CN105301063A - Preparation method for tungsten-oxide-nanosheet-structured gas sensor working at room temperature - Google Patents
Preparation method for tungsten-oxide-nanosheet-structured gas sensor working at room temperature Download PDFInfo
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- CN105301063A CN105301063A CN201510718189.2A CN201510718189A CN105301063A CN 105301063 A CN105301063 A CN 105301063A CN 201510718189 A CN201510718189 A CN 201510718189A CN 105301063 A CN105301063 A CN 105301063A
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Abstract
The invention discloses a preparation method for a tungsten-oxide-nanosheet-structured gas sensor working at room temperature. The preparation method comprises the steps that a ceramic wafer substrate is cleaned, a platinic interdigital electrode is prepared on the ceramic wafer substrate, a solvothermal reaction solution is prepared, a tungsten-oxide-nanorod-structured gas sensor is prepared through a solvothermal method, an aluminum oxide substrate after a solvothermal reaction is cleaned, and thermal treatment is performed on elements of the tungsten-oxide-nanorod-structured gas sensor. According to the preparation method, the tungsten-oxide-nanosheet-structured gas sensor can be prepared at low cost. According to the solvothermal method, operation is easier, the technological conditions needing to be controlled are few, and no pollution to the environment is generated. The preparation method for the tungsten-oxide-nanosheet-structured gas sensor which can detect nitrogen oxide gas with the extremely low concentration (can reach 0.1 ppm) and is high in sensitivity and rapid to respond/recover is supplied, and the important practice and research significances are achieved.
Description
Technical field
The present invention relates to a kind of preparation method of oxides of nitrogen gas sensors, particularly a kind of preparation method of the tungsten oxide nanometer chip architecture gas sensor for working and room temperature.
Background technology
Modern industry while develop rapidly also along with ever-increasing various harmful gas (as NO
3, CO, NH
3, SO
2deng), this causes very large harm to the health of the mankind.Wherein oxides of nitrogen (NO
x) as a kind of toxic and harmful, be the main cause that acid rain and photo-chemical smog are formed.Along with the enhancing of mankind's environmental consciousness, the gas sensor with features such as high sensitivity, high selectivity, repeatabilities is desirable.WO
3the shortcoming of gas sensitive working temperature high (about 250 DEG C) brings complicacy and instability to sensor-based system is integrated.For this reason, scientific and technical personnel are devoted to the research reducing gas sensitive working temperature always.Research shows, two dimensional oxidation tungsten nanometer sheet has larger specific surface area, surfactivity and stronger gas sorption ability, thus effective lower working temperature while of carrying highly sensitive further.
Tungsten oxide, as a kind of semiconductor sensitive material having research and apply prospect, has been widely used in and has detected various poisonous and dangerous gas.It belongs to surface resistance control type to the sensitive mechanism of oxides of nitrogen gas, be based on the oxygen in air and detected nitrogen dioxide gas at metal oxide semiconductor adsorption and reaction the resistance modulated process to semiconductor material.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation method of the tungsten oxide nanometer chip architecture gas sensor for working and room temperature, overcoming the problem that in prior art, tungsten oxide gas sensor working temperature is high, power consumption is large.
Technical scheme of the present invention is: a kind of preparation method of the tungsten oxide nanometer chip architecture gas sensor for working and room temperature, has following steps:
(1) cleaning ceramic sheet (alundum (Al2O3)) substrate
Adopt potsherd as substrate, potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15-20min, removing surface organic matter impurity.Subsequently deionized water is put in potsherd substrate to clean, after having rinsed, put into absolute ethyl alcohol, and be placed in IR bake and dry;
(2) in potsherd substrate, prepare the interdigital electrode of Pt
Potsherd substrate is placed in the vacuum chamber of DPS-III type high vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, sputtering operating pressure is 2.0Pa, sputtering power 80-90W, sputtering time 8-10min, base reservoir temperature is room temperature, forms interdigital platinum electrode at alumina base basal surface;
(3) solvent thermal reaction solution is prepared
First configure the tungsten hexachloride solution of 0.04M-0.06M, be dissolved in by tungsten hexachloride in 65ml ethylene glycol, magnetic agitation, to all dissolving, forms the tungsten hexachloride solution of yellow transparent;
(4) solvent-thermal method prepares tungsten oxide nanometer chip architecture gas sensor
The alumina substrate being coated with platinum electrode in step (2) is placed in the stainless steel hydrothermal reaction kettle that liner is teflon, tungsten hexachloride solution prepared by step (3) is also transferred in reactor simultaneously, sealing, then reactor is placed in thermostatic drying chamber, in alumina base basal surface synthesis tungsten oxide nanometer chip architecture at temperature of reaction 180-210 DEG C, reaction time is 6-10h, after completion of the reaction, reactor is naturally cooled to room temperature;
(5) cleaning solvent thermal response rear oxidation aluminium substrate
By the alumina substrate after solvent thermal reaction in step (4), repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8-10h in the vacuum drying chamber of 60-80 DEG C;
(6) thermal treatment of tungsten oxide nanometer chip architecture gas sensor element
Tungsten oxide nanometer chip architecture gas sensor element prepared by step (4) is placed in muffle furnace heat-treat, heat treatment temperature is 300-400 DEG C, temperature retention time is 2h, and heating rate is 2-5 DEG C/min, in order to increase the crystallinity of tungstic oxide nano-sheets.
Compared with the prior art, the invention has the beneficial effects as follows:
1) provide and a kind ofly low cost can prepare the method for tungsten oxide nanometer chip architecture gas sensor.Solvent-thermal method operation is comparatively simple, and the process conditions of required control are few, and environmentally safe.
2) provide one and room temperature can detect extremely low concentration (can 0.1ppm be reached) oxides of nitrogen gas, there is the preparation method of high sensitivity, the quick tungsten oxide nanometer chip architecture gas sensor responding/recover, there is important practice and Research Significance.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the tungstic oxide nano-sheets prepared by embodiment 1, and scale is 2 μm;
Fig. 2 is the transmission electron microscope photo of the tungstic oxide nano-sheets prepared by embodiment 1, and scale is 200nm;
Fig. 3 is the XRD collection of illustrative plates of the tungstic oxide nano-sheets prepared by embodiment 1;
Fig. 4 is that tungsten oxide nanometer chip architecture gas sensor element prepared by embodiment 1 is at ambient temperature to 0.1-3ppmNO
2the dynamic response curve figure of gas;
Fig. 5 is the sensitivity at ambient temperature of tungsten oxide nanometer chip architecture gas sensor element prepared by embodiment 1 and NO
2the corresponding relation figure of gas concentration.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
(1) cleaning ceramic sheet (alundum (Al2O3)) substrate:
Adopt potsherd (1cm × 2cm) as substrate, potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15min, removing surface organic matter impurity.And be placed in IR bake and dry stand-by.
(2) in potsherd substrate, prepare the interdigital electrode of Pt:
Potsherd substrate is placed in the vacuum chamber of DPS-III type high vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, sputtering operating pressure is 2.0Pa, sputtering power 85W, sputtering time 10min, base reservoir temperature is room temperature, forms interdigital platinum electrode at alumina base basal surface.
(3) solvent thermal reaction solution is prepared:
First configure the tungsten hexachloride solution of 0.05M, take 1.19g tungsten hexachloride and be dissolved in 65ml ethylene glycol, magnetic agitation, to all dissolving, forms the tungsten hexachloride solution of yellow transparent.
(4) solvent-thermal method prepares tungsten oxide nanometer chip architecture gas sensor:
The alumina substrate being coated with platinum electrode in step (2) is placed in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, tungsten hexachloride solution prepared by step (3) is also transferred in reactor simultaneously, sealing, then reactor is placed in thermostatic drying chamber, in alumina base basal surface synthesis tungsten oxide nanometer chip architecture at temperature of reaction 200 DEG C, reaction time is 9h, after completion of the reaction, reactor is naturally cooled to room temperature;
(5) cleaning solvent thermal response rear oxidation aluminium substrate:
By the alumina substrate after solvent thermal reaction in step (4), repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 9h in the vacuum drying chamber of 80 DEG C.
The electron microscopic analysis result of the surface topography of the tungstic oxide nano-sheets prepared by embodiment 1 as shown in Figure 1.Can form equally distributed thickness in alumina sensor substrate is 30-300nm, and diameter is the nanometer sheet of 0.3-3.5 μm; In addition, the tem study result of tungstic oxide nano-sheets as shown in Figure 2.
(6) thermal treatment of tungsten oxide nanometer chip architecture gas sensor element:
Tungsten oxide nanometer chip architecture gas sensor element prepared by step (4) is placed in muffle furnace heat-treat, heat treatment temperature is 350 DEG C, and temperature retention time is 2h, and heating rate is 2.5 DEG C/min.
The X-ray diffraction analysis result of the tungstic oxide nano-sheets prepared by embodiment 1 as shown in Figure 3.The crystalline phase of XRD spectra display tungstic oxide nano-sheets is six side phase WO of monocrystalline
3, and there is good crystallinity.
The obtained tungsten oxide nanometer chip architecture gas sensor element of embodiment 1 at room temperature to the dynamic response curve of the NO2 gas of 0.1-3ppm as shown in Figure 4.Its sensitivity at room temperature and NO
2the corresponding relation schematic diagram of gas concentration as shown in Figure 5, wherein to 0.1,0.5,1,2,3ppmNO
2the sensitivity of gas is respectively 3.9,9.6,15.9,22.3 and 30.5.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in step (4), the temperature of reaction of solvent thermal reaction is 180 DEG C, and obtained tungsten oxide nanometer chip architecture gas sensor element is at room temperature to lppmNO
2the sensitivity of gas is 6.72.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in step (4), the temperature of reaction of solvent thermal reaction is 190 DEG C, and obtained tungsten oxide nanometer chip architecture gas sensor element is at room temperature to lppmNO
2the sensitivity of gas is 8.34.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in step (4), the temperature of reaction of solvent thermal reaction is 210 DEG C, and obtained tungsten oxide nanometer chip architecture gas sensor element is at room temperature to lppmNO
2the sensitivity of gas is 3.87.
Above with reference to drawings and Examples, to invention has been schematic description, this description is not restricted.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1., for a preparation method for the tungsten oxide nanometer chip architecture gas sensor of working and room temperature, it is characterized in that there are following steps:
(1) cleaning ceramic sheet substrate
Adopt potsherd as substrate, potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15-20min, removing surface organic matter impurity; Subsequently deionized water is put in potsherd substrate to clean, after having rinsed, put into absolute ethyl alcohol, and be placed in IR bake and dry;
(2) in potsherd substrate, prepare the interdigital electrode of Pt
Potsherd substrate is placed in the vacuum chamber of high vacuum facing-target magnetron sputtering system equipment, forms interdigital platinum electrode at alumina base basal surface;
(3) solvent thermal reaction solution is prepared
First configure the tungsten hexachloride solution of 0.04M-0.06M, be dissolved in by tungsten hexachloride in 65ml ethylene glycol, magnetic agitation, to all dissolving, forms the tungsten hexachloride solution of yellow transparent;
(4) solvent-thermal method prepares tungsten oxide nanometer chip architecture gas sensor
The alumina substrate being coated with platinum electrode in step (2) is placed in the stainless steel hydrothermal reaction kettle that liner is teflon, tungsten hexachloride solution prepared by step (3) is also transferred in reactor simultaneously, sealing, then reactor is placed in thermostatic drying chamber, in alumina base basal surface synthesis tungsten oxide nanometer chip architecture at temperature of reaction 180-210 DEG C, reaction time is 6-10h, after completion of the reaction, reactor is naturally cooled to room temperature;
(5) cleaning solvent thermal response rear oxidation aluminium substrate
By the alumina substrate after solvent thermal reaction in step (4), repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8-10h in the vacuum drying chamber of 60-80 DEG C;
(6) thermal treatment of tungsten oxide nanometer chip architecture gas sensor element
Tungsten oxide nanometer chip architecture gas sensor element prepared by step (4) is placed in muffle furnace heat-treat.
2. according to claim 1 for the preparation method of the tungsten oxide nanometer chip architecture gas sensor of working and room temperature, it is characterized in that, described step (2) high vacuum facing-target magnetron sputtering system equipment is in the vacuum chamber of DPS-III type high vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, sputtering operating pressure is 2.0Pa, sputtering power 80-90W, sputtering time 8-10min, base reservoir temperature is room temperature.
3., according to claim 1 for the preparation method of the tungsten oxide nanometer chip architecture gas sensor of working and room temperature, it is characterized in that, described step (6) heat treatment temperature is 300-400 DEG C, and temperature retention time is 2h, and heating rate is 2-5 DEG C/min.
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Cited By (7)
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| CN105717109A (en) * | 2016-04-21 | 2016-06-29 | 林业城 | Hydrogen gas sensor based on gasochromic function |
| CN105928933A (en) * | 2016-04-21 | 2016-09-07 | 林业城 | Smell-seeing hydrogen generator |
| CN105953067A (en) * | 2016-04-21 | 2016-09-21 | 林业城 | Hydrogen cylinder with leak detection function |
| CN107117831A (en) * | 2017-05-26 | 2017-09-01 | 桂林理工大学 | A kind of WO3The preparation method of nano-chip arrays |
| CN110849955A (en) * | 2019-12-03 | 2020-02-28 | 浙江大学 | High-sensitivity ammonia gas sensor and preparation method thereof |
| CN115128134A (en) * | 2022-06-21 | 2022-09-30 | 武汉铂纳智感科技有限公司 | Gas sensor based on optical excitation, preparation method and application |
| CN115611315A (en) * | 2022-12-14 | 2023-01-17 | 南方电网数字电网研究院有限公司 | Tungsten oxide/sodium niobate composite material and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105717109A (en) * | 2016-04-21 | 2016-06-29 | 林业城 | Hydrogen gas sensor based on gasochromic function |
| CN105928933A (en) * | 2016-04-21 | 2016-09-07 | 林业城 | Smell-seeing hydrogen generator |
| CN105953067A (en) * | 2016-04-21 | 2016-09-21 | 林业城 | Hydrogen cylinder with leak detection function |
| CN107117831A (en) * | 2017-05-26 | 2017-09-01 | 桂林理工大学 | A kind of WO3The preparation method of nano-chip arrays |
| CN107117831B (en) * | 2017-05-26 | 2020-10-09 | 桂林理工大学 | Preparation method of WO3 nanosheet array |
| CN110849955A (en) * | 2019-12-03 | 2020-02-28 | 浙江大学 | High-sensitivity ammonia gas sensor and preparation method thereof |
| CN110849955B (en) * | 2019-12-03 | 2022-01-04 | 浙江大学 | High-sensitivity ammonia gas sensor and preparation method thereof |
| CN115128134A (en) * | 2022-06-21 | 2022-09-30 | 武汉铂纳智感科技有限公司 | Gas sensor based on optical excitation, preparation method and application |
| CN115611315A (en) * | 2022-12-14 | 2023-01-17 | 南方电网数字电网研究院有限公司 | Tungsten oxide/sodium niobate composite material and preparation method and application thereof |
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Application publication date: 20160203 |