CN102749357A - Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material - Google Patents
Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material Download PDFInfo
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- CN102749357A CN102749357A CN2012102313961A CN201210231396A CN102749357A CN 102749357 A CN102749357 A CN 102749357A CN 2012102313961 A CN2012102313961 A CN 2012102313961A CN 201210231396 A CN201210231396 A CN 201210231396A CN 102749357 A CN102749357 A CN 102749357A
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Abstract
The invention discloses a method of preparing a high temperature gas sensor with silicon carbide nanowires used as a gas sensitive material. In the invention, silicon carbide nanowires are used as a gas sensitive material, nanoparticles of a noble metal catalyst are formed on the surface of the silicon carbide nanowires, a material like quartz, alumina or glass is used as a substrate, the silicon carbide nanowires are disposed on the substrate, metals like gold, silver and platinum are used as electrodes and are subjected to annealing treatment, and then leads are introduced at two ends of the electrodes so as to realize preparation of a single-nanowire sensor. According to the invention, through utilization of the SiC nanowires as a gas sensitive material, preparation of the gas sensor at a high temperature is realized, which is of significance to gas sensing under severe working conditions like high temperature and high radiation resistance; noble metal nanoparticles (such as Pt, Pd and Ag ) are used for surface modification of the silicon carbide nanowires, and utilization of the noble metal nanoparticle catalyst enables the response speed and sensitivity of the gas sensor to be improved.
Description
Technical field
The present invention relates to a kind of method for preparing high-temperature gas sensors, especially relating to the silicon carbide nanometer line is the method that gas sensitive prepares high-temperature gas sensors.
Background technology
Along with development of science and technology, growing field like Aeronautics and Astronautics, military affairs, communication, nuclear energy, commercial production and safety detection etc., presses for the gas sensor that can under harsh conditions such as high temperature, radioresistance, work.Most of gas sensitives can not satisfy this rigorous environment.Silit has a series of excellent properties, like high thermal stability, strong chemical resistance, high saturated electron drift velocity, high critical breakdown electric field and high thermoconductivity etc., is suitable for making high temperature, high frequency, radioresistance and high-power electronic device.With the existing report of the hydrogen gas sensor of silicon carbide body material or film preparation, response speed is slow, sensitivity is not high and the high serial problem of cost but still exist at present.
Monodimension nanometer material has big specific surface area, and surfactivity is high, and is very responsive to physics and chemical environment, in senser element, represents good application prospects.The fast development of one dimension silicon carbide nano material in recent years is that the exploitation of new type high temperature gas sensitive provides opportunity.Based on the advantage of carbofrax material, the preparation of one dimension silicon carbide nano material high-temperature hydrogen sensor is significant for the exploitation of high-temperature gas sensors.
Summary of the invention
In order to be implemented in the gas sensing of working under the harsh conditions such as high temperature, high radiation preventing, improve gas sensing sensitivity and reaction velocity, the object of the present invention is to provide a kind of is the method that gas sensitive prepares high-temperature gas sensors with the silicon carbide nanometer line.
The present invention realizes that through following technical scheme concrete steps are following:
With the nano wire is gas sensitive, adopts electronation or photoreduction met hod and generates the noble metal catalyst nano particle on the surface of nano wire, the nano wire centrifuging of then surperficial noble metal nano particles being modified; And be dispersed in the ethanol its deposited mixture is ultrasonic; Then with nanowire suspended drop in the high-temperature insulation material substrate, introduce metal electrode at the two ends of nano wire, and carry out annealing in process; The lead-in conductor at the two ends of electrode is realized the preparation of single nano-wire sensor then; Described gas sensitive is a silicon carbide nanometer line.
Chemical reduction method generates the Pt catalyst nanoparticles on silicon carbide nanometer line surface, silicon carbide nanometer line is ultrasonic is dispersed in the 10 ml water with 0.1 gram, is the K of 20-30 mmol/L with 1 ml concentration then
2PtCl
4Join in the suspending liquid with the ascorbic acid of 2 ml 0.1-0.5 mol/L; After concussion mixes; Potpourri is placed 80oC water-bath reaction 10-15 hour; Centrifuging then will obtain that deposited mixture is ultrasonic to be dispersed in the 10 ml ethanol, obtain the silicon carbide nanometer line of surface deposition precious metals pt.
Utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals pd, is the PdCl of 5-10 mmol/L with 5 ml concentration
2With 20 ml concentration be the acetic acid aqueous solution of 1-2%, be moved into contain 0.1 the gram silicon carbide nanometer line container in, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that obtains the surface deposition precious metals pd with drying steps.
Utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals ag, is the AgNO of 5-10 mmol/L with 5ml concentration
3With 20 ml concentration be the acetic acid aqueous solution of 1-2%, be moved into contain 0.1 the gram silicon carbide nanometer line container in, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that just can obtain the surface deposition precious metals ag with drying and other steps.
Described high-temperature insulation material substrate is with quartz, aluminium oxide or glass high-temperature insulation material.
The electrode of said employing is gold, silver and platinum.
The present invention compares with background technology, and the useful effect that has is:
1. the present invention utilizes the SiC nano wire to be gas sensitive, has realized the preparation of gas sensor under the high temperature, has certain meaning for the gas sensing of working under the harsh conditions such as high temperature, high radiation preventing.
2. be the finishing of silicon carbide nanometer line with noble metal nano particles (as: Pt, Pd and Ag), the use of precious metal nano-particle catalyst, the reaction velocity and the sensitivity that have improved air-sensitive.
Description of drawings
Fig. 1 is the transmission electron microscope photo that silicon carbide nanometer line surface nano platinum particle is modified.
Fig. 2 is under 600 oC high temperature, and the silicon carbide nanometer line pyrostat detects the time current curve of hydrogen.
Embodiment
A kind of is the embodiment of gas sensitive high-temperature gas sensors preparation with the SiC nano wire:
Embodiment 1:
Chemical reduction method generates the Pt catalyst nanoparticles on silicon carbide nanometer line surface, silicon carbide nanometer line is ultrasonic is dispersed in the 10 ml water with 0.1 gram, is 25mmol/L K with 1ml concentration then
2PtCl
4With 2ml concentration be that the ascorbic acid of 0.1mol/L joins in the suspending liquid; After concussion mixes; Potpourri was placed 80oC water-bath reaction 12 hours, and centrifuging then will obtain that deposited mixture is ultrasonic to be dispersed in the 10 ml ethanol; Obtain nanowire suspended liquid, silicon carbide nanometer line as shown in Figure 1 surface generates the transmission electron microscope photo of nano platinum particle.On glass sheet, ag paste electrode on the two-end-point of nano wire, and carry out annealing in process is introduced copper conductor at the two ends of electrode then, realizes the preparation of single nanometer silicon carbide line sensor with nanowire suspended drop.
The nanometer silicon carbide line sensor is placed a high-temperature gas sensing testing device, and under nitrogen protection, the feeding volumetric concentration in proving installation of discontinuity is 4% hydrogen, realizes over time that based on measuring current air-sensitive detects; As shown in Figure 2, under 600 oC high temperature, the silicon carbide nanometer line pyrostat detects the time current curve of hydrogen, and this sensor has high sensitivity and fast reaction velocity to hydrogen.
Embodiment 2:
Chemical reduction method generates the Pt catalyst nanoparticles on silicon carbide nanometer line surface, silicon carbide nanometer line is ultrasonic is dispersed in the 10 ml water with 0.1 gram, is the K of 20 mmol/L with 1 ml concentration then
2PtCl
4Join in the suspending liquid with the ascorbic acid of 2 ml, 0.5 mol/L, after concussion mixes, potpourri is placed 80oC water-bath reaction 10 hours; Centrifuging then will obtain that deposited mixture is ultrasonic to be dispersed in the 10 ml ethanol, obtain nanowire suspended liquid; With nanowire suspended drop on glass sheet, ag paste electrode on the two-end-point of nano wire, and carry out annealing in process; Introduce copper conductor at the two ends of electrode then, realize the preparation of single nanometer silicon carbide line sensor.
Embodiment 3:
Utilize photoreduction met hod at silicon carbide nanometer line surface deposition precious metals pd nano particle.With 5ml concentration is the PdCl of 7 mmol/L
2With 20ml concentration be 1.25% acetic acid aqueous solution, be moved in the beaker that contains 0.1 gram silicon carbide nanometer line, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that just can obtain the surface deposition precious metals pd with drying and other steps.The nano wire alcohol suspension is dropped on the glass sheet, gold electrode on the two-end-point of nano wire, and carry out annealing in process, and introduce copper conductor at the two ends of electrode then, realize the preparation of single nanometer silicon carbide line sensor.
The nanometer silicon carbide line sensor is placed a high-temperature gas sensing testing device; Under nitrogen protection; The feeding volumetric concentration in proving installation of discontinuity is 2% hydrogen; Realize over time that based on measuring current air-sensitive detects, this sensor has high sensitivity and fast reaction velocity to hydrogen.
Embodiment 4:
Utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals pd nano particle, is the PdCl of 5 mmol/L with 5 ml concentration
2With 20 ml concentration be 2% acetic acid aqueous solution, be moved in the container that contains 0.1 gram silicon carbide nanometer line, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that obtains the surface deposition precious metals pd with drying steps.
Embodiment 5:
Utilize photoreduction met hod at silicon carbide nanometer line surface deposition precious metals ag nano particle.With 5ml concentration is the AgNO of 7 mmol/L
3With 20ml concentration be 1.25% acetic acid aqueous solution, be moved in the beaker that contains 0.1 gram silicon carbide nanometer line, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that just can obtain the surface deposition precious metals ag with drying and other steps.The nano wire alcohol suspension is dropped on the glass sheet, platinum electrode on the two-end-point of nano wire, and carry out annealing in process, and introduce copper conductor at the two ends of electrode then, realize the preparation of single nanometer silicon carbide line sensor.
The nanometer silicon carbide line sensor is placed a high-temperature gas sensing testing device; Under nitrogen protection; The feeding volumetric concentration in proving installation of discontinuity is 1% hydrogen; Realize over time that based on measuring current air-sensitive detects, this sensor has high sensitivity and fast reaction velocity to hydrogen.
Embodiment 6:
Utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals ag nano particle, is the AgNO of 10 mmol/L with 5ml concentration
3With 20 ml concentration be 1% acetic acid aqueous solution, be moved in the container that contains 0.1 gram silicon carbide nanometer line, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor.After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that just can obtain the surface deposition precious metals ag with drying and other steps.
Claims (6)
1. one kind is the method that gas sensitive prepares gas sensor with the silicon carbide nanometer line; With the nano wire is gas sensitive, adopts electronation or photoreduction met hod and generates the noble metal catalyst nano particle on the surface of nano wire, the nano wire centrifuging of then surperficial noble metal nano particles being modified; And be dispersed in the ethanol its deposited mixture is ultrasonic; Then with nanowire suspended drop in the high-temperature insulation material substrate, introduce metal electrode at the two ends of nano wire, and carry out annealing in process; The lead-in conductor at the two ends of electrode is realized the preparation of single nano-wire sensor then; It is characterized in that: described gas sensitive is a silicon carbide nanometer line.
2. according to claim 1 a kind of be the method that gas sensitive prepares gas sensor with the silicon carbide nanometer line; It is characterized in that: chemical reduction method generates the Pt catalyst nanoparticles on the silicon carbide nanometer line surface; Silicon carbide nanometer line is ultrasonic is dispersed in the 10 ml water with 0.1 gram, is the K of 20-30 mmol/L with 1 ml concentration then
2PtCl
4Join in the suspending liquid with the ascorbic acid of 2 ml 0.1-0.5 mol/L; After concussion mixes; Potpourri is placed 80oC water-bath reaction 10-15 hour; Centrifuging then will obtain that deposited mixture is ultrasonic to be dispersed in the 10 ml ethanol, obtain the silicon carbide nanometer line of surface deposition precious metals pt.
3. according to claim 1 a kind of be the method that gas sensitive prepares gas sensor with the silicon carbide nanometer line, it is characterized in that: utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals pd, is the PdCl of 5-10 mmol/L with 5 ml concentration
2With 20 ml concentration be the acetic acid aqueous solution of 1-2%, be moved into contain 0.1 the gram silicon carbide nanometer line container in, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor; After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that obtains the surface deposition precious metals pd with drying steps.
4. according to claim 1 a kind of be the method that gas sensitive prepares gas sensor with the silicon carbide nanometer line, it is characterized in that: utilizing photoreduction met hod at silicon carbide nanometer line surface deposition precious metals ag, is the AgNO of 5-10 mmol/L with 5ml concentration
3With 20 ml concentration be the acetic acid aqueous solution of 1-2%, be moved into contain 0.1 the gram silicon carbide nanometer line container in, behind supersonic oscillations 10 min, mixed liquor is transferred in the quartz reactor; After the reactor sealing, purge 20 min, the oxygen in the reactor removed with high purity nitrogen. then, with reactor with lamp and high pressure mercury 6 h, again through centrifuging, embathe the silicon carbide nanometer line that just can obtain the surface deposition precious metals ag with drying and other steps.
5. according to claim 1 a kind of be the method that gas sensitive prepares high-temperature gas sensors with the silicon carbide nanometer line, it is characterized in that: described high-temperature insulation material substrate is for quartzy, aluminium oxide or glass high-temperature insulation material.
6. according to claim 1 a kind of be the method that gas sensitive prepares high-temperature gas sensors with the silicon carbide nanometer line, it is characterized in that: the electrode of said employing is gold, silver and platinum.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149247A (en) * | 2013-03-04 | 2013-06-12 | 上海交通大学 | Loose thin-wall gas sensitive element and manufacturing method thereof |
| CN105428184A (en) * | 2015-11-06 | 2016-03-23 | 宁波工程学院 | Preparation method for SiC nano wire decorated with Au nano particles |
| CN107102033A (en) * | 2016-02-23 | 2017-08-29 | 延世大学校产协力团 | Hydrogen sensor and preparation method thereof |
| CN113945611A (en) * | 2021-09-06 | 2022-01-18 | 复旦大学 | Heterogeneous gas-sensitive nano material based on cerium oxide particle modified copper oxide nanowire structure, preparation process and application thereof |
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| CN1861521A (en) * | 2006-05-30 | 2006-11-15 | 浙江理工大学 | Synthesis process of needle shape nano silicon carbide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1861521A (en) * | 2006-05-30 | 2006-11-15 | 浙江理工大学 | Synthesis process of needle shape nano silicon carbide |
Non-Patent Citations (3)
| Title |
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| 《APPLIED PHYSICS LETTERS》 20061201 Weimin Zhou et al. Simple approach tobeta-SiC nanowires: Synthesis, optical, and electrical properties 223124 1、5-6 , 第89期 * |
| WEIMIN ZHOU ET AL.: "SiC nanowires: A photocatalytic nanomaterial", 《APPLIED PHYSICS LETTERS》 * |
| WEIMIN ZHOU ET AL.: "Simple approach toβ-SiC nanowires: Synthesis, optical, and electrical properties", 《APPLIED PHYSICS LETTERS》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149247A (en) * | 2013-03-04 | 2013-06-12 | 上海交通大学 | Loose thin-wall gas sensitive element and manufacturing method thereof |
| CN105428184A (en) * | 2015-11-06 | 2016-03-23 | 宁波工程学院 | Preparation method for SiC nano wire decorated with Au nano particles |
| CN105428184B (en) * | 2015-11-06 | 2017-09-26 | 宁波工程学院 | A kind of preparation method of the nano-particle modified SiC nanowires of Au |
| CN107102033A (en) * | 2016-02-23 | 2017-08-29 | 延世大学校产协力团 | Hydrogen sensor and preparation method thereof |
| CN107102033B (en) * | 2016-02-23 | 2020-01-03 | 新星C&T | Hydrogen sensor and preparation method thereof |
| CN113945611A (en) * | 2021-09-06 | 2022-01-18 | 复旦大学 | Heterogeneous gas-sensitive nano material based on cerium oxide particle modified copper oxide nanowire structure, preparation process and application thereof |
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