraction phase analysis (XRD) and the XRD pattern obtained was as shown in FIG. 3. Its main characteristic peak can be combined with Ta 2 O 5 The diffraction peaks of (JCPDS Card number 79-1375) coincide. Furthermore, the diffraction results of XRD showed that the prepared prismatic Ta was 2 O 5 Is single-phase, high-purity and almost free of other crystal impurity phases.
FIG. 4 is Ta prepared 2 O 5 Scanning Electron Microscope (SEM) images of the material. The results show that Ta prepared 2 O 5 The material has a prismatic structure, the length is about 0.5-1 μm, the width is about 250-450 nm (as shown in figure 4 (a)), and the length-diameter ratio can reach 2-4. FIG. 4(b) shows a prismatic Ta 2 O 5 The surface of the material is relatively smooth and compact.
Example 3:
this example differs from example 1 in that (NH) is to be prepared by a hydrothermal process 4 ) 2 Ta 2 O 3 F 6 The powder is used as a precursor; under the condition of argon (inert atmosphere, oxygen-free) atmosphere, raising the temperature to 1200 ℃ at the temperature rise rate of 5 ℃/min, and preserving the heat for 2 hours; cooling with the furnace to obtain prismatic Ta 2 O 5 A nanomaterial; the rest is the same as in example 1.
Ta to be prepared 2 O 5 The powder was subjected to X-ray diffraction phase analysis (XRD) and the XRD pattern obtained was as shown in FIG. 5. Its main characteristic peak can be combined with Ta 2 O 5 (JCPDS Card number 79-1375) shows a coincidence of diffraction peaks, indicating that calcination (NH) was performed in an Ar atmosphere at 1200 ℃ 4 ) 2 Ta 2 O 3 F 6 The precursor is kept warm for 2h, and then Ta can be successfully prepared 2 O 5 . In addition, the diffraction results of XRD showed Ta produced 2 O 5 Is single-phase, high-purity and almost free of other crystal impurity phases.
Example 4:
this example differs from example 1 in that (NH) is to be prepared by a hydrothermal process 4 ) 2 Ta 2 O 3 F 6 The powder is used as a precursor; under the condition of argon (inert atmosphere, oxygen-free) atmosphere, raising the temperature to 1400 ℃ at the temperature rise rate of 5 ℃/min, and preserving the heat for 2 hours; cooling with the furnace to obtain prismatic Ta 2 O 5 A nanomaterial; the rest is the same as in example 1.
Ta to be prepared 2 O 5 The powder was subjected to X-ray diffraction phase analysis (XRD), and the XRD pattern obtained was as shown in FIG. 6. Its main characteristic peak can be combined with Ta 2 O 5 The diffraction peaks of (JCPDS Card number 79-1375) coincide. In addition, the diffraction results of XRD showed Ta produced 2 O 5 Is single-phase, high-purity and almost free of other crystal impurity phases.
Example 5:
this example differs from example 1 in that (NH) is to be prepared by a hydrothermal process 4 ) 2 Ta 2 O 3 F 6 The powder is used as a precursor; under the atmosphere of argon (inert atmosphere and without oxygen), the temperature is raised to 750 ℃ at the heating rate of 1 ℃/min and is preserved for 5 hours; cooling with the furnace to obtain prismatic Ta 2 O 5 A nanomaterial; the rest is the same as in example 1.
Example 6:
this example differs from example 1 in that (NH) is to be prepared by a hydrothermal process 4 ) 2 Ta 2 O 3 F 6 The powder is used as a precursor; under the condition of argon (inert atmosphere, oxygen-free) atmosphere, raising the temperature to 1500 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 0.5 hour; cooling with the furnace to obtain prismatic Ta 2 O 5 A nanomaterial; the rest is the same as in example 1.
Claims (1)
1. Prismatic Ta 2 O 5 The preparation method of the nano material is characterized by comprising the following steps: rod-shaped (NH) prepared by hydrothermal method 4 ) 2 Ta 2 O 3 F 6 Taking the nano material as a precursor, heating to 750-1500 ℃ at a heating rate of 1-10 ℃/min in an inert atmosphere, preserving heat for 0.5-5 hours, and cooling to obtain the Ta with a prismatic shape 2 O 5 A nanomaterial; said (NH) 4 ) 2 Ta 2 O 3 F 6 The precursor preparation method comprises the following steps: the method takes metal tantalum powder, hydrofluoric acid with the mass fraction of 40%, analytically pure acetic acid, urea and deionized water as raw materials, and comprises the following steps: (1) hydrofluoric acid and metal tantalum powder are mixed according to a molar ratio (3-12): 1, mixing, and fully stirring until the metal tantalum powder is dissolved; (2) deionized water and glacial acetic acid are mixed according to the volume ratio (0.17-6): 1, uniformly mixing; gradually dripping the acetic acid solution into the mixed solution obtained in the step (1) to obtain a milky mixed solution; (3) according to the molar ratio of (0.25-2) urea to metal tantalum powder: 1, weighing urea, adding the urea into the milky white solution system obtained in the step (2), and uniformly stirring; (4) transferring the solution system into a lining of a hydrothermal reaction kettle, screwing down the reaction kettle, transferring the reaction kettle into a drying oven, heating to 160-210 ℃, and reacting for 3-48 hours; (5) after the reaction is finished, naturally cooling the reaction kettle to room temperature, then centrifugally separating the product to obtain white precipitate, repeatedly washing the white precipitate with ethanol and water, centrifuging until the filtrate is neutral, and finally drying to obtain white (NH) 4 ) 2 Ta 2 O 3 F 6 A material.
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| CN111924880A (en) * | 2020-07-20 | 2020-11-13 | 山东理工大学 | Preparation method of carbon-coated tantalum pentoxide nanosheet |
| CN111905772A (en) * | 2020-07-27 | 2020-11-10 | 山东理工大学 | Preparation method of carbon-coated tantalum oxyfluoride nanosheet |
| US20240002250A1 (en) * | 2020-12-07 | 2024-01-04 | Dic Corporation | Tantalum oxide particle and method for producing tantalum oxide particle |
| CN114351239B (en) * | 2021-12-15 | 2024-05-17 | 中国科学院金属研究所 | Preparation method of porous metal compound array film |
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