CN103030137A - Overlong vanadium pentoxide nanowire harness with hierarchical structure and preparation method thereof - Google Patents
Overlong vanadium pentoxide nanowire harness with hierarchical structure and preparation method thereof Download PDFInfo
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- CN103030137A CN103030137A CN2013100211489A CN201310021148A CN103030137A CN 103030137 A CN103030137 A CN 103030137A CN 2013100211489 A CN2013100211489 A CN 2013100211489A CN 201310021148 A CN201310021148 A CN 201310021148A CN 103030137 A CN103030137 A CN 103030137A
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Abstract
The invention provides an overlong vanadium pentoxide nanowire harness with a hierarchical structure and a preparation method thereof. The length of the wire harness is not shorter than 10 cm; the diameter of the wire harness is 1-3 microns; the wire harness comprises parallel overlong nanowires; the diameters of the nanowires are 20-30 nm and the lengths of the nanowires are longer than 100 microns to 1 mm. The preparation method comprises the following steps: preparing a vanadium pentoxide sol by using a melting and quenching method; putting 40 ml sol to a reaction kettle; reacting the sol for 2-4 days under a condition of 160-200 DEG C so as to obtain a suspension containing overlong vanadium pentoxide nanowires; enabling a slender glass fiber to extend into the vanadium pentoxide nanowire suspension; lifting the slender glass fiber at a constant speed so as to obtain the wire harness; drying the obtained wire harness; carrying out heat treatment on the wire harness under an air atmosphere under a condition of 400-600 DEG C; and finally obtaining the overlong vanadium pentoxide nanowire harness with the hierarchical structure. A gas sensitive device assembled by using materials has the advantages of rapid response, good stability, sensitivity of 2.6 and low working temperature of 60 DEG C.
Description
Technical field
The invention belongs to nano material and gas sensor technical field, be specifically related to a kind of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness and preparation method thereof, this material can be used for preparing the highly sensitive gas sensor.
Background technology
The gas sensor prospect that has a very wide range of applications in fields such as safety in production, energy-saving and emission-reduction, environment protection, traffic safety management, aerospace, modern military, chemical defence anti-terrorisms at present; along with the development of nanotechnology, the application of nano material on gas sensor improved performance and the range of application of gas sensor greatly.Wherein, one-dimensional metal oxide nano-material has its unique structure and character, such as transistor field-effect, surface effects and small-size effect etc., becomes the focus that investigators pay close attention to.Vanadium Pentoxide in FLAKES is a kind of wide energy carrying semiconductor material, its one dimension Nano structure surface exists many and the avtive spot gas-selectively effect, in addition its unique laminate structure, the rapid diffusion that can provide more gas passage to be conducive to gas is a kind of gas sensitive of having very much potentiality.In recent years, utilize the linear structure of monodimension nanometer material very active in the research that nanoscale makes up the micro-nano device elementary cell.But, because it constructs the process complexity, need multiple advanced high-end technology and equipment, greatly limited it and used and promote.Because monodimension nanometer material is as the smallest dimension structure of electronics and the effective transmission of photon, to realize nano-device functionalization and integrated crucial elementary cell, therefore the monodimension nanometer material for preparing super-long structural has just become to simplify the manufacturing processed of nano-device, reduce preparation cost, realize the key of micro-nano device macroscopic viewization structure.
Summary of the invention
The object of the present invention is to provide the simple hierarchy overlength of a kind of technique Vanadium Pentoxide in FLAKES nano wire wire harness and preparation method thereof.
The technical scheme that realizes the object of the invention is: a kind of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, and this wire harness length 〉=10 cm, diameter is 1 ~ 3 μ m; Wire harness is comprised of parallel overlong nanowire, and described nanowire diameter is 20 ~ 30 nm, length greater than 100 μ m to 1 mm.
The preparation method of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness of the present invention may further comprise the steps:
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the vanadium pentoxide powder melting, pour the Vanadium Pentoxide in FLAKES of melting in deionized water quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, controls the concentration range of resulting Vanadium Pentoxide in FLAKES colloidal sol at 0.700wt % ~ 0.990 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, under 160 ~ 200 ℃ of conditions, reacted 2 ~ 4 days, obtain containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 2 ~ 6 hours under 400 ~ 600 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
Above-mentioned steps 3) manipulation require in carried out before the nanowire suspended liquid drying of Vanadium Pentoxide in FLAKES.
The hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness of the present invention preparation is applied on the gas sensor as gas sensitive, and its gas sensitive device preparation process is: will obtain wire harness and be wrapped in Al with Au electrode and Pt lead-in wire
2O
3On the vitrified pipe (internal diameter of vitrified pipe is 0.8 mm, and external diameter is 1.2 mm, and length is 4 mm), the nano wire wire harness gas sensitive device that obtains aligning; With the thermal treatment 2 ~ 6 hours under 400 ~ 600 ℃ of conditions in air atmosphere of this device.
The structure of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness is determined by X-ray powder diffraction instrument among the present invention.The X-ray powder diffraction shows that this wire harness is the monoclinic phase Vanadium Pentoxide in FLAKES.Field emission scanning electron microscope test shows that the diameter of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness is 1 ~ 3 μ m, and wire harness is comprised of parallel overlong nanowire, and nanowire diameter is 20 ~ 30 nm, length greater than 100 μ m to 1 mm.The optics picture shows that the wire harness snappiness is good, and plasticity-is high, and length can reach 〉=10 cm.
The invention has the beneficial effects as follows: take Vanadium Pentoxide in FLAKES as raw material, the method of employing hydro-thermal is prepared the Vanadium Pentoxide in FLAKES nano wire of overlength, and be that the glass fibre of 0.5 mm at the uniform velocity lifts the formation wire harness by diameter, this wire harness length can reach 〉=10 cm, and plasticity-is good, and snappiness is high, be fit to the assembling micro-nano device, can greatly simplify the manufacturing processed of nano-device, reduce preparation cost, realize micro-nano device macroscopic viewization structure.
The air-sensitive test environment is 20 ~ 28 ℃ of room temperatures among the present invention, and humidity is 27% RH, and test gas is alcohol gas, and concentration is 10,50,100,500,1000 ppm, and working temperature is 60,150,240,330 ℃.Test result shows that the response device of being made by hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness is rapid, good stability, and Sensitirity va1ue reaches 2.6, and working temperature is low to moderate 60 ℃.Compare with the device of direct coated with nano material, gas sensitive device by the preparation of nano wire wire harness aligns, and is conducive to the transmission of electronics, and hierarchy is so that it has larger specific surface area, be beneficial to quick adsorption and the desorption of detected gas, therefore can show better air-sensitive performance.
Description of drawings
Fig. 1 is the XRD figure spectrum of the hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness that makes of embodiment 1;
The FESEM image (a) of the overlength Vanadium Pentoxide in FLAKES nano wire that Fig. 2-the 1st, embodiment 1 obtain in the state of nature drying, as shown in the figure, the diameter of nano wire is 20 ~ 30 nm, length greater than 100 μ m to 1 mm;
Fig. 2-the 2nd, the FESEM image (b) that at the uniform velocity lifts the hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness that obtains of embodiment 1, as shown in the figure, beam diameter is 1 ~ 3 μ m, length can reach 〉=10 cm;
Fig. 3-the 1st, the FESEM image (a) of the hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness gas sensitive device of embodiment 1, as shown in the figure, wire harness is parallel to axial orientation and arranges;
Fig. 3-the 2nd, the FESEM image (b) of single bundle hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness of embodiment 1; As shown in the figure, this wire harness is comprised of parallel nano wire;
Fig. 4 is the sensitivity curve figure of the hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness gas sensitive device of embodiment 1.
Embodiment
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
The preparation of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, concrete steps are as follows:
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the Vanadium Pentoxide in FLAKES melting, pour the Vanadium Pentoxide in FLAKES of melting in 1000 ml deionized waters quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, and demarcating concentration is 0.9707 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, reaction is 2 days under 180 ℃ of conditions, obtains containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 2 hours under 400 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
The XRD figure spectrum of overlength Vanadium Pentoxide in FLAKES nano wire wire harness as shown in Figure 1, the FESEM image of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness is shown in Fig. 2-1 and Fig. 2-2, the FESEM image of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness assembling gas sensitive device is shown in Fig. 3-1 and Fig. 3-2, and the sensitivity curve of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness assembly device as shown in Figure 4.
Embodiment 2
The preparation of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, concrete steps are as follows:
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the Vanadium Pentoxide in FLAKES melting, pour fast the Vanadium Pentoxide in FLAKES of melting in 1400 ml deionized waters quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, demarcates concentration 0.7087 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, reaction is 4 days under 200 ℃ of conditions, obtains containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 4 hours under 600 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
Embodiment 3
The preparation of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, concrete steps are as follows:
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the Vanadium Pentoxide in FLAKES melting, pour fast the Vanadium Pentoxide in FLAKES of melting in 1200 ml deionized waters quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, demarcates concentration 0.8840 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, reaction is 2.5 days under 180 ℃ of conditions, obtains containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 4 hours under 400 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
Embodiment 4
The preparation of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, concrete steps are as follows:
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the Vanadium Pentoxide in FLAKES melting, pour fast the Vanadium Pentoxide in FLAKES of melting in 1300 ml deionized waters quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, demarcates concentration 0.7230 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, reaction is 2 days under 200 ℃ of conditions, obtains containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 4 hours under 600 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
1) gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the Vanadium Pentoxide in FLAKES melting, pour fast the Vanadium Pentoxide in FLAKES of melting in 1000 ml deionized waters quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, and demarcating concentration is 0.9707 wt %;
2) measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, reaction is 4 days under 160 ℃ of conditions, obtains containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3) be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4) with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, and thermal treatment 6 hours under 400 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
The XRD figure spectrum of embodiment 2,3,4 and 5 resulting overlength Vanadium Pentoxide in FLAKES nano wire wire harness, the FESEM image of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness, the FESEM image of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness assembling gas sensitive device, the sensitivity curve of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness assembly device is all similar to embodiment 1 result.
Claims (3)
1. a hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness is characterized in that, this wire harness length 〉=10 cm, and diameter is 1 ~ 3 μ m; Wire harness is comprised of parallel overlong nanowire, and described nanowire diameter is 20 ~ 30 nm, length greater than 100 μ m to 1 mm.
2. the preparation method of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness claimed in claim 1 is characterized in that may further comprise the steps:
1), gets 10 g vanadium pentoxide powders and put into crucible, after retort furnace is warming up to 800 ℃, crucible is put into retort furnace insulation 30 min make the vanadium pentoxide powder melting, pour the Vanadium Pentoxide in FLAKES of melting in deionized water quenching, the gained liquid heat is to boiling and clockwise stirring, suction filtration after the cooling, filtrate is left standstill and was obtained Vanadium Pentoxide in FLAKES colloidal sol in seven days, controls the concentration range of resulting Vanadium Pentoxide in FLAKES colloidal sol at 0.700 wt % ~ 0.990 wt %;
2), measure step 1) gained colloidal sol 40 ml, put into the reactor of 50 ml volumes, under 160 ~ 200 ℃ of conditions, reacted 2 ~ 4 days, obtain containing the suspension of overlength Vanadium Pentoxide in FLAKES nano wire;
3), be that the glass fibre of 0.5 mm stretches into step 2 with diameter) in the gained suspension, at the uniform velocity lift with the speed of 30 cm/min, obtain Vanadium Pentoxide in FLAKES nano wire wire harness;
4), with step 3) the Vanadium Pentoxide in FLAKES nano wire wire harness that obtains is dry, thermal treatment 2 ~ 6 hours under 400 ~ 600 ℃ of conditions finally obtains hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness in air atmosphere.
3. the preparation method of hierarchy overlength Vanadium Pentoxide in FLAKES nano wire wire harness as claimed in claim 2 is characterized in that step 3) in manipulation require before the nanowire suspended liquid drying of Vanadium Pentoxide in FLAKES, carry out.
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| CN104701516A (en) * | 2015-02-06 | 2015-06-10 | 武汉理工大学 | Nano-sheet water-containing V2O5 dry gel assembled by needle-like nanowires as well as preparation method and application thereof |
| CN105118977A (en) * | 2015-09-02 | 2015-12-02 | 武汉理工大学 | V2O5 hollow micron wire ball with nano wire three-dimensional winding structure and preparation method and application thereof |
| CN107331717A (en) * | 2017-06-26 | 2017-11-07 | 暨南大学 | A kind of organic-inorganic nano line and preparation method thereof and organic-inorganic photo-detector and preparation method thereof |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macroscopic inorganic semiconductor nano fiber and its preparation method and application |
| CN111584839A (en) * | 2020-05-07 | 2020-08-25 | 武汉理工大学 | Porphyrin compound doped vanadium pentoxide sol composite material and preparation method and application thereof |
| CN112546748A (en) * | 2020-11-18 | 2021-03-26 | 西安热工研究院有限公司 | Preparation method of low-temperature denitration filter material based on water quenching method |
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Cited By (8)
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| CN104701516A (en) * | 2015-02-06 | 2015-06-10 | 武汉理工大学 | Nano-sheet water-containing V2O5 dry gel assembled by needle-like nanowires as well as preparation method and application thereof |
| CN104701516B (en) * | 2015-02-06 | 2017-01-18 | 武汉理工大学 | Nano-sheet water-containing V2O5 dry gel assembled by needle-like nanowires as well as preparation method and application thereof |
| CN105118977A (en) * | 2015-09-02 | 2015-12-02 | 武汉理工大学 | V2O5 hollow micron wire ball with nano wire three-dimensional winding structure and preparation method and application thereof |
| CN107331717A (en) * | 2017-06-26 | 2017-11-07 | 暨南大学 | A kind of organic-inorganic nano line and preparation method thereof and organic-inorganic photo-detector and preparation method thereof |
| CN110306260A (en) * | 2019-06-18 | 2019-10-08 | 东华大学 | A kind of macroscopic inorganic semiconductor nano fiber and its preparation method and application |
| CN111584839A (en) * | 2020-05-07 | 2020-08-25 | 武汉理工大学 | Porphyrin compound doped vanadium pentoxide sol composite material and preparation method and application thereof |
| CN111584839B (en) * | 2020-05-07 | 2022-05-06 | 武汉理工大学 | Porphyrin compound doped vanadium pentoxide sol composite material and preparation method and application thereof |
| CN112546748A (en) * | 2020-11-18 | 2021-03-26 | 西安热工研究院有限公司 | Preparation method of low-temperature denitration filter material based on water quenching method |
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