CN109911929A - A kind of Pt is catalyst preparation SnO2The methods and applications of nano material - Google Patents
A kind of Pt is catalyst preparation SnO2The methods and applications of nano material Download PDFInfo
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Abstract
A kind of Pt is catalyst preparation SnO2The methods and applications of nano material belong to the gas sensor domain of metal oxide semiconductor material.A kind of Pt is the SnO of catalyst preparation2Nano material, the SnO2Nano material is in pectinate texture, and around trunk surface, dense growth has nano wire；The nano material is by the SnO of rutile tetragonal phase crystal structure2It constitutes；Trunk diameter is 100~500nm, and length is 100~500 μm, and the diameter of nano wire is 80~200nm, and length is 400nm~2 μm.H of the present invention2S gas sensor obtains under lower operating temperature to H2The maximum sensitivity of S gas has quickly response and resume speed, Monitoring lower-cut 500ppb, to H2S has excellent selectivity.The invention overcomes existing H2The deficiencies of S gas sensor operating temperature is excessively high, response resume speed is slow, poor selectivity, there is good application prospect.
Description
Technical field
The invention belongs to the gas sensor technical fields of metal oxide semiconductor material, and in particular to a kind of to be with Pt
Catalyst preparation SnO2The methods and applications of nano material.
Background technique
The exploitation and utilization of mineral resources are in China's economic development always in occupation of not replaceable status.However, I
The safety production situation of state's mining industry is but always and pessimistic, and various regions mine safety event happens occasionally, and especially China part contains
Sulphur mine all occurred because of hypertoxic hydrogen sulfide gas (H2S) gush out and caused by accident.Therefore, for H2Effective monitoring of S gas
Become the bottleneck problem of China mine urgent need to resolve with timely early warning.
Gas sensor is a kind of gas componant that will test and concentration is converted to signal that people are easier to identify (such as electricity
Signal, acoustical signal, optical signal, digital signal etc.) component or device.Currently used for monitor hydrogen sulfide gas sensor be mostly
Electrochemistry or semiconductor-type sensors, but the problems such as electrochemical sensor is high, the service life is short in the prevalence of price.Semiconductor-type
Sensor is easy to minimize, integrated feature with high sensitivity, service life length, low-power consumption, low cost, is expected to become mine
It is used to detect H in safety in production2The efficient sensor of S.Metal oxide semiconductor material SnO2It is the most widely used at present
Gas sensitive, and to H2S also has good response.Preparation SnO at present2Method include that hydro-thermal method, sol-gal process, chemistry are heavy
Shallow lake method etc., wherein the low-dimensional SnO based on thermal evaporation preparation2Nano material has huge specific surface area and excellent major diameter
Than；Low-dimension nano material is easily formed latticed sensitive layer simultaneously, and loose and porous structure abundant is highly advantageous to H2S gas is fast
Speed is penetrated into entire sensitive layer, to significantly improve its response/recovery time, and is overlapped and is formed between a large amount of low-dimension nano materials
Nano-node also contribute to promoting sensitivity of the material to object gas.However, there is also yield for thermal evaporation at present
The disadvantages of low, technological parameter is difficult to control.Because generally needing to control furnace internal pressure during preparing low-dimension nano material
By force, the position of growth substrates and type etc.；In addition, some need is mixed into micro oxygen into argon gas in thermal evaporation, have
Be then using the oxygen of residual volume in argon gas in furnace, therefore the repeatability of obtained product pattern is universal poor.According to Americanized
Learn research disclosed in institute periodical (Journal of Physical Chemistry C, 2018,122,24407-24414)
Show the thermal evaporation preparation SnO based on " gas-liquid-solid " growth mechanism2During nano material, excessive or very few oxygen
Supply can all inhibit its growth.Therefore, the control of flow of oxygen is one of the key influence factor in thermal evaporation, while oxygen
Dosage also will affect the structure and application of final product.Therefore, it is necessary to can be under atmospheric pressure environment, using having using one kind
The straightforward procedure of oxygen flow in the porous ceramics substrate of more surface binding sites and easily controllable thermal evaporation process, thus
Efficiently prepare low-dimensional SnO2Nano material, and it is used for H2In S gas sensor.
Summary of the invention
The present invention is intended to provide one kind prepares SnO using thermal evaporation using Pt metal as catalyst2The side of nano material
Method, to realize that Pt metal had both promoted SnO as catalyst2The formation of nanometer material structure, but can be used as dopant raising should
Material is to H2The gas-sensitive property of S gas.For this method under atmospheric pressure environment, oxygen flow is easily controllable, easy to operate, repeatability
It is high.
A kind of Pt is the SnO of catalyst preparation2Nano material, the SnO2Nano material is in pectinate texture, surrounds trunk table
Face dense growth has nano wire；The nano material is by the SnO of rutile tetragonal phase crystal structure2It constitutes；The trunk is straight
Diameter is 100~500nm, and length is 100~500 μm, and the diameter of the nano wire is 80~200nm, and length is 400nm~2 μm.
Pectinate texture of the present invention is that multiple nano wires are distributed on a trunk and form the knot as comb form
Structure.
It is a further object of the present invention to provide one kind using Pt as catalyst preparation SnO2The method of nano material, the method
It is as follows:
1. sputtering one layer of Pt film in porous ceramics substrate surface, sputtering current is 4~12mA, is splashed by d.c. sputtering instrument
Penetrating the time is 45~60s；
2. the Sn particle that 0.2~0.5g purity is 99.99% is put into the middle part of aluminium oxide porcelain boat, and by above-mentioned porous ceramics
Substrate is coated with the side of Pt film towards Sn particle and to place with air inlet direction in 30~60 ° of angles, and porcelain boat is sent into tubular type
The central heating zone of furnace quartz ampoule, and install flange and be sealed；
After 3. the argon gas 20min that purity is 99.99% is passed through into tube furnace with the flow velocity of 200~300ml/min, adjustment
Argon gas flow velocity opens heating device to 50~100ml/min, 900 are warming up to the heating rate of 5~10 DEG C/min~
1000 DEG C, and keep the temperature 60~90min；Wherein, when tubular type furnace temperature rises to 200~300 DEG C, start to be passed through into tube furnace pure
The oxygen that degree is 99.99%；The flow of the oxygen is by noticeable degree with a scale, and the aperture of needle-valve is 2~5 circles；
4. closing argon gas and oxygen after tube furnace cooled to room temperature, aluminium oxide porcelain boat is taken out, white flock is produced
Object is scraped from porous ceramics substrate surface, and white fluffy solid is using Pt as the SnO of catalyst preparation2Nano material.
Preferably, the material of the porous ceramics substrate is diatomite or kaolin containing aluminosilicate ingredient, is used
Pore creating material hole forming method carries out porous processing, and pore creating material is ball-type graphite or PMMA microsphere, and the average diameter of the pore creating material is
10~70 μm, adding proportion is 20~50wt.%, is formed using moulding sintering process, and firing temperature is 1000~1200 DEG C.
Preferably, a length of 15~20mm of porous ceramics substrate, width are 5~10mm, and thickness is 1~2mm.
It is a further object of the present invention to provide a kind of with following SnO2Nano material is the H of sensitive layer2S gas sensor,
The sensor is with following SnO2Nano material is gas sensitive, and the gas sensitive is coated uniformly on electrode element surface,
Electrode member is plane electrode.
A kind of Pt is the SnO of catalyst preparation2Nano material, the SnO2Nano material is in pectinate texture, surrounds trunk table
Face dense growth has nano wire；The nano material is by the SnO of rutile tetragonal phase crystal structure2It constitutes；The trunk is straight
Diameter is 100~500nm, and length is 100~500 μm, and the diameter of the nano wire is 80~200nm, and length is 400nm~2 μm.
It is yet another object of the invention to provide a kind of following H2The preparation method of S gas sensor, the method are as follows:
1. by following SnO2Nano material is poured into the 2ml conical centrifuge tube equipped with 0.5ml dehydrated alcohol, is shaken in ultrasound
It swings in device and is uniformly dispersed, until solution presentation white is suspended, obtain suspension；
2. suspension is dripped on electrode element surface dropwise, with hot blast drying, and repeatedly operation until sensitive layer
Thickness is about 2mm；
3. electrode member is welded in the detection pedestal of air-sensitive test macro, it is subsequently placed on agingtable with 2 DEG C/min
It is heated to 200~300 DEG C and keeps the temperature 24~36h, obtain with SnO2Nano material is the H of sensitive layer2S gas sensor.
It is a kind of with following SnO2Nano material is the H of sensitive layer2S gas sensor, the sensor is with following SnO2
Nano material is gas sensitive, and the gas sensitive is coated uniformly on electrode element surface, and electrode member is plane electrode.
A kind of Pt is the SnO of catalyst preparation2Nano material, the SnO2Nano material is in pectinate texture, surrounds trunk table
Face dense growth has nano wire；The nano material is by the SnO of rutile tetragonal phase crystal structure2It constitutes；The trunk is straight
Diameter is 100~500nm, and length is 100~500 μm, and the diameter of the nano wire is 80~200nm, and length is 400nm~2 μm.
Hot blast drying is without actual temp requirement, drying in the present invention.
The invention has the benefit that
1, the present invention can carry out under normal pressure, easy to operate, and the flow of oxygen micro using noticeable degree, and test can
It is repeated high.
2, using porous ceramics substrate, it is placed with air inlet direction in 30~60 ° of angles, to be conducive to improve product
Yield.
3, SnO is promoted based on Pt metal catalyst2The formation of nanometer material structure improves its specific surface area and nano junction
Quantity, and the codope of Pt and Si can make the material under lower operating temperature to H2S gas has highly sensitive, quick
Response and recovery, selectivity are good.H of the invention2The excellent low temperature H of S gas sensor2S gas-sensitive property makes it be expected to become mine
Efficient H in industry production field2S gas sensor.
Detailed description of the invention
Fig. 1 (a) and Fig. 1 (b) is the obverse and reverse of the structural schematic diagram of 1~3 planar-type electrode of the embodiment of the present invention,
Wherein, 1: aluminum oxide substrate；2: gold electrode；3: platinum guide wire；4: ruthenium-oxide heating layer；5: gas sensitive layer；
Fig. 2 is the structural schematic diagram of thermal evaporation apparatus in the embodiment of the present invention 1~3；A: porous ceramics substrate；B: high purity tin
Grain；C: aluminium oxide porcelain boat；D: quartz ampoule；E: sealing flange；F: air inlet；G: gas outlet；
Fig. 3 is the X ray diffracting spectrum of prepared product in the embodiment of the present invention 1；
Fig. 4 (4-1) is the low range electron scanning micrograph of prepared product in the embodiment of the present invention 1, and (4-2) is
The electron scanning micrograph of high magnification side view angle.
Fig. 5 (5-1) is the x-ray photoelectron spectroscopy full scan figure of prepared product in the embodiment of the present invention 1；(5-2) is
To the high-resolution x-ray photoelectron spectroscopy figure of Pt element；(5-3) is the high-resolution x-ray photoelectron spectroscopy figure to Si element.
Fig. 6 (6-1) is sensor prepared in the embodiment of the present invention 1 to 3ppm H2The sensitivity of S and operating temperature it
Between relational graph；(6-2) sensor is to 3ppm H2The relational graph of the response of S/between recovery time and operating temperature；(6-3) is passed
Sensor is at 85 DEG C of operating temperature to various concentration H2The dynamic response curve figure of S；(6-4) sensor is at 85 DEG C of operating temperature
Sensitivity and H2Relational graph between S concentration；
Fig. 7 be sensor prepared in the embodiment of the present invention 1 at 85 DEG C of operating temperature to different detected gas
Sensitivity.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
H based on plane electrode2Sensor element, structural schematic diagram is as shown in Figure 1, by aluminum oxide substrate, gold electricity
Pole, platinum lead, ruthenium-oxide heating layer and air-sensitive material layer composition.The front and back of substrate fixes two width respectively and is
The gold electrode of 0.3mm, the distance between electrode are 0.15mm；Substrate back is by RuO2The heating layer of layer composition, and pass through platinum
Spun gold lead welds the gold electrode of substrate tow sides on the base.Gas sensitive is equably added dropwise in substrate front side and stacks
Form nanowire mesh trellis sensitive layer.
It is a kind of using Pt as the SnO of catalyst preparation2The method of nano material:
By d.c. sputtering instrument, one layer of Pt film, sputtering current 8mA, sputtering time are sputtered in porous ceramics substrate surface
For 60s；
The Sn particle that 0.2g purity is 99.99% is put into the middle part of aluminium oxide porcelain boat, and above-mentioned porous ceramics substrate is plated
There is the side of Pt film towards Sn particle and, in the placement of 45° angle degree, porcelain boat is sent into tube furnace quartz ampoule with air inlet direction
Central heating zone, and install flange and be sealed, schematic diagram is as shown in Figure 2.
After being passed through the argon gas 20min that purity is 99.99% into tube furnace with the flow velocity of 200ml/min, argon gas stream is adjusted
Speed opens heating device to 50ml/min, is warming up to 900 DEG C with the heating rate of 10 DEG C/min, and keep the temperature 60min；Its
In, when tubular type furnace temperature rises to 200 DEG C, start to be passed through the oxygen that purity is 99.99% into tube furnace；The stream of the oxygen
Amount is by noticeable degree with a scale, and the aperture of needle-valve is 2 circles.
After tube furnace cooled to room temperature, argon gas and oxygen are closed, aluminium oxide porcelain boat is taken out, by white fluffy solid
It is lightly scraped from porous ceramics substrate surface, then to obtained SnO2Nano material carries out Analysis of Structural Characteristics；
The material of porous ceramics substrate described in above-mentioned steps is kaolin, and porous processing method is using pore-creating
Agent hole forming method, pore creating material are PMMA microsphere, and average diameter is 30 μm, adding proportion 30wt.%；Its molding mode is using mould
Sintering process is pressed, firing temperature is 1200 DEG C, porous ceramics substrate a length of 20mm, width 10mm, thickness 2mm.
A kind of SnO2The H of nano material2S gas sensor, sensor SnO in the above way obtained2Nano material
For gas sensitive, the gas sensitive is dropped evenly in electrode element surface.
A kind of above-mentioned SnO2The H of nano material2S gas sensor preparation method, the method are as follows:
By SnO made from the above method2Nano material is dispersed in the 2ml conical centrifuge tube equipped with 0.5ml dehydrated alcohol,
It is then uniformly dispersed in ultrasonator, until solution presentation white is suspended, obtains suspension；
Suspension is extracted with pipettor, is dripped on electrode element surface dropwise, then uses hot blast drying, and grasp repeatedly
Make until sensitive layer thickness is about 2mm.
Electrode member is welded in the detection pedestal of air-sensitive test macro, is subsequently placed on agingtable and is added with 2 DEG C/min
Heat is to 300 DEG C and keeps the temperature 36h, finally obtains SnO2The H of nano material2S gas sensor.
Using thermal evaporation, " gas-liquid-solid " growth mechanism is based in the XRD diagram of porous ceramics substrate surface obtained product
Spectrum is as shown in Figure 3.It can be seen from the figure that other than the cristobalite phase and mullite phase from porous ceramics substrate, institute
Some diffraction maximums can correspond to the SnO of rutile tetragonal phase crystal structure2(JCPDS NO.41-1445).Fig. 4-1 for institute
Obtain the low range stereoscan photograph of product, it can be seen that apparent pectinate texture is presented in product.Fig. 4-2 is the high magnification of product
Stereoscan photograph, obtained SnO2Nano material trunk diameter is 100~500nm, and length is 100~500 μm, surrounds trunk table
Face dense arrangement the nano wire that diameter is 80~200nm, length is 400nm~2 μm.Fig. 5 is the X-ray photoelectricity of obtained product
Sub- energy spectrum diagram, there it can be seen that there are also a small amount of Pt distributions and Si to be distributed other than the characteristic peak of Sn, O, C, in product,
Si's is not intended to adulterate in its residual and porous ceramics substrate respectively from Pt in the catalyst layer in thermal evaporation process.Fig. 6-
1 is based on SnO2The gas sensor of nano material is under different working temperature conditions to 3ppm H2The sensitivity of S.It can from figure
To find out, which obtains peak response value 65 at 85 DEG C of operating temperature.Fig. 6-2 is gas sensor in different operating
To 3ppm H under the conditions of temperature2Response/recovery time of S, it can be seen that response/recovery time is bright with the raising of operating temperature
It is aobvious to reduce, and response/recovery time at 85 DEG C of optimum working temperature is respectively 3s and 396s, show that the sensor can be
Excellent gas-sensitive property is shown under low operating temperature.Fig. 6-3 be gas sensor at 85 DEG C of operating temperature to various concentration
H2The dynamic response curve of S, corresponding sensitivity and H2Relationship between S concentration is as shown in Fig. 6-4.It can from figure
Out, the sensor is in discharge H2After S, resistance can be completely recovered at its initial baseline, and it is good to illustrate that the sensor has
Respond recovery characteristics.Under cryogenic, current major part H2At the beginning of the resistance of S gas sensor cannot generally be completely recovered to it
Primordium line can only be restored by additional pulse voltage, this can dramatically increase the cost of manufacture of sensor.Fig. 7 is gas
Sensitivity of the sensor at 85 DEG C of operating temperature to variety classes gas.The sensor is to 3ppm H as we can see from the figure2S
Sensitivity it is maximum, be significantly higher than 30ppm SO2And the sensitivity of the other interference gas of 1000ppm, show it to H2S has excellent
Different selectivity.
Embodiment 2
H based on plane electrode2Sensor element, structural schematic diagram is as shown in Figure 1, by aluminum oxide substrate, gold electricity
Pole, platinum lead, ruthenium-oxide heating layer and air-sensitive material layer composition.The front and back of substrate fixes two width respectively and is
The gold electrode of 0.3mm, the distance between electrode are 0.15mm；Substrate back is by RuO2The heating layer of layer composition, and pass through platinum
Spun gold lead welds the gold electrode of substrate tow sides on the base.Gas sensitive is equably added dropwise in substrate front side and stacks
Form nanowire mesh trellis sensitive layer.
It is a kind of using Pt as the SnO of catalyst preparation2The method of nano material:
By d.c. sputtering instrument, one layer of Pt film, sputtering current 8mA, sputtering time are sputtered in porous ceramics substrate surface
For 60s；
The Sn particle that 0.2g purity is 99.99% is put into the middle part of aluminium oxide porcelain boat, and above-mentioned porous ceramics substrate is plated
There is the side of Pt film towards Sn particle and, in the placement of 45° angle degree, porcelain boat is sent into tube furnace quartz ampoule with air inlet direction
Central heating zone, and install flange and be sealed, schematic diagram is as shown in Figure 2.
After being passed through the argon gas 20min that purity is 99.99% into tube furnace with the flow velocity of 200ml/min, argon gas stream is adjusted
Speed opens heating device to 50ml/min, is warming up to 900 DEG C with the heating rate of 10 DEG C/min, and keep the temperature 60min；Its
In, when tubular type furnace temperature rises to 200 DEG C, start to be passed through the oxygen that purity is 99.99% into tube furnace；The stream of the oxygen
Amount is by noticeable degree with a scale, and the aperture of needle-valve is 2 circles.
After tube furnace cooled to room temperature, argon gas and oxygen are closed, aluminium oxide porcelain boat is taken out, by white fluffy solid
It is lightly scraped from porous ceramics substrate surface, then to obtained SnO2Nano material carries out Analysis of Structural Characteristics；
The material of porous ceramics substrate described in above-mentioned steps is diatomite, and porous processing method is using pore-creating
Agent hole forming method, pore creating material are ball-type graphite, and average diameter is 24 μm, adding proportion 40wt.%；Its molding mode is using mould
Sintering process is pressed, firing temperature is 1000 DEG C, porous ceramics substrate a length of 20mm, width 10mm, thickness 2mm.
One kind being based on above-mentioned SnO2The H of nano material preparation2S gas sensor, the sensor is with above-mentioned SnO2Nanometer material
Material is gas sensitive, and the gas sensitive is dropped evenly in electrode element surface.
One kind being based on above-mentioned SnO2The H of nano material2The preparation method of S gas sensor, the method are as follows:
By above-mentioned SnO2Nano material is dispersed in the 2ml conical centrifuge tube equipped with 0.5ml dehydrated alcohol, then in ultrasound
It is uniformly dispersed in oscillator, until solution presentation white is suspended, obtains suspension；
Suspension is extracted with pipettor, is dripped on electrode element surface dropwise, then uses hot blast drying, and grasp repeatedly
Make until sensitive layer thickness is about 2mm.
Electrode member is welded in the detection pedestal of air-sensitive test macro, is subsequently placed on agingtable, added with 2 DEG C/min
Heat is to 300 DEG C and keeps the temperature 36h, finally obtains SnO2The H of nano material2S gas sensor.
It is manufactured in the present embodiment to be based on SnO through detecting2The gas sensor of nano material operating temperature be 85 DEG C when pair
0.5~10ppm H2S has good gas-sensitive property.
Embodiment 3
H based on plane electrode2Sensor element, structural schematic diagram is as shown in Figure 1, by aluminum oxide substrate, gold electricity
Pole, platinum lead, ruthenium-oxide heating layer and air-sensitive material layer composition.The front and back of substrate fixes two width respectively and is
The gold electrode of 0.3mm, the distance between electrode are 0.15mm；Substrate back is by RuO2The heating layer of layer composition, and pass through platinum
Spun gold lead welds the gold electrode of substrate tow sides on the base.Gas sensitive is equably added dropwise in substrate front side and stacks
Form nanowire mesh trellis sensitive layer.
It is a kind of using Pt as the SnO of catalyst preparation2The method of nano material:
By d.c. sputtering instrument, one layer of Pt film, sputtering current 12mA, sputtering time are sputtered in porous ceramics substrate surface
For 60s；
The Sn particle that 0.2g purity is 99.99% is put into the middle part of aluminium oxide porcelain boat, and above-mentioned porous ceramics substrate is plated
There is the side of Pt film towards Sn particle and, in the placement of 45° angle degree, porcelain boat is sent into tube furnace quartz ampoule with air inlet direction
Central heating zone, and install flange and be sealed, schematic diagram is as shown in Figure 2.
After being passed through the argon gas 20min that purity is 99.99% into tube furnace with the flow velocity of 200ml/min, argon gas stream is adjusted
Speed opens heating device to 50ml/min, is warming up to 900 DEG C with the heating rate of 10 DEG C/min, and keep the temperature 60min；Its
In, when tubular type furnace temperature rises to 200 DEG C, start to be passed through the oxygen that purity is 99.99% into tube furnace；The stream of the oxygen
Amount is by noticeable degree with a scale, and the aperture of needle-valve is 2 circles.
After tube furnace cooled to room temperature, argon gas and oxygen are closed, aluminium oxide porcelain boat is taken out, by white fluffy solid
It is lightly scraped from porous ceramics substrate surface, then to obtained SnO2Nano material carries out Analysis of Structural Characteristics；
The material of porous ceramics substrate described in above-mentioned steps is kaolin, and porous processing method is using pore-creating
Agent hole forming method, pore creating material are PMMA microsphere, and average diameter is 30 μm, adding proportion 30wt.%；Its molding mode is using mould
Sintering process is pressed, firing temperature is 1200 DEG C, porous ceramics substrate a length of 20mm, width 10mm, thickness 2mm.
One is be based on above-mentioned SnO2The H of nano material preparation2S gas sensor, the sensor is with above-mentioned SnO2Nanometer
Material is gas sensitive, and the gas sensitive is dropped evenly in electrode element surface.
One kind being based on above-mentioned SnO2The H of nano material2The preparation method of S gas sensor, the method are as follows:
By SnO obtained above2Nano material is dispersed in the 2ml conical centrifuge tube equipped with 0.5ml dehydrated alcohol, then
It is uniformly dispersed in ultrasonator, until solution is presented, white is suspended to obtain suspension；
Suspension is extracted with pipettor, is dripped on electrode element surface dropwise, then uses hot blast drying, and grasp repeatedly
Make until sensitive layer thickness is about 2mm.
Electrode member is welded in the detection pedestal of air-sensitive test macro, is subsequently placed on agingtable, added with 2 DEG C/min
Heat is to 300 DEG C and keeps the temperature 36h, finally obtains SnO2The H of nano material2S gas sensor.
It is manufactured in the present embodiment to be based on SnO through detecting2The gas sensor of nano material operating temperature be 85 DEG C when pair
0.5~10ppm H2S has good gas-sensitive property.
Claims (6)
1. the SnO that a kind of Pt is catalyst preparation2Nano material, which is characterized in that the SnO2Nano material is in pectinate texture,
Around trunk surface, dense growth has nano wire；The nano material is by the SnO of rutile tetragonal phase crystal structure2It constitutes；
The trunk diameter is 100~500nm, and length is 100~500 μm, and the diameter of the nano wire is 80~200nm, and length is
400nm~2 μm.
2. one kind is using Pt as catalyst preparation SnO2The method of nano material, which is characterized in that the method is as follows:
1. sputtering one layer of Pt film in porous ceramics substrate surface by d.c. sputtering instrument, sputtering current is 4~12mA, when sputtering
Between be 45~60s；
2. the Sn particle that 0.2~0.5g purity is 99.99% is put into the middle part of aluminium oxide porcelain boat, and by above-mentioned porous ceramics substrate
The side of Pt film is coated with towards Sn particle and to place with air inlet direction in 30~60 ° of angles, porcelain boat is sent into tubular type hearthstone
The central heating zone of English pipe, and install flange and be sealed；
3. after being passed through the argon gas 20min that purity is 99.99% into tube furnace with the flow velocity of 200~300ml/min, adjusting argon gas
Flow velocity opens heating device to 50~100ml/min, is warming up to 900~1000 with the heating rate of 5~10 DEG C/min
DEG C, and keep the temperature 60~90min；Wherein, when tubular type furnace temperature rises to 200~300 DEG C, start to be passed through purity into tube furnace be
99.99% oxygen；The flow of the oxygen is by noticeable degree with a scale, and the aperture of needle-valve is 2~5 circles；
4. closing argon gas and oxygen after tube furnace cooled to room temperature, take out aluminium oxide porcelain boat, by white fluffy solid from
Porous ceramics substrate surface scrapes, and white fluffy solid is using Pt as the SnO of catalyst preparation2Nano material.
3. according to the method described in claim 2, it is characterized in that, the material of the porous ceramics substrate is to contain aluminosilicate
The diatomite or kaolin of ingredient carry out porous processing using pore creating material hole forming method, and pore creating material is that ball-type graphite or PMMA are micro-
Ball, the average diameter of the pore creating material are 10~70 μm, and adding proportion is 20~50wt.%, is formed using moulding sintering process, are burnt
It is 1000~1200 DEG C at temperature.
4. according to the method described in claim 2, it is characterized in that, a length of 15~20mm of porous ceramics substrate, width 5
~10mm, thickness are 1~2mm.
5. one kind is with SnO described in claim 12Nano material is the H of sensitive layer2S gas sensor, which is characterized in that described
Sensor is with SnO described in claim 12Nano material is gas sensitive, and the gas sensitive is coated uniformly on electrode member
Surface, electrode member are plane electrode.
6. H described in claim 52The preparation method of S gas sensor, which is characterized in that the method is as follows:
1. by SnO described in claim 12Nano material is poured into the 2ml conical centrifuge tube equipped with 0.5ml dehydrated alcohol, super
It is uniformly dispersed in sonic oscillator, until solution presentation white is suspended, obtains suspension；
2. suspension is dripped on electrode element surface dropwise, with hot blast drying, and repeatedly operation until sensitive layer thickness
About 2mm；
3. electrode member is welded in the detection pedestal of air-sensitive test macro, it is subsequently placed on agingtable with 2 DEG C/min heating
To 200~300 DEG C and 24~36h is kept the temperature, is obtained with SnO2Nano material is the H of sensitive layer2S gas sensor.
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Cited By (3)
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| CN110261445A (en) * | 2019-07-12 | 2019-09-20 | 东北大学 | One kind growing nanometer In based on nonmetallic mineral electrode substrate surface in situ2O3Room temperature NO2Sensor and preparation method |
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
| CN112225245A (en) * | 2019-06-28 | 2021-01-15 | 东北大学 | Rare earth element doped SnO2Basic high response SO2Method for preparing sensitive material |
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| CN102623635A (en) * | 2012-03-29 | 2012-08-01 | 杭州电子科技大学 | Tin dioxide based resistance type random read memorizer and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225245A (en) * | 2019-06-28 | 2021-01-15 | 东北大学 | Rare earth element doped SnO2Basic high response SO2Method for preparing sensitive material |
| CN110261445A (en) * | 2019-07-12 | 2019-09-20 | 东北大学 | One kind growing nanometer In based on nonmetallic mineral electrode substrate surface in situ2O3Room temperature NO2Sensor and preparation method |
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
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