CN102012386A - Preparation method of nitric oxide gas sensor element based on pseudodirected tungsten trioxide nano tape - Google Patents
Preparation method of nitric oxide gas sensor element based on pseudodirected tungsten trioxide nano tape Download PDFInfo
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- CN102012386A CN102012386A CN 201010517340 CN201010517340A CN102012386A CN 102012386 A CN102012386 A CN 102012386A CN 201010517340 CN201010517340 CN 201010517340 CN 201010517340 A CN201010517340 A CN 201010517340A CN 102012386 A CN102012386 A CN 102012386A
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Abstract
The invention discloses a preparation method of a nitric oxide gas sensor element based on a pseudodirected tungsten trioxide nano tape, which comprises the steps of: 1, preparing a tungsten hexachloride solution; 2, regulating the mol concentration of tungsten hexachloride to be 0.003-0.012M; 3, synthesizing a pseudodirected tungsten oxide nano wire; 4, preparing a pseudodirected tungsten oxide nano wire; 5, preparing a sensitive material slurry; and 6, preparing the sensor element based on the pseudodirected tungsten trioxide nano tape. The sensor element based on the pseudodirected tungsten trioxide nano tape, prepared by using the method, has the advantages of high sensitivity, high selectivity, low working temperature and low power consumption for the low-concentration nitric oxide gas detection.
Description
Technical field
The invention relates to oxides of nitrogen gas sensors, relate in particular to a kind of based on certainly to the preparation method of the oxides of nitrogen gas sensors element of tungsten trioxide nano band.
Background technology
The modern industry development has produced a large amount of inflammable, explosive, poisonous harmful gases, wherein oxides of nitrogen (NO
X) be a kind of Typical Air Pollution thing that causes serious environmental problems such as acid rain, photo-chemical smog and human health is brought grave danger.Research is used for NO
XAccurate detection and the high-performance gas sensor material of monitoring and device significant to protection environment and human health.Metal oxide semiconductor is that a class is to NO
XHave good sensitivity can gas sensitive, its gas sensing mechanism belongs to the surface resistance control type, and the detection of gas is based on oxygen and the tested gas modulated process at semiconductor grain surface adsorption and reaction pair tungsten oxide semiconductor surface resistance.In the many decades in the past, the scientific worker has carried out broad research to various conductor oxidates.The result shows that n type tungsten oxide semiconductor is to NO
XGas has very high sensitivity and selectivity, is the NO that a kind of utmost point has research and application prospect
XSensitive material.
Along with the enhancing of environmental consciousness, people are to the demands for higher performance of oxides of nitrogen gas sensors.The researchist also constantly improves the sensitive property of gas sensor always at the sensitive material by research and development new structure and composition, as passing through precious metal doping, formation composite oxide material, preparation has the nanostructured tungsten oxide of high activity surface etc.Begin one's study quasi-one-dimensional tungsten oxide nanostructured such as nanotube, nano wire and nanometer rods possibility of its application in oxides of nitrogen gas sensors of people in recent years particularly.Although present research only is in the starting stage, relevant report is less, but from these few research reports of quantity, can find, thereby since accurate one dimension tungsten oxide nano structural material have high specific surface area with and vertical axial size and Debye length is comparable can obtain higher gas sensitivity, better choice and lower working temperature, shown the bright prospect that this class material is used in the high-performance oxides of nitrogen gas sensors.Yet, for the nanostructure-based gas sensor of the accurate one dimension tungsten oxide of this class, its NO
XSensitive property still has very big room for promotion, because the optimum working temperature of the type sensor is still than higher, about 200 ℃, high working temperature has been brought high power consumption usually; And, the type sensor is still lower to the sensitivity of low-concentration nitrogen oxide gas, for example, people such as ReitArtzi-Gerlitz (ReitArtzi-Gerlitzet al.sensors and Actuators B 2009,136:257) the tungsten oxide nanotube that utilized the template assistant depositing and investigated it to NO
2The sensitivity response of gas, the tungsten oxide nanotube is to 0.2ppm NO when finding 200 ℃
2Sensitivity be about 4; People such as ZhifuLiu (Zhifu Liu, et al.sensors and Actuators B 2009,140:514) report tungsten oxide nanorod microspheres material in the time of 200 ℃ to 1ppmNO
2Sensitivity maxima be about 20, and our problem group (Yuxiang Qin et al.sensors andActuators B, 150:339,2010) is to the NO of the tungsten oxide nano wire of solvent thermal synthesis
2The gas sensitization The Characteristic Study shows that in the time of 200 ℃, the tungsten oxide nano wire is to 1ppm NO
2Sensitivity only be 13.4, therefore, still there are very big gap in the sensitive property of present accurate one dimension tungsten oxide nanostructured and current high performance demands to low-power consumption, high sensitivity, integrated NOx sensor.
Summary of the invention
The objective of the invention is to further improve the sensitive property of tungsten oxide nano wire base gas sensor to oxides of nitrogen gas, provide a kind of utilization certainly in air atmosphere, to anneal preparation certainly to the method for tungsten trioxide nano band gas sensitive to the tungsten oxide nano wire bundle, and provide then a kind of to oxides of nitrogen gas have high sensitivity, high selectivity certainly to the preparation method of tungsten trioxide nano belt sensor element.
The present invention has following steps:
(1) tungsten hexachloride is dissolved in 50 milliliters of n-propanols or the cyclohexanol, the addition of described n-propanol or cyclohexanol is lower than the addition of initial concentration, and magnetic agitation 0.5 hour forms blue transparent tungsten hexachloride solution;
(2) the tungsten hexachloride solution for continuous in step (1) is added n-propanol or cyclohexanol, and the volumetric molar concentration of regulating tungsten hexachloride is 0.003～0.012M;
(3) to be transferred to 100～500 milliliters liner be in the stainless steel hydrothermal reaction kettle of teflon to the tungsten hexachloride solution that step (2) is obtained, sealing, under 180～200 ℃ temperature, adopt then solvent-thermal method synthetic certainly to the tungsten oxide nano wire, the solvent thermal reaction time is 6～10 hours, the reactor natural cooling;
(4) with the hot product centrifuging of the solvent in the step (3), fully dry under 70 ℃ air atmosphere behind deionized water and absolute ethyl alcohol cyclic washing, make certainly to the tungsten oxide nano wire;
(5) step (4) is obtained certainly to tungsten oxide nano wire and volume ratio be that 1: 2 absolute ethyl alcohol mixes with terpinol, ultrasonic mixing 2 hours makes sensitive material slurry;
(6) sensitive material slurry described in the step (5) is coated on the alumina substrate that is covered with interdigital platinum electrode, placed 30 minutes under the room temperature, in the program sintering furnace in 400～600 ℃ of air atmosphere thermal treatments 1～2 hour, the control heating rate makes certainly to tungsten trioxide nano tape base sensor element less than 2.5 ℃/min.
Described step (4) certainly to the tungsten oxide nano wire be the pencil form and exist, the diameter of nano wire bundle is 60～90 nanometers, length is 500～1000 nanometers, the single nano-wire diameter that constitutes nanometer bundle is 5～10 nanometers.
The interdigital platinum electrode that is covered with on the alumina substrate of described step (6) is to adopt the radio-frequency magnetron sputter method preparation on the alumina substrate surface of cleaning, and thickness is 100～150 nanometers.
The sensitive material slurry of described step (6) adopts spin-coating method, print process or czochralski method to be coated on the alumina substrate that is covered with interdigital platinum electrode.
The invention has the beneficial effects as follows, provide a kind of for low-concentration nitrogen oxide gas have high sensitivity, high selectivity, low working temperature, low-power consumption certainly to the preparation method of tungsten trioxide nano belt sensor element.
Description of drawings
Fig. 1 be embodiment 6 certainly to the electron scanning micrograph of tungsten oxide nano wire;
Fig. 2 be embodiment 6 certainly to the electron scanning micrograph of tungsten trioxide nano band;
Fig. 3 be 450 ℃ of annealing certainly to tungsten trioxide nano belt sensor element under the different operating temperature to 1ppmNO
2The sensitivity of gas;
Fig. 4 be 450 ℃ of annealing certainly to tungsten trioxide nano belt sensor element under 100 ℃ to NO
2The dynamic response curve of gas;
Fig. 5 be 450 ℃ of annealing certainly to tungsten trioxide nano belt sensor element selectivity synoptic diagram to gas with various during at 100 ℃.
Embodiment
The present invention adopts WCl
6As reaction W source, adopt solvent-thermal method synthetic certainly to the tungsten oxide nano wire bundle, the organic ink of tungsten oxide nano wire bundle is coated in the sensor substrate surface, air atmosphere annealing forms certainly to tungsten trioxide nano tape base gas sensor element.
The present invention is raw materials used all to adopt commercially available chemically pure reagent, with WCl
6As reaction W source, as synthetic, adopt solvent-thermal method synthetic with n-propanol or cyclohexanol certainly to tungsten oxide nano wire bundle (step (1)～(4)), preparation certainly sees table 1 for details to the specific embodiment of tungsten oxide nano wire bundle.
Table 1
With table 1 preparation be original material certainly to the tungsten oxide nano wire bundle, preparation is certainly to tungsten trioxide nano tape base gas sensor element (step (5)～(6)), specific embodiment sees table 2 for details.
Table 2
In the table 2 embodiment 6 prepared certainly as shown in Figure 2 to the scanning electron microscope analysis result on tungsten trioxide nano band air-sensitive film surface.
The 6th the nano wire bundle material that specific embodiment is prepared by tungsten oxide nano wire bundle material, adopt certainly to the 6th specific embodiment of tungsten trioxide nano tape base gas sensor element prepared certainly to tungsten trioxide nano tape base gas sensor element, its under the different operating temperature to 1ppm NO
2The sensitivity of gas and under 100 ℃ of working temperatures to variable concentrations NO
2The dynamic response curve of gas respectively as shown in Figure 3 and Figure 4.As can be seen from Figure 3, the optimum working temperature of this tungsten trioxide nano tape base gas sensor element is 100 ℃.As seen from Figure 4, this sensor element is to low concentration of NO
2Gas has the response of tangible gas, under 100 ℃ of optimum working temperatures, to 0.2,0.4,1 and 2ppm NO
2The sensitivity of gas is respectively up to 120,476,836 and 1095, and this sensor element has good reversibility and NO fast
2The gas response characteristic, its response time is lower than 30s.
The 6th the nano wire bundle material that specific embodiment is prepared by tungsten oxide nano wire bundle material, adopt certainly to the 6th specific embodiment of tungsten trioxide nano tape base gas sensor element prepared certainly to tungsten trioxide nano tape base gas sensor element, its in the time of 100 ℃ to the selectivity of gas with various as shown in Figure 5.As can be seen from Figure 5, this certainly to tungsten trioxide nano tape base gas sensor element to 1ppmNO
2, 200ppmNH
3, the 200ppm alcohol vapour sensitivity be respectively 836.26,1.57,1.21, show in this invention preparation certainly to tungsten trioxide nano tape base gas sensor element during at 100 ℃ to NO
2Gas has splendid selectivity.
Claims (4)
- One kind based on certainly to the preparation method of the oxides of nitrogen gas sensors element of tungsten trioxide nano band, have following steps:(1) tungsten hexachloride is dissolved in 50 milliliters of n-propanols or the cyclohexanol, the addition of described n-propanol or cyclohexanol is lower than the addition of initial concentration, and magnetic agitation 0.5 hour forms blue transparent tungsten hexachloride solution;(2) the tungsten hexachloride solution for continuous in step (1) is added n-propanol or cyclohexanol, and the volumetric molar concentration of regulating tungsten hexachloride is 0.003～0.012M;(3) to be transferred to 100～500 milliliters liner be in the stainless steel hydrothermal reaction kettle of teflon to the tungsten hexachloride solution that step (2) is obtained, sealing, under 180～200 ℃ temperature, adopt then solvent-thermal method synthetic certainly to the tungsten oxide nano wire, the solvent thermal reaction time is 6～10 hours, the reactor natural cooling;(4) with the hot product centrifuging of the solvent in the step (3), fully dry under 70 ℃ air atmosphere behind deionized water and absolute ethyl alcohol cyclic washing, make certainly to the tungsten oxide nano wire;(5) step (4) is obtained certainly to tungsten oxide nano wire and volume ratio be that 1: 2 absolute ethyl alcohol mixes with terpinol, ultrasonic mixing 2 hours makes sensitive material slurry;(6) sensitive material slurry described in the step (5) is coated on the alumina substrate that is covered with interdigital platinum electrode, placed 30 minutes under the room temperature, in the program sintering furnace in 400～600 ℃ of air atmosphere thermal treatments 1～2 hour, the control heating rate makes certainly to tungsten trioxide nano tape base sensor element less than 2.5 ℃/min.
- According to claim 1 based on certainly to the preparation method of the oxides of nitrogen gas sensors element of tungsten trioxide nano band, it is characterized in that, described step (4) certainly to the tungsten oxide nano wire be the pencil form and exist, the diameter of nano wire bundle is 60～90 nanometers, length is 500～1000 nanometers, and the single nano-wire diameter that constitutes nanometer bundle is 5～10 nanometers.
- According to claim 1 based on certainly to the preparation method of the oxides of nitrogen gas sensors element of tungsten trioxide nano band, it is characterized in that, the interdigital platinum electrode that is covered with on the alumina substrate of described step (6), be to adopt the radio-frequency magnetron sputter method preparation on the alumina substrate surface of cleaning, thickness is 100～150 nanometers.
- According to claim 1 based on certainly to the preparation method of the oxides of nitrogen gas sensors element of tungsten trioxide nano band, it is characterized in that the sensitive material slurry of described step (6) adopts spin-coating method, print process or czochralski method to be coated on the alumina substrate that is covered with interdigital platinum electrode.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102495109A (en) * | 2011-12-07 | 2012-06-13 | 天津大学 | Preparation method of nitrogen oxide sensor component based on WO3 single-crystal particle |
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
| CN103570070A (en) * | 2013-11-07 | 2014-02-12 | 东华大学 | Preparation method of self-assembly W18049 nanostructure |
| CN103852496A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires |
| CN104627959A (en) * | 2015-01-28 | 2015-05-20 | 天津大学 | Preparation method for porous silicon-based orderly tungsten oxide nanorod composite structure |
| CN105954325A (en) * | 2016-04-28 | 2016-09-21 | 华北水利水电大学 | Preparation method for preparing rod-shaped tungsten trioxide nano gas-sensitive material |
| CN106865997A (en) * | 2017-02-21 | 2017-06-20 | 上海第二工业大学 | A kind of method that tungsten oxide film is directly grown on electro-conductive glass |
| CN107055618A (en) * | 2016-12-23 | 2017-08-18 | 青岛大学 | Preparation method while a kind of tungsten oxide quantum dot and tungsten oxide nano |
| CN107915212A (en) * | 2016-10-08 | 2018-04-17 | 中国科学院大连化学物理研究所 | Caterpillar shape WN nano materials that lamella stacks and preparation method thereof |
| CN109298027A (en) * | 2017-07-25 | 2019-02-01 | 天津大学 | Gas sensor and preparation method thereof based on the nano-particle modified tungsten oxide nanometer stick of tellurium oxide |
| CN113511682A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | Doping of WO3Nanowire, preparation method thereof and gas sensor |
| CN114813724A (en) * | 2022-06-28 | 2022-07-29 | 安徽维纳物联科技有限公司 | Nitrogen oxide detection system and preparation method thereof |
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Cited By (16)
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| CN102495109A (en) * | 2011-12-07 | 2012-06-13 | 天津大学 | Preparation method of nitrogen oxide sensor component based on WO3 single-crystal particle |
| CN103570070A (en) * | 2013-11-07 | 2014-02-12 | 东华大学 | Preparation method of self-assembly W18049 nanostructure |
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
| CN103852496A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires |
| CN104627959A (en) * | 2015-01-28 | 2015-05-20 | 天津大学 | Preparation method for porous silicon-based orderly tungsten oxide nanorod composite structure |
| CN105954325A (en) * | 2016-04-28 | 2016-09-21 | 华北水利水电大学 | Preparation method for preparing rod-shaped tungsten trioxide nano gas-sensitive material |
| CN105954325B (en) * | 2016-04-28 | 2018-10-30 | 华北水利水电大学 | A kind of preparation method of rodlike tungsten trioxide nano gas sensitive |
| CN107915212A (en) * | 2016-10-08 | 2018-04-17 | 中国科学院大连化学物理研究所 | Caterpillar shape WN nano materials that lamella stacks and preparation method thereof |
| CN107055618A (en) * | 2016-12-23 | 2017-08-18 | 青岛大学 | Preparation method while a kind of tungsten oxide quantum dot and tungsten oxide nano |
| CN107055618B (en) * | 2016-12-23 | 2018-05-29 | 青岛大学 | Preparation method while a kind of tungsten oxide quantum dot and tungsten oxide nano |
| CN106865997A (en) * | 2017-02-21 | 2017-06-20 | 上海第二工业大学 | A kind of method that tungsten oxide film is directly grown on electro-conductive glass |
| CN106865997B (en) * | 2017-02-21 | 2019-06-07 | 上海第二工业大学 | A method of growing tungsten oxide film directly on electro-conductive glass |
| CN109298027A (en) * | 2017-07-25 | 2019-02-01 | 天津大学 | Gas sensor and preparation method thereof based on the nano-particle modified tungsten oxide nanometer stick of tellurium oxide |
| CN113511682A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | Doping of WO3Nanowire, preparation method thereof and gas sensor |
| CN113511682B (en) * | 2020-04-10 | 2023-12-22 | 中国石油化工股份有限公司 | Doping WO 3 Nanowire, preparation method thereof and gas sensor |
| CN114813724A (en) * | 2022-06-28 | 2022-07-29 | 安徽维纳物联科技有限公司 | Nitrogen oxide detection system and preparation method thereof |
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Application publication date: 20110413 |