CN105911112A - Iron-smelting blast furnace with CO gas detection function - Google Patents
Iron-smelting blast furnace with CO gas detection function Download PDFInfo
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- CN105911112A CN105911112A CN201610427985.5A CN201610427985A CN105911112A CN 105911112 A CN105911112 A CN 105911112A CN 201610427985 A CN201610427985 A CN 201610427985A CN 105911112 A CN105911112 A CN 105911112A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to an iron-smelting blast furnace with a CO gas detection function. The iron-smelting blast furnace is provided with a CO gas sensor, wherein the CO gas sensor comprises a Si substrate, an silicon oxide film formed on the Si substrate, a W film arranged on the silicon oxide film, a WO3 nanowire film formed on the W film, a SnO2 nano-film covering the WO3 nanowire film, two Pt electrodes manufactured on the SnO2 nano-film, and a heating module located on the Si substrate. The iron-smelting blast furnace is high in sensitivity to CO gas, short in response time, and high in repeatability and stability.
Description
Technical field
The application relates to blast furnace field, particularly relates to a kind of refining based on CO gas detection function
Iron blast furnace.
Background technology
Blast furnace ironmaking is the important step in steel manufacture process, owing to its technique is simple, energy consumption is low,
It it is a kind of main method producing ferrum.Iron ore, coke, limestone is loaded from furnace roof during blast fumance
Deng, it is blown into preheated air from being positioned at the lower furnace air port along stove week.
Owing to can produce CO (carbon monoxide converter) gas during blast furnace ironmaking, and CO (carbon monoxide converter) gas belongs to dangerous
Property gas, a large amount of accumulations personal security can be caused a hidden trouble, but, existing blast furnace does not the most possess one
The detection function of carbon oxide gas.
Summary of the invention
For overcoming problem present in correlation technique, the application provides a kind of based on CO gas detecting merit
The blast furnace of energy.
The present invention is achieved through the following technical solutions: a kind of ironmaking based on CO gas detection function is high
Stove, this blast furnace is provided with CO gas sensor;Described CO gas sensor include Si substrate,
The W film that be formed at the suprabasil silicon oxide film of described Si, is placed on described silicon oxide film, shape
Become the WO on W film3Nano wire film, it is overlying on WO3SnO on nano wire film2Nanometer thin
Film, at SnO2On nano thin-film make two Pt electrodes and be positioned at the heating below described Si substrate
Module;Described WO3Nanowire length is 500~4000nm.
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 CO gas detection function the ironmaking that embodiments herein is provided is high
Stove, it is provided with CO gas sensor, and this CO gas sensor is based on SnO2Nano material
Resistor-type CO sensor, pass through WO3Nano wire and SnO2The combination of nano material, enhances
The aspect effects such as selectivity that CO is detected by CO gas sensor, stability;CO gas sensor
At WO3On the basis of nano wire film, coat one layer of SnO2Nano material, is filled between nano wire
Space, due to WO3Nano wire has bigger specific surface area so that itself and SnO2Nano material connects
Contacting surface is long-pending to be substantially increased, WO3Nano wire makees catalyst and substantially increases SnO2Sensitivity to CO
With selectivity, and then improve the sensitivity of blast furnace.
(2) a kind of based on CO gas detection function the ironmaking that embodiments herein is provided is high
Stove, owing to its CO gas sensor used uses SnO2Nano material is prepared by sol-gal process,
And SnO2Nano material increases with the contact area of gas, and then improves SnO2Nano material is to gas
The absorbability of body, simultaneously because doping TiO2Nanoparticle, it is possible to promote material surface oxonium ion with
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 is the structural representation of the CO gas sensor of the present invention.Wherein: 01-Si substrate, 02-
Silicon oxide film, 03-W film, 04-WO3Nano wire film, 05-SnO2Nano thin-film, 06-Pt electricity
Pole, 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 blast furnace based on CO gas detection function, this ironmaking
Blast furnace is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si base
The end (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in described oxidation
W film (03) on silicon thin film (02), the WO being formed on W film (03)3Nano wire film
(04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), at SnO2
Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at adding below described Si substrate
Thermal modules (07);Described WO3Nanowire length is 500~4000nm.
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 5,9,15,24, 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 blast furnace 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 blast furnace based on CO gas detection function, this ironmaking
Blast furnace is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si base
The end (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in described oxidation
W film (03) on silicon thin film (02), the WO being formed on W film (03)3Nano wire film
(04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), at SnO2
Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at adding below described Si substrate
Thermal modules (07);Described WO3Nanowire length is 500~4500nm.
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 0.04wt%~0.1wt%, described MgB2The addition of material is 0.01
Wt%~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 12,29,41,72,
H2 concentration be respectively 200,500,1000,1500ppm time, this sensor response value is corresponding
It is 5,9,19,24, shows preferable CO selectivity;By the reperformance test of 2000 times,
Under same concentrations CO, response value drops to original 92%, has good stability.
Test specification, the blast furnace 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 blast furnace based on CO gas detection function, this ironmaking
Blast furnace is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si base
The end (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in described oxidation
W film (03) on silicon thin film (02), the WO being formed on W film (03)3Nano wire film
(04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), at SnO2
Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at adding below described Si substrate
Thermal modules (07);Described WO3Nanowire length is 500~5000nm.
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 700nm 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 5 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 5,9,16,27, 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 blast furnace 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 blast furnace based on CO gas detection function, this ironmaking
Blast furnace is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si base
The end (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in described oxidation
W film (03) on silicon thin film (02), the WO being formed on W film (03)3Nano wire film
(04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), at SnO2
Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at adding below described Si substrate
Thermal modules (07);Described WO3Nanowire length is 500~5500nm.
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 200nm, size is 3cm × 3
cm;
Then silicon chip is put in tube furnace, at ambient pressure, be passed through the Ar gas of 40sccm, 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 5 μm, silicon chip is dried at 90 DEG C 5min subsequently, at WO3Nano wire film region is filled out
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 5,9,14,24, shows preferable CO selectivity;By the reperformance test of 2000 times,
Under same concentrations CO, response value drops to original 94%, has good stability.
Test specification, the blast furnace 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 blast furnace based on CO gas detection function, this ironmaking
Blast furnace is provided with CO gas sensor;As it is shown in figure 1, described CO gas sensor includes Si base
The end (01), the silicon oxide film (02) being formed on described Si substrate (01), it is placed in described oxidation
W film (03) on silicon thin film (02), the WO being formed on W film (03)3Nano wire film
(04), it is overlying on WO3SnO on nano wire film (04)2Nano thin-film (05), at SnO2
Nano thin-film (05) is gone up two the Pt electrodes (06) made and is positioned at adding below described Si substrate
Thermal modules (07);Described WO3Nanowire length is 500~6000nm.
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 50sccm, 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%~0.01wt%.
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 93%, has good stability.
Test specification, the blast furnace 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 blast furnace based on CO gas detection function, this blast furnace is provided with CO gas
Body sensor;Described CO gas sensor includes Si substrate, is formed at the suprabasil oxygen of described Si
SiClx thin film, the W film being placed on described silicon oxide film, the WO that is formed on W film3Nano wire
Thin film, it is overlying on WO3SnO on nano wire film2Nano thin-film, at SnO2Make on nano thin-film
Make two Pt electrodes and be positioned at the heating module below described Si substrate;Described WO3Nanometer line length
Degree is 500~4000nm.
Blast furnace 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.
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Cited By (1)
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