CN109626425B - Nano linear Na1.1V3O7.9Material, method for the production thereof and use thereof - Google Patents

Nano linear Na1.1V3O7.9Material, method for the production thereof and use thereof Download PDF

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CN109626425B
CN109626425B CN201910137638.2A CN201910137638A CN109626425B CN 109626425 B CN109626425 B CN 109626425B CN 201910137638 A CN201910137638 A CN 201910137638A CN 109626425 B CN109626425 B CN 109626425B
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CN109626425A (en
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李冬冬
类延华
周佳贝
谭宁
邱智超
孙士斌
张玉良
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Shanghai Maritime University
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    • C01G31/00—Compounds of vanadium
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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Abstract

The invention discloses a nano linear Na1.1V3O7.9A material, a method for its preparation and use, the method comprising the steps of: step 1: adding NaNO3Heating and melting; step 2: will VCl3Adding to molten NaNO3Stirring uniformly, and keeping the temperature to ensure that the reaction is complete; and step 3: cooling to room temperature, washing, centrifuging and drying the reaction product to obtain the nano linear Na1.1V3O7.9A material. The method provided by the invention has the advantages of cheap and easily obtained raw materials, simple preparation process and low production cost, and the prepared Na1.1V3O7.9The shape of microscopic particles of the material is controllable, the nanowires are uniformly distributed, no by-product is generated in the whole process, and the material is green, energy-saving, environment-friendly and efficient. The prepared material is an orthorhombic system with a layered structure, has a large specific surface area, can allow gas molecules to easily enter between layers, and is suitable for sensitive materials for gas sensors and electrode materials of lithium ion batteries.

Description

Nano linear Na1.1V3O7.9Material, method for the production thereof and use thereof
Technical Field
The invention relates to the technical field of nano material preparation, in particular to nano linear Na1.1V3O7.9Materials, methods of making and uses thereof.
Background
Currently, gas sensors capable of detecting toxic gases and flammable gases in real time have received much attention due to the needs in medical care, environmental protection, food detection, industrial safety monitoring, and the like. In the field of gas-sensitive sensing, various gas sensing detection methods are available based on different gas-sensitive sensing principles. When the detected target gas appears, the resistance of the material changes due to the electronic exchange and chemical reaction, and the material is detected, so that the gas-sensitive sensing method is simple and convenient, and is easy to combine with a semiconductor process and integrate into a detection chip.
Transition metal oxide used as gas sensitive material with variable resistance, such as ZnO and SnO2、Fe2O3、TiO2、WO3、Cu2O, NiO, where vanadium oxide is a promising class of gas sensitive materials, such as VO2，V2O5And the like. Since the crystal structure thereof belongs to the orthorhombic system of the layered structure, gas molecules can easily enter between the layers. Wherein, V2O5Has better gas-sensitive property to ethanol, organic amine and helium. The traditional oxide gas sensor is based on structures such as single crystal, polycrystal, thin film and powder. With the progress of the technology, the oxide materials with nano-structures such as nano-wires, nano-belts, nano-tubes and the like can effectively improve the sensitivity of gas detection due to the larger specific surface area, and are increasingly paid more attention. For example: v2O5The nanobelt has better selectivity and stability to ethanol gas; v2O5The nanowires exhibit gas-sensitive properties to helium.
However, the gas sensor based on vanadium oxide has good gas-sensitive characteristics which are usually obtained at a temperature of more than 150 ℃, and are more convenient, safe and energy-saving when the gas sensor is obtained at room temperature.
At present, the preparation methods of vanadium oxide mainly comprise an electrodeposition method, a sol-gel method, a hydrothermal method and the like, wherein the hydrothermal method is the most mature. There are many methods for preparing vanadium oxides, such as: the Chinese patent with publication number CN102826603A adopts vanadium dioxide powder as a vanadium source, and vanadium pentoxide nanowires are obtained by hydrothermal reaction in a nitric acid aqueous solution, wherein the length of the vanadium pentoxide nanowires is about 10-60 mu m, the diameter of the vanadium pentoxide nanowires is 10-50 nm, but the hydrothermal temperature of the vanadium pentoxide nanowires is 140-250 ℃, and the temperature of the vanadium pentoxide nanowires is higher; chinese patent with publication number CN108288701A utilizes vanadium dioxide powder as vanadium source, and obtains Na through hydrothermal reaction in oxalic acid and sodium hydroxide water solution1.1V3O7.9And complex phase Na1.1V3O7.9/NaV6O15The hydrothermal reaction time of the material is longer, and 24 hours are needed.
Most vanadium oxides prepared by the method adopt a hydrothermal method, and have the defects of overhigh hydrothermal temperature, overlong reaction time, low yield of reaction products and the like. The preparation method has the disadvantages of complicated process, high requirement on conditions and poor operability.
Disclosure of Invention
The invention aims to provide nano linear Na1.1V3O7.9The material, the preparation method and the application thereof are used for simplifying the preparation process, reducing the requirement of the preparation process, providing possibility for mass production and realizing energy conservation and environmental protection.
In order to achieve the above purpose, the invention provides a nanowire-shaped Na1.1V3O7.9A method of preparing a material comprising the steps of:
step 1: adding NaNO3Heating and melting;
step 2: will VCl3Adding to molten NaNO3Stirring uniformly, and keeping the temperature to ensure that the reaction is complete;
and step 3: cooling to room temperature, washing, centrifuging and drying the reaction product to obtain the nano linear Na1.1V3O7.9A material.
The above-mentioned nanowire-like Na1.1V3O7.9A method for preparing a material, wherein, in step 1, NaNO3The heating temperature is 300-380 ℃.
The above-mentioned nanowire-like Na1.1V3O7.9The preparation method of the material comprises the step 2, wherein the heat preservation time is 1-10 min.
The above-mentioned nanowire-like Na1.1V3O7.9Method for the preparation of a material, wherein, NaNO3And VCl3In a mass ratio of 50: 1.
The invention also provides the nano linear Na prepared by the method1.1V3O7.9A material.
The invention further provides the nano linear Na1.1V3O7.9The application of the material, which is used for preparing sensitive materials of gas sensors.
The invention further provides the nano linear Na1.1V3O7.9Use of a material for the preparation of an electrode material for a lithium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention has the advantages of cheap and easily obtained raw materials, simple preparation process and low production cost, and the prepared Na1.1V3O7.9The shape of microscopic particles of the material is controllable, the nanowires are uniformly distributed, no by-product is generated in the whole process, and the material is green, energy-saving, environment-friendly and efficient. The prepared material is an orthorhombic system with a layered structure, has a large specific surface area, can allow gas molecules to easily enter between layers, and is suitable for sensitive materials for gas sensors and electrode materials of lithium ion batteries.
Drawings
FIG. 1 shows nanowire-like Na prepared in example 11.1V3O7.9XRD spectrum of the material;
FIG. 2a shows nanowire-like Na prepared in example 21.1V3O7.9Material in proportionSEM photograph at 1 micron ruler;
FIG. 2b shows nanowire-like Na prepared in example 21.1V3O7.9SEM photograph of the material at a scale bar of 100 nm;
FIG. 3a shows nanowire-like Na prepared in example 11.1V3O7.9A performance analysis chart of the material as a sensitive material of the gas sensor;
FIG. 3b shows nanowire-like Na prepared in example 21.1V3O7.9A performance analysis chart of the material as a sensitive material of the gas sensor;
FIG. 3c shows nanowire-like Na prepared in example 31.1V3O7.9A performance analysis chart of the material as a sensitive material of the gas sensor;
FIG. 4 shows Na prepared in examples 1 to 3 under the optimum working temperature (480 ℃ C.)1.1V3O7.9Sensitivity data plots for different concentrations of ethanol gas.
Detailed Description
The invention will be further described by the following specific examples in conjunction with the drawings, which are provided for illustration only and are not intended to limit the scope of the invention.
Example 1
The muffle furnace was first brought from room temperature to 320 ℃ and then 5g of NaNO was added3Placing into a muffle furnace, and keeping the temperature for 10min to allow the NaNO to react3Melted and then 0.1g VCl3Adding already molten NaNO3Keeping the temperature for 1-2min, naturally cooling to room temperature, washing, centrifuging, and drying to obtain nanometer linear Na1.1V3O7.9The material is in a nanowire shape.
Example 2
The muffle furnace was first brought from room temperature to 350 ℃ and then 5g of NaNO was added3Placing into a muffle furnace, and keeping the temperature for 10min to allow the NaNO to react3Melted and then 0.1g VCl3Adding already molten NaNO3Stirring to complete reaction, maintaining the temperature for 1-10min, cooling to room temperature, washing, centrifuging, and drying to obtain nanowireNa1.1V3O7.9A material.
Nanowire-like Na prepared in this example1.1V3O7.9The XRD spectrum of the material is shown in figure 1, and the diffraction peaks of the material correspond to Na1.1V3O7.9(ref. code 00-045-. Description of Na1.1V3O7.9The crystallization degree is better and the purity of the substance is higher.
Nanowire-like Na prepared in this example1.1V3O7.9The material was subjected to a scanning electron microscope (SEM test), fig. 2a representing a low magnification (scale bar 1 micron) SEM photograph after firing at 350 ℃, and fig. 2b representing a high magnification (scale bar 100 nm) SEM photograph after firing at 350 ℃. The Na can be seen from the SEM image1.1V3O7.9The material has an obvious and ordered nanowire structure, uniformly distributed nanowire clusters are formed, the specific surface area of the substance is increased, gas molecules can easily enter between layers, and the sensing effect of the substance on gas is greatly increased.
Example 3
The muffle furnace was first brought from room temperature to 380 ℃ and then 5g of NaNO were added3Placing into a muffle furnace, and keeping the temperature for 10min to allow the NaNO to react3Melted and then 0.1g VCl3Adding already molten NaNO3Keeping the temperature for 1-2min, naturally cooling to room temperature, washing, centrifuging, and drying to obtain nanometer linear Na1.1V3O7.9The material is in a nanowire shape.
Examples 1-3 preparation of nanowire-like Na1.1V3O7.9The performance test parts of the material as the sensitive material of the gas sensor on the gas-sensitive performance are shown in figures 3 a-3 c and 4, and figures 3 a-3 c show Na obtained under different melting preparation temperature conditions1.1V3O7.9Transient response data for 100ppm ethanol at various operating temperatures are shown in FIG. 3a, where Na is shown at a preparation temperature of 320 deg.C1.1V3O7.9Graphs of transient response data to 100ppm ethanol at different operating temperatures (340 deg.C, 370 deg.C, 400 deg.C, 440 deg.C, 480 deg.C); FIG. 3b shows Na at a preparation temperature of 350 deg.C1.1V3O7.9Graphs of transient response data to 100ppm ethanol at different operating temperatures (340 deg.C, 370 deg.C, 400 deg.C, 440 deg.C, 480 deg.C); FIG. 3c shows Na at a preparation temperature of 380 deg.C1.1V3O7.9Graph of transient response data for 100ppm ethanol at different operating temperatures (340 deg.C, 370 deg.C, 400 deg.C, 440 deg.C, 480 deg.C). The Na obtained under different preparation temperature conditions can be intuitively found from the transient response diagram1.1V3O7.9Has the best sensitivity under the working temperature condition of 480 ℃. FIG. 4 shows Na under the condition of optimum working temperature (480 ℃ C.)1.1V3O7.9Sensitivity data of ethanol gas with different concentrations are shown, and Na can be seen from the graph1.1V3O7.9The response sensitivity to ethanol gas with different concentrations is increased and then reduced along with the increase of the ethanol concentration, wherein Na obtained under the condition of 350 ℃ sintering temperature1.1V3O7.9Most obviously, the sensitivity reaches about 3 at the maximum of 400ppm ethanol concentration. Therefore, the nano linear Na prepared by the method provided by the invention1.1V3O7.9The material has excellent gas sensing performance after detection, and is suitable for gas sensors.
Due to Na prepared in examples 1-31.1V3O7.9The material is orthorhombic with a laminated structure, has a large specific surface area, and gas molecules can easily enter between layers, so the Na1.1V3O7.9The material is also suitable for preparing electrode materials of lithium ion batteries so as to improve various performances of the lithium ion batteries.
In conclusion, the method provided by the invention has the advantages of cheap and easily available raw materials, simple preparation process, low production cost and capability of preparing the Na1.1V3O7.9The shape of microscopic particles of the material is controllable, the nano wires are uniformly distributed, no by-product is generated in the whole process, and the material is green, energy-saving, environment-friendly and high in degree of environmental protectionAnd (5) effect. The prepared material is an orthorhombic system with a layered structure, has a large specific surface area, can allow gas molecules to easily enter between layers, and is suitable for sensitive materials for gas sensors and electrode materials of lithium ion batteries.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.

Claims (4)

1. Nano linear Na1.1V3O7.9The preparation method of the material is characterized by comprising the following steps:
step 1: adding NaNO3Heating and melting;
step 2: will VCl3Adding to molten NaNO3Stirring uniformly, and keeping the temperature to ensure that the reaction is complete;
and step 3: cooling to room temperature, washing, centrifuging and drying the reaction product to obtain the nano linear Na1.1V3O7.9A material.
2. The nanowire-like Na of claim 11.1V3O7.9The method for preparing the material is characterized in that in the step 1, NaNO is added3The heating temperature is 300-380 ℃.
3. The nanowire-like Na of claim 11.1V3O7.9The preparation method of the material is characterized in that in the step 2, the heat preservation time is 1-10 min.
4. The nanowire-like Na of claim 11.1V3O7.9A method for producing a material, characterized in that NaNO is used3And VCl3In a mass ratio of 50: 1.
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CN111769276A (en) * 2020-06-01 2020-10-13 上海海事大学 Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application
CN114956171A (en) * 2021-02-24 2022-08-30 陕西则明未来科技有限公司 Preparation and application of sodium-vanadium-oxygen heterojunction material

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