CN102749357B - 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
- Publication number
- CN102749357B CN102749357B CN201210231396.1A CN201210231396A CN102749357B CN 102749357 B CN102749357 B CN 102749357B CN 201210231396 A CN201210231396 A CN 201210231396A CN 102749357 B CN102749357 B CN 102749357B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- nanometer line
- carbide nanometer
- reactor
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
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 of preparing high-temperature gas sensors, especially relate to the method for preparing high-temperature gas sensors take silicon carbide nanometer line as gas sensitive.
Background technology
Along with scientific and technological development, increasing field, as Aeronautics and Astronautics, military affairs, communication, nuclear energy, commercial production and safety detection etc., in the urgent need to the gas sensor that can work under the harsh conditions such as high temperature, radioresistance.Most of gas sensitives can not meet the environment of this harshness.Silit has a series of excellent properties, as high thermal stability, strong chemical resistance, high saturated electron drift velocity, high critical breakdown electric field and high thermoconductivity etc., is suitable for manufacturing high temperature, high frequency, radioresistance and high-power electronic device.Have been reported with the hydrogen gas sensor of silicon carbide body material or film preparation at present, but still exist, response speed is slow, sensitivity is not high and high in cost of production series of problems.
Monodimension nanometer material has large specific surface area, and surfactivity is high, very responsive to physical and chemical factor, represents good application prospect in senser element.The fast development of one dimension silicon carbide nano material in recent years provides opportunity for the exploitation of new type high temperature gas sensitive.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 realize 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 method of preparing high-temperature gas sensors take silicon carbide nanometer line as gas sensitive.
The present invention is achieved by the following technical solutions, and concrete steps are as follows:
Take nano wire as gas sensitive, adopt electronation or the photoreduction met hod Surface Creation noble metal catalyst nano particle at nano wire, the nano wire centrifuging of then surperficial noble metal nano particles being modified, and be dispersed in ethanol ultrasonic its deposited mixture, then by nanowire suspended drop in high-temperature insulation material substrate, introduce metal electrode at the two ends of nano wire, and carry out annealing in process, then at the two ends of electrode lead-in conductor, realize the preparation of single nano-wire sensor; Described gas sensitive is silicon carbide nanometer line.
Chemical reduction method, in silicon carbide nanometer line Surface Creation Pt catalyst nanoparticles, by 0.1 gram of ultrasonic being dispersed in 10 ml water of silicon carbide nanometer line, is then the K of 20-30 mmol/L by 1 ml concentration
2ptCl
4join in suspending liquid with the ascorbic acid of 2 ml 0.1-0.5 mol/L, after concussion mixes, potpourri is placed in to 80oC water-bath and reacts 10-15 hour, then centrifuging, be dispersed in 10 ml ethanol ultrasonic acquisition deposited mixture, 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 by 5 ml concentration
2with the acetic acid aqueous solution that 20 ml concentration are 1-2%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that obtains 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 by 5ml concentration
3with the acetic acid aqueous solution that 20 ml concentration are 1-2%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that just can obtain 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 described employing is gold, silver and platinum.
The present invention is compared with background technology, and the useful effect having is:
1. the present invention utilizes SiC nano wire for gas sensitive, has realized the preparation of gas sensor under high temperature, has certain meaning for the gas sensing of working under the harsh conditions such as high temperature, high radiation preventing.
2. the finishing take noble metal nano particles (as: Pt, Pd and Ag) as silicon carbide nanometer line, the use of precious metal nano-particle catalyst, the reaction velocity and the sensitivity that have improved air-sensitive.
Accompanying drawing explanation
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 silicon carbide nanometer line pyrostat detects the time current curve of hydrogen.
Embodiment
A kind of embodiment preparing as gas sensitive high-temperature gas sensors take SiC nano wire:
Embodiment 1:
Chemical reduction method, in silicon carbide nanometer line Surface Creation Pt catalyst nanoparticles, by 0.1 gram of ultrasonic being dispersed in 10 ml water of silicon carbide nanometer line, is then 25mmol/L K by 1ml concentration
2ptCl
4the ascorbic acid that is 0.1mol/L with 2ml concentration joins in suspending liquid, after concussion mixes, potpourri is placed in to 80oC water-bath to react 12 hours, then centrifuging, be dispersed in 10 ml ethanol ultrasonic acquisition deposited mixture, obtain nanowire suspended liquid, as shown in Figure 1 the transmission electron microscope photo of silicon carbide nanometer line Surface Creation nano platinum particle.By nanowire suspended drop, on glass sheet, ag paste electrode on the two-end-point of nano wire, and carry out annealing in process, then introduces copper conductor at the two ends of electrode, realizes the preparation of single nanometer silicon carbide line sensor.
Nanometer silicon carbide line sensor is placed in to a high-temperature gas sensing testing device, under nitrogen protection, discontinuity be 4% hydrogen to passing into volumetric concentration in proving installation, realize over time air-sensitive based on measuring current and detect; As shown in Figure 2, under 600 oC high temperature, 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, in silicon carbide nanometer line Surface Creation Pt catalyst nanoparticles, by 0.1 gram of ultrasonic being dispersed in 10 ml water of silicon carbide nanometer line, is then the K of 20 mmol/L by 1 ml concentration
2ptCl
4join in suspending liquid with the ascorbic acid of 2 ml 0.5 mol/L, after concussion mixes, potpourri is placed in to 80oC water-bath and reacts 10 hours, then centrifuging, is dispersed in 10 ml ethanol ultrasonic acquisition deposited mixture, obtain nanowire suspended liquid, by nanowire suspended drop on glass sheet, ag paste electrode on the two-end-point of nano wire, and carry out annealing in process, then introduce copper conductor at the two ends of electrode, 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.Be the PdCl of 7 mmol/L by 5ml concentration
2with the acetic acid aqueous solution that 20ml concentration is 1.25%, be moved in the beaker that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that just can obtain surface deposition precious metals pd with drying and other steps.Nano wire alcohol suspension is dropped on glass sheet, gold electrode on the two-end-point of nano wire, and carry out annealing in process, and then introduce copper conductor at the two ends of electrode, realize the preparation of single nanometer silicon carbide line sensor.
Nanometer silicon carbide line sensor is placed in to a high-temperature gas sensing testing device; under nitrogen protection; discontinuity be 2% hydrogen to passing into volumetric concentration in proving installation; realize over time air-sensitive based on measuring current and detect, 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 by 5 ml concentration
2with the acetic acid aqueous solution that 20 ml concentration are 2%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that obtains 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.Be the AgNO of 7 mmol/L by 5ml concentration
3with the acetic acid aqueous solution that 20ml concentration is 1.25%, be moved in the beaker that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that just can obtain surface deposition precious metals ag with drying and other steps.Nano wire alcohol suspension is dropped on glass sheet, platinum electrode on the two-end-point of nano wire, and carry out annealing in process, and then introduce copper conductor at the two ends of electrode, realize the preparation of single nanometer silicon carbide line sensor.
Nanometer silicon carbide line sensor is placed in to a high-temperature gas sensing testing device; under nitrogen protection; discontinuity be 1% hydrogen to passing into volumetric concentration in proving installation; realize over time air-sensitive based on measuring current and detect, 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 by 5ml concentration
3with the acetic acid aqueous solution that 20 ml concentration are 1%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10 min, mixed liquor is transferred in quartz reactor.After reactor sealing, purge 20 min with High Purity Nitrogen, the oxygen in reactor removed. then, by lamp and high pressure mercury 6 h for reactor, then through centrifuging, embathe the silicon carbide nanometer line that just can obtain surface deposition precious metals ag with drying and other steps.
Claims (3)
1. prepare the method for gas sensor take silicon carbide nanometer line as gas sensitive for one kind, take nano wire as gas sensitive, adopt the Surface Creation noble metal catalyst nano particle of photoreduction met hod at nano wire, the nano wire centrifuging of then surperficial noble metal nano particles being modified, and be dispersed in ethanol ultrasonic its deposited mixture, then by nanowire suspended drop in high-temperature insulation material substrate, metal electrode is introduced at two ends at nano wire, and carry out annealing in process, then at the two ends of electrode lead-in conductor, realize the preparation of single nano-wire sensor; It is characterized in that: described gas sensitive is silicon carbide nanometer line; The step of the method is as follows:
Utilize photoreduction met hod at silicon carbide nanometer line surface deposition precious metals pd, the PdCl that is 5-10mmol/L by 5ml concentration
2with the acetic acid aqueous solution that 20ml concentration is 1-2%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10min, mixed liquor is transferred in quartz reactor; After reactor sealing, purge 20min with High Purity Nitrogen, the oxygen in reactor is removed; Then, by reactor lamp and high pressure mercury 6h, then through centrifuging, embathe the silicon carbide nanometer line that obtains surface deposition precious metals pd with drying steps;
Or utilize photoreduction met hod at silicon carbide nanometer line surface deposition precious metals ag, the AgNO that is 5-10mmol/L by 5ml concentration
3with the acetic acid aqueous solution that 20ml concentration is 1-2%, be moved in the container that contains 0.1 gram of silicon carbide nanometer line, with after supersonic oscillations 10min, mixed liquor is transferred in quartz reactor; After reactor sealing, purge 20min with High Purity Nitrogen, the oxygen in reactor is removed; Then, by reactor lamp and high pressure mercury 6h, then through centrifuging, embathe the silicon carbide nanometer line that obtains surface deposition precious metals ag with drying steps.
2. a kind of method of preparing gas sensor take silicon carbide nanometer line as gas sensitive according to claim 1, is characterized in that: quartz, aluminium oxide or glass high-temperature insulation material are selected in described high-temperature insulation material substrate.
3. a kind of method of preparing gas sensor take silicon carbide nanometer line as gas sensitive according to claim 1, is characterized in that: described metal electrode adopts gold, silver or platinum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210231396.1A CN102749357B (en) | 2012-07-05 | 2012-07-05 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210231396.1A CN102749357B (en) | 2012-07-05 | 2012-07-05 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102749357A CN102749357A (en) | 2012-10-24 |
| CN102749357B true CN102749357B (en) | 2014-05-14 |
Family
ID=47029719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210231396.1A Expired - Fee Related CN102749357B (en) | 2012-07-05 | 2012-07-05 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102749357B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149247B (en) * | 2013-03-04 | 2015-08-12 | 上海交通大学 | Loose thin-wall gas sensor and preparation method thereof |
| 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 |
| KR101765412B1 (en) * | 2016-02-23 | 2017-08-04 | 연세대학교 산학협력단 | Hydrogen sensor and method for manufacturing the same |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861521A (en) * | 2006-05-30 | 2006-11-15 | 浙江理工大学 | Synthesis process of needle shape nano silicon carbide |
-
2012
- 2012-07-05 CN CN201210231396.1A patent/CN102749357B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (4)
| Title |
|---|
| SiC nanowires: A photocatalytic nanomaterial;Weimin Zhou et al.;《APPLIED PHYSICS LETTERS》;20060705(第89期);013105 * |
| Simple approach toβ-SiC nanowires: Synthesis, optical, and electrical properties;Weimin Zhou et al.;《APPLIED PHYSICS LETTERS》;20061201(第89期);223124 * |
| Weimin Zhou et al..SiC nanowires: A photocatalytic nanomaterial.《APPLIED PHYSICS LETTERS》.2006,(第89期),013105. |
| Weimin Zhou et al..Simple approach toβ-SiC nanowires: Synthesis, optical, and electrical properties.《APPLIED PHYSICS LETTERS》.2006,(第89期),223124. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102749357A (en) | 2012-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102778478B (en) | Graphene-modified doped tin oxide composite material and preparation method thereof | |
| Choi et al. | Synthesis and gas sensing performance of ZnO–SnO2 nanofiber–nanowire stem-branch heterostructure | |
| Majhi et al. | Effect of Au nanorods on potential barrier modulation in morphologically controlled Au@ Cu2O core–shell nanoreactors for gas sensor applications | |
| Yin et al. | Improved gas sensing properties of silver-functionalized ZnSnO 3 hollow nanocubes | |
| Lin et al. | Highly stabilized and rapid sensing acetone sensor based on Au nanoparticle-decorated flower-like ZnO microstructures | |
| Li et al. | NiO-wrapped mesoporous TiO2 microspheres based selective ammonia sensor at room temperature | |
| Hou et al. | Room temperature gas sensing under UV light irradiation for Ti3C2Tx MXene derived lamellar TiO2-C/g-C3N4 composites | |
| CN102749357B (en) | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material | |
| Sun et al. | Application of photocatalytic materials in sensors | |
| Wang et al. | Synthesis of Au decorated SnO 2 mesoporous spheres with enhanced gas sensing performance | |
| CN103412008A (en) | Pd-doped SnO2 nanowire gas sensor for detecting H2 under low temperature, and preparation method thereof | |
| Wang et al. | Special nanostructure control of ethanol sensing characteristics based on Au@ In 2 O 3 sensor with good selectivity and rapid response | |
| CN110589875B (en) | Gas-sensitive nano material based on single-layer ordered tin oxide nano bowl branched zinc oxide nanowire structure, preparation process and application thereof | |
| Zu et al. | In situ synergistic crystallization-induced synthesis of novel Au nanostar-encrusted ZnO mesocrystals with high-quality heterojunctions for high-performance gas sensors | |
| Chang et al. | Heterostructural (Sr0. 6Bi0. 305) 2Bi2O7/ZnO for novel high-performance H2S sensor operating at low temperature | |
| CN104483365A (en) | Electrochemical gas sensing device adopting precious metal and graphene composite material as sensing electrode and production method of electrochemical gas sensing device | |
| Wang et al. | Microwave preparation and remarkable ethanol sensing properties of ZnO particles with controlled morphologies in water-ethylene glycol binary solvent system | |
| CN104849324A (en) | Resistance-type gas sensor based on graphene/multi-walled carbon nano-tube/zinc oxide composite material, and manufacturing method of resistance-type gas sensor | |
| Kang et al. | Highly sensitive detection of nitrite by using gold nanoparticle-decorated α-Fe 2 O 3 nanorod arrays as self-supporting photo-electrodes | |
| CN106093142B (en) | With SnO2Electric potential type NH is blended together for the YSZ base of sensitive electrode3Sensor and preparation method thereof | |
| Asgari et al. | Facile ultrasonic-assisted synthesis of SiO2/ZnO core/shell nanostructures: A selective ethanol sensor at low temperatures with enhanced recovery | |
| Liu et al. | Charge imbalance induced oxygen-adsorption enhances the gas-sensing properties of Al-doped SnO2 powders | |
| Zhao et al. | Black phosphorus nanosheets-sensitized Zn-doped α-Fe2O3 nanoclusters for trace acetone detection | |
| CN103364446A (en) | Preparation method of rare earth doped zinc oxide nanowire for gas sensor | |
| Li et al. | Highly Sensitive Ethanol Sensor Based on Au-Decorated SnO 2 Nanoparticles Synthesized Through Precipitation and Microwave Irradiation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140514 Termination date: 20150705 |
|
| EXPY | Termination of patent right or utility model |