CN112830516A - Preparation method of porous orthorhombic niobium pentoxide nano material - Google Patents
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Abstract
The invention discloses a preparation method of a porous orthorhombic niobium pentoxide nano material, belonging to the technical field of controllable preparation of metal oxide nano materials and shape control of the metal oxide nano materials. According to the invention, niobium salt is used as a raw material, and the solvothermal reaction is carried out in different solvents to synthesize the orthorhombic niobium pentoxide nanosheets and nanoflowers with good two-dimensional flaky morphology, porous distribution and excellent electrochemical performance. The preparation method has the advantages of simple equipment, convenient operation, controllable appearance, good repeatability, low cost and easy process amplification. The prepared product has uniform appearance, good crystal form, strong controllability, high quality and good performance, and can be widely applied to various fields of batteries, supercapacitors, catalysis and the like. Particularly, as a negative electrode material of a lithium ion battery, the orthorhombic niobium pentoxide two-dimensional nano material has the advantages of high capacity, high multiplying power and long cycle life.
Description
Technical Field
The invention belongs to the technical field of controllable preparation and shape control of metal oxide nano materials, and particularly relates to a preparation method of porous orthorhombic niobium pentoxide nanosheets and nanoflowers. The obtained porous orthorhombic niobium pentoxide nanosheets and nanoflowers show excellent electrochemical performance and can be widely applied to the fields of supercapacitors, batteries, catalysis and the like.
Background
Niobium pentoxide (Nb)2O5) As an important metal oxide material, the material has excellent physical and chemical properties and is widely applied to the fields of photoelectrocatalysis, supercapacitors, lithium ion/sodium ion batteries, sensors and the like. Wherein the niobium pentoxide (T-Nb) is in an orthogonal phase2O5) The lithium ion battery has large interlayer spacing, can provide an effective channel for ion migration, stores a large amount of lithium ions, and has a constant structure, thereby showing high lithium storage capacity and structural stability. And, Nb2O5Has high intercalation/deintercalation lithium potential (1.4-1.8V vs. Li/Li)+) The lithium ion battery does not cause generation of lithium dendrite and a Solid Electrolyte Interface (SEI) film, and is good in safety. Thus, T-Nb2O5Has become a negative electrode material which is concerned with, and is applied to lithium ion batteries and lithium ion capacitors. In particular, Nb2O5The two-dimensional nano material has larger surface area and more exposed atoms, and can provide more electrochemical energy storage sites; meanwhile, the open nano-sheet layer gap is beneficial to the embedding and the separation of electrolyte ions, and the electrochemical performance of the electrode material can be obviously improved. Thus, Nb2O5The nano sheet becomes one of the research focus and the main development direction of the key negative electrode material in recent years.
Prior preparation of Nb2O5The methods of nanoplatelets are relatively few. Chinese patent CN 104852015A reports a preparation method of a niobium pentoxide nanosheet composite material, which takes soluble niobium salt as a raw material to carry out heating reaction in a mixed solvent of deionized water and ethylenediamine to prepare the niobium pentoxide nanosheet. Another chinese patent CN 105381813 a reports a preparation method of carbon and nitrogen doped niobium pentoxide nanosheet, which comprises the steps of solvothermal reaction and high-temperature calcination of a soluble niobium salt raw material, absolute ethyl alcohol as a solvent, and organic ammonium hydroxide as a precipitant and a template agent to obtain the niobium pentoxide nanosheet. In addition, alsoThe niobium pentoxide nanosheets are prepared by hydrofluoric acid dissolution high-temperature reaction method, graphene template method and the like (chem.Mater.2016,28, 5753-containing 5760; Energy Storage Mater.2018,13, 223-containing 232; Adv.Mater.2017,29,1701427) which are mentioned in the literature. However, the product obtained by the methods has the defects of difficult control of appearance, poor crystal form and poor repeatability. Until now, controllable preparation of porous orthorhombic niobium pentoxide nanosheets and nanoflowers has not been found.
The invention provides a novel preparation method of porous orthorhombic niobium pentoxide nanosheets and nanoflowers, which are synthesized through solvothermal reaction through different growth mechanisms of niobium salts in different solvents, have good two-dimensional flaky morphology, porous distribution and excellent electrochemical performance, and have certain novelty and innovation.
Disclosure of Invention
The invention aims to overcome the defects of the existing material preparation technology and provides a preparation method of porous orthorhombic niobium pentoxide nanosheets and nanoflowers, which has the advantages of simple equipment, convenience in operation, controllable appearance, good repeatability, low cost and easiness in process amplification.
The preparation method of the porous orthogonal-phase niobium pentoxide nanosheet and nanoflower is characterized by comprising the following steps of:
(1) adding soluble niobium salt serving as a raw material into a solvent, uniformly mixing, adding alkali to adjust the pH value, carrying out solvothermal reaction for a plurality of hours, washing and drying a reaction product, and thus obtaining the nano flaky or flower-shaped niobium pentoxide precursor powder.
(2) And (2) calcining the niobium pentoxide precursor obtained in the step (1) in a muffle furnace at high temperature for several hours to obtain the porous nano flaky or flower-like orthorhombic niobium pentoxide.
In the step (1), the mass-to-volume ratio (g: mL) of the niobium salt to the solvent is 1: 100-1000, preferably the mass-to-volume ratio is 1: 300-700.
The niobium salt in the step (1) is one or more of niobium ethoxide, niobium oxalate, niobium pentachloride, niobium fluoride and niobium iodide; the niobium salt has a mass of 0.05 to 1.00g, preferably 0.1 to 0.5 g.
The solvent in the step (1) is one or more of water, ethanol, glycol, isopropanol or glycerol; the volume of the solvent is 50-150mL, and the preferred volume is 60-100 mL.
In the step (1): the mixing mode of the reaction raw materials is one or more of stirring, oscillation, ultrasound and the like.
The alkali in the step (1) is one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide and the like.
The pH in the step (1) is 8 to 11, preferably 8.5 to 10.
The solvothermal reaction temperature in the step (1) is 100-300 ℃, and the preferable temperature is 120-200 ℃.
The reaction time in the step (1) is 5-50h, and the preferable time is 12-24 h.
The washing mode in the step (1) is one or more of methods such as centrifugation, suction filtration and the like.
The drying mode in the step (1) is one of natural drying, normal-pressure heating drying, vacuum drying or freeze drying.
The high-temperature calcination temperature in the step (2) is 400-1000 ℃, and preferably the calcination temperature is 550-800 ℃.
The high-temperature calcination time in the step (2) is 1-10h, and preferably 2-5 h.
The pore diameter range of the porous nano sheets and nano flowers obtained in the step (2) is 10-200 nm.
The size of the nano sheet obtained in the step (2) is 100nm-10 μm; the obtained nanoflower has a size of 100nm-5 μm and is formed by self-assembly of nanosheets.
The invention has the beneficial effects that:
the preparation method of the invention avoids the defects of difficult shape control and poor repeatability caused by instability of the prior art; has the obvious advantages of simplicity, easy operation and low cost. The product prepared by the invention has uniform appearance, good crystal form, strong controllability, high quality, good performance and wide application range; the product is applied to the cathode material of the lithium ion battery, and has high capacity, high multiplying power and long cycle life.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is an X-ray diffraction pattern of porous orthorhombic niobium pentoxide nanoplates prepared in example 1.
Fig. 2 is a transmission electron micrograph of porous orthorhombic niobium pentoxide nanoplates prepared in example 1.
Fig. 3 is a scanning electron micrograph of porous orthorhombic niobium pentoxide nanoplates prepared in example 2.
Fig. 4 is a constant current charge and discharge curve of the porous orthorhombic niobium pentoxide nanoplates prepared in example 2.
Fig. 5 is a scanning electron micrograph of porous orthorhombic niobium pentoxide nanoflowers prepared in example 3.
Fig. 6 is a cycle curve of porous orthorhombic niobium pentoxide nanoflowers prepared in example 4.
Detailed Description
The method of the present invention will be described in detail with reference to specific examples, which are carried out on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
(1) Adding 0.1g of niobium pentachloride into 50mL of ethanol, uniformly performing ultrasonic treatment, slowly dropwise adding sodium hydroxide to adjust the pH value to 8.5, and performing solvothermal treatment for 12 hours in a reaction kettle. And centrifugally washing the reaction product, and heating and drying at normal pressure to obtain white niobium pentoxide precursor powder.
(2) And calcining the obtained niobium pentoxide precursor in a muffle furnace at 600 ℃ for 5 hours to obtain the porous nano flaky niobium pentoxide.
The XRD diffraction peak of the obtained niobium pentoxide belongs to PDF card: 30-0837 is orthorhombic niobium pentoxide. The size of the nano-sheet is about 1-2 μm, the thickness is about 10nm, and the aperture range is 10-80 nm. Testing the lithium battery to obtain: when the electrode material is charged and discharged at 100mA/g, the specific capacity of the electrode material is as high as 190 mAh/g.
Example 2
(1) Adding 0.15g of niobium oxalate into 80mL of water, uniformly oscillating, slowly dropwise adding ammonia water to adjust the pH value to 9, and heating the solution in a reaction kettle for 20 hours. And (4) carrying out suction filtration, washing and freeze drying on the reaction product to obtain white niobium pentoxide precursor powder.
(2) And calcining the obtained niobium pentoxide precursor in a muffle furnace at 650 ℃ for 3h to obtain the porous nano flaky orthorhombic niobium pentoxide.
The obtained niobium pentoxide nanosheet is about 1-3 μm in size, about 20nm in thickness and 50-200nm in pore size. Testing the lithium battery to obtain: when the electrode material is charged and discharged at 500mA/g, the specific capacity of the electrode material can reach 170 mAh/g.
Example 3
(1) Adding 0.2g of niobium ethoxide into 100mL of mixed solvent of ethanol and glycol (volume ratio: 1:1), uniformly stirring, slowly dropwise adding potassium hydroxide to adjust the pH value to 10, and heating the solvent in a reaction kettle for 15 hours. And centrifuging and washing the reaction product, and heating and drying in vacuum to obtain white niobium pentoxide precursor powder.
(2) And calcining the obtained niobium pentoxide precursor in a muffle furnace at 700 ℃ for 1.5h to obtain the porous nano flower-shaped orthorhombic niobium pentoxide.
The obtained niobium pentoxide nanometer flower has the size of about 500nm-1.5 μm, is formed by self-assembling porous nanometer sheets with the thickness of about 20nm, and has the pore diameter range of 20-100 nm. Testing the lithium battery to obtain: when the electrode material is charged and discharged at 200mA/g, the specific capacity of the electrode material can reach 185 mAh/g.
Example 4
(1) Adding 0.3g of niobium fluoride into 90mL of mixed solvent of water and glycerol (volume ratio: 1:1), uniformly performing ultrasonic treatment, slowly dropwise adding sodium hydroxide to adjust the pH value to 9.5, and heating the solvent in a reaction kettle for 18 h. And (3) carrying out suction filtration and washing on the reaction product, and heating and drying at normal pressure to obtain white niobium pentoxide precursor powder.
(2) And calcining the obtained niobium pentoxide precursor in a muffle furnace at 800 ℃ for 1h to obtain the porous nano flower-like orthorhombic niobium pentoxide.
The obtained niobium pentoxide nanoflower is about 500nm-3 μm in size, is formed by self-assembly of porous nanosheets with the thickness of about 30nm, and has the pore diameter ranging from 50nm to 200 nm. Testing the lithium battery to obtain: with 1Ag-1The initial capacity of the electrode material is 130mAh g-1The capacity of 500 cycles is almost not attenuated, and the coulombic efficiency is close to 100 percent.
Example 5
(1) Adding 0.5g of niobium iodide into 100mL of isopropanol, uniformly stirring, slowly dropwise adding ammonia water to adjust the pH value to 10, and heating the solution in a reaction kettle for 24 hours. And centrifuging, washing and freeze-drying the reaction product to obtain white niobium pentoxide precursor powder.
(2) And calcining the obtained niobium pentoxide precursor for 5 hours at 550 ℃ in a muffle furnace to obtain the porous nano flaky orthorhombic niobium pentoxide.
The obtained niobium pentoxide nanometer sheet has the size of about 2-5 μm, the thickness of about 5nm and the aperture range of 5-50 nm. Testing the lithium battery to obtain: with 2Ag-1During charging and discharging, the specific capacity of the electrode material can reach 120 mAh/g.
Claims (11)
1. A preparation method of a porous orthorhombic niobium pentoxide nano-material is characterized by comprising the following steps:
(1) adding soluble niobium salt serving as a raw material into a solvent, uniformly mixing, adding alkali to adjust the pH value, carrying out solvothermal reaction, washing and drying a reaction product to obtain nano flaky or flower-shaped niobium pentoxide precursor powder;
(2) and (2) calcining the niobium pentoxide precursor obtained in the step (1) in a muffle furnace at high temperature for several hours to obtain the porous nano flaky or flower-like orthorhombic niobium pentoxide material.
2. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (1): the niobium salt is one or more of niobium ethoxide, niobium oxalate, niobium pentachloride, niobium fluoride and niobium iodide.
3. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (1): the solvent is one or more of water, ethanol, ethylene glycol, isopropanol or glycerol; the alkali is one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide, etc.
4. The method of claim 1, wherein the mass-to-volume ratio (g: mL) of the niobium salt to the solvent is 1: 100-1000.
5. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (1): the reaction raw material mixing mode is one or more of stirring, oscillation, ultrasound and the like; the washing mode is one or more of centrifugation, suction filtration and the like; the drying mode is one of natural drying, normal pressure heating drying, vacuum drying or freeze drying.
6. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (1): adjusting the pH value to 8-11.
7. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (1): the solvent thermal reaction temperature is 100-300 ℃, and the reaction time is 5-50 h.
8. The method for preparing a porous orthorhombic niobium pentoxide nanomaterial according to claim 1, wherein in the step (2): the high-temperature calcination temperature is 400-1000 ℃; the calcination time is 1-10 h.
9. A porous orthorhombic niobium pentoxide nanomaterial obtained by the method according to any of claims 1-8, characterized in that the orthorhombic niobium pentoxide nanomaterial is of a porous nanosheet and nanoflower structure with a pore size in the range of 10-200 nm.
10. The porous orthorhombic niobium pentoxide nanomaterial according to claim 9, characterized in that the size of the nanosheets is 100nm-10 μ ι η; the obtained nanoflower has a size of 100nm-5 μm and is formed by self-assembly of nanosheets.
11. Use of the porous orthorhombic niobium pentoxide nanomaterial according to claim 9 in the fields of batteries, supercapacitors, catalysis. Particularly, as the lithium ion battery cathode material, the lithium ion battery cathode material shows high-quality specific capacity of 100-200mAh/g and good cycle life of 200-2000 circles.
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| CN114054016A (en) * | 2021-09-27 | 2022-02-18 | 西南交通大学 | Porous niobium oxide nano material, preparation method thereof and application thereof in carbon neutralization |
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Non-Patent Citations (2)
| Title |
|---|
| JUNLI CHEN ET AL: ""2D ultrathin nanosheet-assembled Nb2O5 microflowers for lithium ion"", 《MATERIALS LETTERS》 * |
| NICOLA PINNA ET AL: ""A novel nonaqueous route to V2O3 and Nb2O5 nanocrystals"", 《COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114054016A (en) * | 2021-09-27 | 2022-02-18 | 西南交通大学 | Porous niobium oxide nano material, preparation method thereof and application thereof in carbon neutralization |
| CN114054016B (en) * | 2021-09-27 | 2023-01-10 | 西南交通大学 | Porous niobium oxide nano material, preparation method thereof and application thereof in carbon neutralization |
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Application publication date: 20210525 |