CN106018493A - Electrical equipment inspection system based on hazardous gas detection - Google Patents

Electrical equipment inspection system based on hazardous gas detection Download PDF

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Publication number
CN106018493A
CN106018493A CN201610429219.2A CN201610429219A CN106018493A CN 106018493 A CN106018493 A CN 106018493A CN 201610429219 A CN201610429219 A CN 201610429219A CN 106018493 A CN106018493 A CN 106018493A
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film
sno
silicon chip
gas
nano wire
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杨林
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention relates to an electrical equipment inspection system based on hazardous gas detection. The inspection system is provided with a CO gas sensor. The CO gas sensor comprises a Si substrate, a silicon oxide film formed on the Si substrate, a W film arranged on the silicon oxide film, a WO2 nanowire film formed on the W film, a SNO2 nano-film coating the WO3 nanowire film, two Pt electrodes manufactured on the SnO2 nano-film and a heating module located on the Si substrate. The inspection system is high in sensitivity for CO gas, short in reaction time and better in both repeatability and stability.

Description

A kind of power equipment inspection system based on hazardous gas detection
Technical field
The application relates to electric power and inspects field, particularly relates to a kind of electric power based on hazardous gas detection and sets Standby inspection system.
Background technology
Power equipment inspection system is to be applied to power industry, is mainly used in checking, making an inspection tour power equipment The security system of normal operating parameters, is based primarily upon detection of electrical leakage, voltage detecting, current detecting etc..
But, along with expanding economy, the applied environment of power equipment complicates day by day, such as tests Room environmental, chemical industry site surrounding etc., in some special environments, can dangerous gas, such as CO Deng, but, existing power equipment inspection system does not the most possess the detection function of specific gas.
Summary of the invention
For overcoming problem present in correlation technique, the application provides a kind of based on hazardous gas detection Power equipment inspection system.
The present invention is achieved through the following technical solutions: a kind of power equipment inspection based on hazardous gas detection Viewing system, this inspection system is provided with CO gas sensor;Described CO gas sensor includes Si Substrate, the W being formed at the suprabasil silicon oxide film of described Si, being placed on described silicon oxide film Film, the WO being formed on W film3Nano wire film, it is overlying on WO3SnO on nano wire film2 Nano thin-film, at SnO2On nano thin-film make two Pt electrodes and be positioned at below described Si substrate Heating module;Described WO3Nanowire length is 500~1500nm.
Preferably, the preparation method of CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 600nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 7g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 63 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
The technical scheme that embodiments herein provides can include following beneficial effect:
(1) a kind of based on hazardous gas detection the power equipment inspection that embodiments herein is provided Viewing system, it is provided with CO gas sensor, and this CO gas sensor is based on SnO2Nanometer The resistor-type CO sensor of material, passes through WO3Nano wire and SnO2The combination of nano material, increases The aspect effects such as selectivity that CO is detected by strong CO gas sensor, stability;CO gas Sensor is at WO3On the basis of nano wire film, coat one layer of SnO2Nano material, is filled in nanometer Space between line, due to WO3Nano wire has bigger specific surface area so that itself and SnO2Nanometer Material area substantially increases, WO3Nano wire makees catalyst and substantially increases SnO2To CO's Sensitivity and selectivity, and then improve the sensitivity of inspection system.
(2) a kind of based on hazardous gas detection the power equipment inspection that embodiments herein is provided Viewing system, owing to its CO gas sensor used uses SnO2Nano material is by sol-gal process Preparation, and SnO2Nano material increases with the contact area of gas, and then improves SnO2Nanometer material The material absorbability to gas, simultaneously because doping TiO2Nanoparticle, it is possible to promote material surface oxygen Ion and the reaction of reducibility gas CO, and then improve the sensor sensitivity to CO.
Aspect and advantage that the application adds will part be given in the following description, and part will be from following Description in become obvious, or recognized by the practice of the application.It should be appreciated that above It is only exemplary and explanatory that general description and details hereinafter describe, and can not limit the application.
Accompanying drawing explanation
Accompanying drawing herein is merged in description and constitutes the part of this specification, it is shown that meet this Inventive embodiment, and for explaining the principle of the present invention together with description.
Fig. 1 be the present invention inspection system in the structural representation of CO gas sensor.Wherein: 01-Si Substrate, 02-silicon oxide film, 03-W film, 04-WO3Nano wire film, 05-SnO2Nano thin-film, 06-Pt electrode, 07-heating module.
Fig. 2 is to prepare CO gas sensor flow chart.
Detailed description of the invention
Here will illustrate exemplary embodiment in detail, its example represents in the accompanying drawings.Below Description when relating to accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represents identical or phase As key element.Embodiment described in following exemplary embodiment does not represent and present invention phase one The all embodiments caused.On the contrary, they only with as appended claims describes in detail, this The example of the consistent apparatus and method of some aspects of invention.
Following disclosure provides many different embodiments or example for realizing the difference of the application Structure.In order to simplify disclosure herein, hereinafter parts and setting to specific examples are described. Certainly, they are the most merely illustrative, and are not intended to limit the application.Additionally, the application is permissible Repeat reference numerals and/or letter in different examples.This repetition is to simplify and clearly mesh , itself it is more than the relation between various embodiment being discussed and/or arranging.Additionally, the application The various specific technique provided and the example of material, but those of ordinary skill in the art can anticipate Know the applicability to other techniques and/or the use of other materials.It addition, described below first is special Levy Second Eigenvalue " on " structure can include what the first and second features were formed as directly contacting Embodiment, it is also possible to include the embodiment that other feature is formed between the first and second features, this Sample the first and second feature is not likely to be directly contact.
In the description of the present application, it should be noted that unless otherwise prescribed and limit, term " peace Dress ", should be interpreted broadly " being connected ", " connection ", for example, it may be mechanical connection or electrically connect, also Can be the connection of two element internals, can be to be joined directly together, it is also possible to indirect by intermediary It is connected, for the ordinary skill in the art, above-mentioned term can be understood as the case may be Concrete meaning.
At present, sensor technology has become as the pith of modern development in science and technology, itself and computer skill Three broad aspect of art, communication technology composition modern information technologies.Report to the police based on gas detecting and identification Gas sensor is an important branch of sensor.In breed of crop, beverage industry, food work The aspects such as industry, atmospheric monitoring, commercial production, sensor plays the most important effect.
CO gas is a kind of gas harmful to human body and environmental toxic.When people suck a small amount of CO After, its easily in blood haemachrome be combined and form stable associated complex, cause hemoglobin to lose defeated Sending the ability of oxygen, eventually cause tissue anoxia, the lighter produces the symptoms such as headache, vomiting, sternly Severe one can cause brain injury or death.
In productive life, the source of CO is a lot.In coke plant, steel mill, chemical plant etc., behaviour Being likely to be exposed in high concentration CO gas as personnel, family's coal heating, the accident of terminal coal gas are let out Dew, scene of fire etc. also can produce a large amount of CO, easily cause the poisoning of people.It addition, CO It is a kind of inflammable and explosive gas simultaneously, can occur when CO content is at 12%~74% in air Blast.
The sensor being currently based on CO gas detecting mainly has MOS type, electrochemistry Type, solid electrolyte type, catalytic combustion type etc., it is steady that MOS type sensor has heat Qualitative good, low cost, components and parts make the advantages such as simple, have become as the class sensing that research is more Device.
Stannum is a kind of common elements, is positioned at IVA race in periodic chart, and it can be combined into multiple oxygen with oxygen Compound, wherein, SnO2It is most stable of.SnO2Belong to a kind of typical wide bandgap semiconductor metal Oxide, due to self crystal structure, surface characteristic and characterization of adsorption etc., SnO2At gas sensing The fields such as device, solaode, electrochemistry are widely used.SnO2As a kind of important air-sensitive Sensor sensing material, has the advantages such as response is sensitive, cost of manufacture is low, technological process is simple, warp It is commonly used for the detection of reducibility gas.
The probe gas principle of MOS type gas sensor be based on sensing element with The interaction of object gas.Metal-oxide semiconductor (MOS) for gas have stronger physically or chemically Absorbability, when it is with air contact, it is quick that the oxygen in air can be adsorbed in metal-oxide semiconductor (MOS) The surface of sense material, and interact with sensitive material, produce negative oxygen ion;When contact reproducibility gas After body, reducibility gas reacts with the negative oxygen ion on this sensitive material surface, causes quasiconductor sensitivity material Material carrier concentration becomes big, thus causes this sensitive material electrical conductivity to become big, and resistance declines, based on quick The change of sense material electrical properties, it is achieved the detection to reducibility gas.
MOS type gas sensor have corrosion-resistant, cost of manufacture is low, Cleaning Principle The advantage such as simple, but, existing metal oxide semiconductor sensor based on CO gas detecting is still There is the problems such as selectivity, less stable, response be the sensitiveest.
Embodiment one:
Embodiments herein relates to a kind of power equipment inspection system based on hazardous gas detection, should Inspection system is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si substrate (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in institute The WO state the W film (03) on silicon oxide film (02), being formed on W film (03)3Nanometer Line thin film (04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), SnO2Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at below described Si substrate Heating module (07);Described WO3Nanowire length is 500~1500nm.
Preferably, the preparation method such as Fig. 2, CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 600nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 7g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 63 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
Preferably, the test system of described CO sensor is by gas dilution system, electrochemical workstation Composition, can realize the detection to minimum 1ppm gas, and the sample sensor made is put into test chamber, Discharging chamber air, two electrodes are connected with external electrical chem workstation, and test voltage is 10V.Pass Sensor response value is defined as: R=R0/Rg, and wherein R0 is material resistance in atmosphere, and Rg is material Resistance in certain concentration object gas, response time and recovery time are respectively response value and recovery Value reaches the time used during the 90% of balance.Found by test, in CO concentration for being respectively 200,500,1000,1500ppm time, this sensor response value corresponds to 16,29,41,72, H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding It is 5,9,26,28, shows preferable CO selectivity;By the reperformance test of 2000 times, Under same concentrations CO, response value drops to original 93%, has good stability.
Test specification, the inspection system installing this CO sensor is highly sensitive, repeated, stability Well, there is the biggest market application foreground.
Embodiment two:
Embodiments herein relates to a kind of power equipment inspection system based on hazardous gas detection, should Inspection system is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si substrate (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in institute The WO state the W film (03) on silicon oxide film (02), being formed on W film (03)3Nanometer Line thin film (04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), SnO2Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at below described Si substrate Heating module (07);Described WO3Nanowire length is 500~1600nm.
Preferably, the preparation method such as Fig. 2, CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 600nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 8g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 12g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 63 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
Preferably, the test system of described CO sensor is by gas dilution system, electrochemical workstation Composition, can realize the detection to minimum 1ppm gas, and the sample sensor made is put into test chamber, Discharging chamber air, two electrodes are connected with external electrical chem workstation, and test voltage is 10V.Pass Sensor response value is defined as: R=R0/Rg, and wherein R0 is material resistance in atmosphere, and Rg is material Resistance in certain concentration object gas, response time and recovery time are respectively response value and recovery Value reaches the time used during the 90% of balance.Found by test, in CO concentration for being respectively 200,500,1000,1500ppm time, this sensor response value corresponds to 14,25,41,72, H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding It is 5,9,16,24, shows preferable CO selectivity;By the reperformance test of 2000 times, Under same concentrations CO, response value drops to original 93%, has good stability.
Test specification, the inspection system installing this CO sensor is highly sensitive, repeated, stability Well, there is the biggest market application foreground.
Embodiment three:
Embodiments herein relates to a kind of power equipment inspection system based on hazardous gas detection, should Inspection system is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si substrate (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in institute The WO state the W film (03) on silicon oxide film (02), being formed on W film (03)3Nanometer Line thin film (04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), SnO2Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at below described Si substrate Heating module (07);Described WO3Nanowire length is 500~1700nm.
Preferably, the preparation method such as Fig. 2, CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 500nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 7g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 63 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.03wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
Preferably, the test system of described CO sensor is by gas dilution system, electrochemical workstation Composition, can realize the detection to minimum 1ppm gas, and the sample sensor made is put into test chamber, Discharging chamber air, two electrodes are connected with external electrical chem workstation, and test voltage is 10V.Pass Sensor response value is defined as: R=R0/Rg, and wherein R0 is material resistance in atmosphere, and Rg is material Resistance in certain concentration object gas, response time and recovery time are respectively response value and recovery Value reaches the time used during the 90% of balance.Found by test, in CO concentration for being respectively 200,500,1000,1500ppm time, this sensor response value corresponds to 19,29,41,72, H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding It is 5,9,16,24, shows preferable CO selectivity;By the reperformance test of 2000 times, Under same concentrations CO, response value drops to original 93%, has good stability.
Test specification, the inspection system installing this CO sensor is highly sensitive, repeated, stability Well, there is the biggest market application foreground.
Embodiment four:
Embodiments herein relates to a kind of power equipment inspection system based on hazardous gas detection, should Inspection system is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si substrate (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in institute The WO state the W film (03) on silicon oxide film (02), being formed on W film (03)3Nanometer Line thin film (04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), SnO2Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at below described Si substrate Heating module (07);Described WO3Nanowire length is 500~1800nm.
Preferably, the preparation method such as Fig. 2, CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 600nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 13g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed Mixture precipitation, is heated to 63 DEG C by mixture precipitation, adds back dissolving in saturated oxalic acid, until heavy Shallow lake is completely dissolved, and obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surface activity Agent joins in vitreosol, and puts into 90 DEG C of baking oven drying 20h, obtains SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
Preferably, the test system of described CO sensor is by gas dilution system, electrochemical workstation Composition, can realize the detection to minimum 1ppm gas, and the sample sensor made is put into test chamber, Discharging chamber air, two electrodes are connected with external electrical chem workstation, and test voltage is 10V.Pass Sensor response value is defined as: R=R0/Rg, and wherein R0 is material resistance in atmosphere, and Rg is material Resistance in certain concentration object gas, response time and recovery time are respectively response value and recovery Value reaches the time used during the 90% of balance.Found by test, in CO concentration for being respectively 200,500,1000,1500ppm time, this sensor response value corresponds to 14,29,41,72, H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding It is 5,9,16,34, shows preferable CO selectivity;By the reperformance test of 2000 times, Under same concentrations CO, response value drops to original 91%, has good stability.
Test specification, the inspection system installing this CO sensor is highly sensitive, repeated, stability Well, there is the biggest market application foreground.
Embodiment five:
Embodiments herein relates to a kind of power equipment inspection system based on hazardous gas detection, should Inspection system is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si substrate (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in institute The WO state the W film (03) on silicon oxide film (02), being formed on W film (03)3Nanometer Line thin film (04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), SnO2Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at below described Si substrate Heating module (07);Described WO3Nanowire length is 500~1900nm.
Preferably, the preparation method such as Fig. 2, CO gas sensor comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 400nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 17g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 60 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.03wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
Preferably, the test system of described CO sensor is by gas dilution system, electrochemical workstation Composition, can realize the detection to minimum 1ppm gas, and the sample sensor made is put into test chamber, Discharging chamber air, two electrodes are connected with external electrical chem workstation, and test voltage is 10V.Pass Sensor response value is defined as: R=R0/Rg, and wherein R0 is material resistance in atmosphere, and Rg is material Resistance in certain concentration object gas, response time and recovery time are respectively response value and recovery Value reaches the time used during the 90% of balance.Found by test, in CO concentration for being respectively 200,500,1000,1500ppm time, this sensor response value corresponds to 14,29,41,72, H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding It is 5,9,16,24, shows preferable CO selectivity;By the reperformance test of 2000 times, Under same concentrations CO, response value drops to original 93%, has good stability.
Test specification, the inspection system installing this CO sensor is highly sensitive, repeated, stability Well, there is the biggest market application foreground.
Those skilled in the art, after considering description and putting into practice invention disclosed herein, will readily occur to Other embodiments of the present invention.The application is intended to any modification of the present invention, purposes or fits Answering property changes, and these modification, purposes or adaptations are followed the general principle of the present invention and wrap Include the undocumented common knowledge in the art of the application or conventional techniques means.Description and reality Executing example and be considered only as exemplary, true scope and spirit of the invention are referred to by claim below Go out.
It should be appreciated that the invention is not limited in essence described above and illustrated in the accompanying drawings Really structure, and various modifications and changes can carried out without departing from the scope.The scope of the present invention is only Limited by appended claim.

Claims (2)

1. a power equipment inspection system based on hazardous gas detection, this inspection system is provided with CO gas sensor;Described CO gas sensor includes Si substrate, is formed in described Si substrate Silicon oxide film, the W film being placed on described silicon oxide film, the WO that is formed on W film3 Nano wire film, it is overlying on WO3SnO on nano wire film2Nano thin-film, at SnO2Nanometer thin On film make two Pt electrodes and be positioned at the heating module below described Si substrate;Described WO3Receive Rice noodle a length of 500~1500nm.
Inspection system the most according to claim 1, wherein, the preparation side of CO gas sensor Method comprises the steps:
Step one, preparation Si substrate:
Take the silicon chip of certain size (5cm × 5cm), sequentially pass through acetone, ethanol, deionized water Ultrasonic cleaning, ultrasonic time is 30min, is then putting in oxidation furnace by silicon chip, at 1100 DEG C Thermal oxide, obtains the silicon oxide film of a layer thickness about 600nm at silicon chip surface;
Step 2, prepares WO3Nano wire film:
Silicon chip through step one thermal oxide is put in magnetic control sputtering device, is evacuated to 2.0 × 10-3Hereinafter, Then utilize magnetron sputtering technique, plate one layer of W film at silicon oxide surface, using as WO3Nano wire Growth source, magnetron sputtering power be the thickness of 300W, W film be 300nm, size is 3cm × 3 cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 20sccm, the most steady Determining 1h, discharge the air in tube furnace, following heated Tube-furnace is with the ramp of 10 DEG C/min To 380 DEG C, and it is incubated 6h, is incubated complete its natural cooling that allows, after dropping to room temperature, take out silicon chip, One layer of WO is obtained on the W film surface of silicon chip3Nano wire film;
Step 3, prepares SnO2Nano thin-film:
First, prepare 100ml deionized water, weigh 5g SnCl4·5H2O is dissolved in deionized water, with Rear interpolation 0.3g citric acid, heated solution to 53 DEG C, under magnetic stirring, add 0.5mol/L's Ammonia to pH value is 3, prepares Sn (OH)4Precipitate, precipitation stands 15h, through repeatedly washing Remove removing chloride;Then 7g TiO is weighed2Nanoparticle, with precipitation mixed grinding 0.5h, is formed mixed Compound precipitates, and mixture precipitation is heated to 63 DEG C, adds back dissolving in saturated oxalic acid, until precipitation It is completely dissolved, obtains transparent SnO2Colloidal sol, using saturated for 10ml Polyethylene Glycol as surfactant Join in vitreosol, and put into 90 DEG C of baking oven drying 20h, obtain SnO2Gel Precursor, By this SnO2Gel Precursor is roasting 1.5h at 580 DEG C, obtains the TiO that adulterates2Nanoparticle SnO2Nanometer powder;
Use terpineol and SnO2Nanometer powder mixes, and preparation becomes SnO2Slurry, and use silk screen The method of printing is by SnO2Slurry is coated in the WO of silicon chip3Nano wire film region, SnO2Slurry is thick Degree is 2 μm, silicon chip is dried at 100 DEG C 5min subsequently, at WO3Nano wire film region Fill one layer of SnO2Nano thin-film;
Step 4, preparation pt electrode:
This sensor electrode uses Pt electrode, utilizes magnetron sputtering to combine template at SnO2Slurry table Face makes two Pt electrodes;Described Pt electrode is added with Bi2O3Material and MgB2Material, described Bi2O3The addition of material is 0.01wt%~0.1wt%, described MgB2The addition of material is 0.005wt%~0.05wt%.
Step 5, assembling CO gas sensor:
Wire and two Pt electrodes are connected, at Si backside of substrate, heating module and sensor is installed Shell mechanism.
CN201610429219.2A 2016-06-15 2016-06-15 Electrical equipment inspection system based on hazardous gas detection Pending CN106018493A (en)

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