CN107607591A - One kind is based on SnO2Hypersensitive toluene gas sensor of NiO nanostructured sensitive materials of modification and preparation method thereof - Google Patents
One kind is based on SnO2Hypersensitive toluene gas sensor of NiO nanostructured sensitive materials of modification and preparation method thereof Download PDFInfo
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Abstract
One kind is based on SnO2Hypersensitive toluene gas sensor of NiO nanostructured sensitive materials of modification and preparation method thereof, belongs to conductor oxidate gas sensor technical field.Sensor construction is by the commercially available Al with 2 annular gold electrodes2O3Ceramics pipe outer, coated in annular gold electrode and Al2O3Semiconductor sensitive material in ceramics pipe outer and through Al2O3The nichrome heating coil composition of ceramics pipe outer.The present invention utilizes N-type SnO2The method of semi-conducting material modification is modified to p-type NiO semiconductor sensitive materials, realizes the very big leap of gas-sensitive property.Based on SnO2The NiO nanostructured sensitive material sensors of modification show the selectivity of brilliance and sensitivity (60.2~100ppm) and the extremely low Monitoring lower-cut (10ppb) of moisture resistance and superelevation to toluene.Device technology is simple, small volume, suitable for producing in enormous quantities, has broad application prospects in terms of Toluene pollutant in detecting microenvironment.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical field, and in particular to one kind is based on SnO2Modification
Hypersensitive toluene gas sensor of NiO nanostructured sensitive materials and preparation method thereof.
Background technology
With the progress and growth in the living standard of society, the life style of people is varied widely, more and more
People devote a tremendous amount of time work and amusement indoors, indoor air quality is also increasingly taken seriously.Toluene is indoor
One of representative pollutant of VOC (VOCs) in environment, can be from construction material, ornament materials, wood furniture
Discharged with carpet.It is well known that it not only results in environmental pollution, and directly threaten human health.Therefore, grind
Fixture has a good selectivity, and the toluene gas sensors of high sensitivity and low detection limits is to realize the height to toluene gas in environment
Effect detection tool is of great significance.
In the gas sensor of huge number, the resistor-type gas sensing utensil using conductor oxidate as sensitive material
Have the advantages that high sensitivity, Monitoring lower-cut are low, selectivity is good, response and resume speed are fast, preparation method is simple, cost is relatively low,
It is one of current most widely used gas sensor.And mainly have following three for the modified method of semiconductor sensitive material
Kind：Noble metal supports, aliovalent metal ion mixing and formation composite, wherein, it is a kind of effective to form composite
Method of modifying.Substantial amounts of achievement in research shows that the homojunction or hetero-junctions formed in composite are to carrier concentration and lead
Electric raceway groove has preferable regulating and controlling effect, can effectively lift the gas-sensitive property of sensitive material.
Nickel oxide (NiO) is a kind of important P-type mos, because it has stabilization chemically and electrically
Property, it is widely used in the fields such as energy storage, lithium ion battery, catalyst and gas sensor.To NiO nanostructured sensitivities
The research of energy shows that, although compared with some N-type metal-oxide semiconductor (MOS)s, its sensitivity is relatively low, but nickel oxide exists
There is outstanding catalytic activity in terms of oxidation to VOC (VOC), this causes the modification to NiO sensitive materials
Become significant.SnO has been prepared using the method for forming Nano semiconductor PN heterojunction in this patent2The NiO nanometers of modification
Structure sensitive material, realize air-sensitive performance and greatly leap,
The content of the invention
It is an object of the invention to provide one kind to be based on SnO2The hypersensitive toluene gas of the NiO nanostructured sensitive materials of modification
Body sensor and preparation method thereof.
Utilize SnO2The NiO nanostructureds of modification have as sensitive material, on the one hand unmodified NiO nano flower balls
Stronger oxidisability, and all there is preferable catalytic oxidation activity to a variety of VOC gas, more oxygen molecules can be caused to participate in
Reaction；Moreover, by carrying out SnO to NiO2Moditied processing, the specific surface area (improving 3 times) of material is drastically increased, is made
The enhancing of oxygen ability must be adsorbed；Further, since foring the heterogeneous semiconductor PN junction of nanoscale, realize has to conducting channel
Effect regulation and control, i.e., the change of small conducting channel thickness cause the significant changes of material resistance.Three aspects is common based on more than
Effect, sensor show sensitivity (60.2~100ppm) and the extremely low Monitoring lower-cut (10ppb) of superelevation to toluene gas,
In addition selectivity and moisture resistance also have a distinct increment.Commercially available tubular structure sensor manufacturing process letter of the present invention
It is single, small volume, beneficial to industrial batch production, therefore there is important application value.
One kind of the present invention is based on SnO2The hypersensitive toluene gas sensing of the NiO nanostructured sensitive materials of modification
Device, by Al of the outer surface with two parallel, ring-types and gold electrode separate2O3Earthenware substrate, coated in Al2O3Pottery
Sensitive material on porcelain tube outer surface and gold electrode, it is placed in Al2O3Nichrome heating coil composition in earthenware；Its feature
It is：Sensitive material is SnO2The NiO nano structural materials of modification, and be prepared by following steps,
(1) by 0.1~0.4g SnCl4.5H2O, 0.4~0.7g NiCl2·6H2(six is sub- by O and 0.2~0.4g HMT
Tetramine) it is added in 20~40mL deionized waters, it is stirred continuously until it all dissolves, then adds 1~4mL second thereto
Hydramine；
(2) above-mentioned solution being transferred in water heating kettle, hydro-thermal reaction is taken out after 10~14 hours at 140~200 DEG C, from
So it is cooled to the multiple eccentric cleaning of precipitation deionized water and ethanol of generation after room temperature, exists again after being then dried at room temperature for
Calcined 1~3 hour at 300~500 DEG C, so as to obtain SnO2The NiO nano structural material powder of modification.
One kind of the present invention is based on SnO2The hypersensitive toluene gas sensing of the NiO nanostructured sensitive materials of modification
The preparation method of device, its step are as follows：
(1) SnO is taken2The NiO nano structural materials powder (10~20mg) of modification is mixed with deionized water (40~100 μ L)
Close, and grind form pasty slurry, then dip a small amount of slurry be uniformly coated on outer surface with two parallel, ring-types and that
The Al of this discrete gold electrode2O3Earthenware substrate surface, sensitive material film is formed, and make sensitive material that annular be completely covered
Gold electrode；
(2) toasted 30~45 minutes under infrared lamp, after sensitive material drying, Al2O3Earthenware is 300~500
Calcined 1~3 hour at DEG C；Then the nichrome heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside
As heater strip, finally above-mentioned device is welded and encapsulated according to general heater-type gas sensor, so as to be based on
SnO2The hypersensitive toluene gas sensor of the NiO nanostructured sensitive materials of modification.Wherein, Al2O3A length of the 4 of earthenware~
4.5mm, external diameter are 1.2~1.5mm, and internal diameter is 0.8~1.0mm.
The present invention prepare based on SnO2The hypersensitive toluene gas sensing utensil of the NiO nanostructured sensitive materials of modification
Have the advantage that：
1. successfully prepare SnO using the simple hydro-thermal method of a step2The NiO nanostructured sensitive materials of modification, synthesis side
Method is simple, and cost is cheap；
2. by carrying out SnO to NiO sensitive materials2The processing of modification, improve choosing of the NiO bases gas sensor to toluene
Selecting property and moisture resistance, sensitivity (60.2~100ppm) is drastically increased, under the gas concentration detection for reducing sensitive material
Limit (1.2~10ppb), and there is good repeatability and stability, have extensively in detection Environmental Trace toluene concentration object space face
Wealthy application prospect；
3. using commercially available tubular type sensor, device technology is simple, small volume, suitable for producing in enormous quantities.
Brief description of the drawings
Fig. 1：(a, b) is respectively unmodified NiO (comparative example 1) and SnO2Modify the SEM of NiO (embodiment 1) nanostructured
Shape appearance figure；
Fig. 2：(a, b) is respectively SnO2Modify the XRD of NiO (embodiment 1) and unmodified NiO (comparative example 1) nanostructured
Spectrum；
Fig. 3：(a) in comparative example 1 and embodiment 1 sensor at a temperature of different operating to the sensitive of 100ppm toluene gas
Write music line；(b) in comparative example 1 and embodiment 1 sensor at 250 DEG C to the selective column of 8 kinds of 100ppm under test gas
Figure；
Fig. 4：(a) for working sensor at 250 DEG C, resistance is relative to electric under 30% humidity under different humidity in embodiment 1
The change curve of resistance；(b) for working sensor at 250 DEG C, sensitivity is relative under 30% humidity under different humidity in embodiment 1
The change curve of sensitivity；
Fig. 5：(a) electricity with toluene concentration real-time change of the sensor under optimum working temperature (250 DEG C) in embodiment 1
Characteristic curve is hindered, sensitivity of the sensor under optimum working temperature (250 DEG C) is special with toluene concentration change in (b) embodiment 1
Linearity curve；
Fig. 6：(a) in comparative example 1 and embodiment 1 sensor under respective optimum working temperature on toluene concentration gradient
The sensitivity curve figure of (1~200ppm)；(b) in embodiment 1 working sensor in optimum working temperature in (250 DEG C) air
Resistance and the linearity curve steady in a long-term in 100ppm toluene gas medium sensitivities；
As shown in figure 1, unmodified NiO (comparative example 1) is graduation nano flower spherical structure, and favorable dispersibility, single nanometer
Bouquet is made up of the two-dimensional nano piece of many flexural deformations, and the diameter of nanometer bouquet is about 2.5~4.5 μm. SnO2Modify NiO
(embodiment 1) is the irregular nanostructured that nanoparticle aggregate is formed.
As shown in Fig. 2 SnO2Substantially there is SnO in the XRD spectra of modification NiO (embodiment 1) nanostructured2With spreading out for NiO phases
Peak is penetrated, and the miscellaneous peak of other phases does not occur, shows SnO2Contain SnO simultaneously in modification NiO materials2With NiO two-phases, and do not repair
The XRD spectra of NiO (comparative example 1) nanometer bouquet is adornd compared with standard NiO, characteristic peak coincide, and the miscellaneous of other phases does not occur
Peak.
As shown in figure 3, the optimum working temperature of the sensor in comparative example 1 is 225 DEG C, the sensor in embodiment 1
Optimum working temperature is 250 DEG C, and now sensitivity of the device to 100ppm toluene is respectively 1.3 and 60.2, sensitivity enhancement
46 times, and it is best to the selectivity of toluene, for sensor in comparative example 1, the sensor gas sensing property in embodiment 1
Can have and greatly be lifted.
As shown in figure 4, at 250 DEG C, the initial resistance in air increases and increased working sensor with humidity in embodiment 1
Greatly, sensitivity increases and reduced with humidity, and this coincide with variation tendency reported in the literature.In addition, under different humidity resistance and
Sensitivity is smaller (ratio is near 1) relative to the change of resistance and sensitivity under 30% humidity, shows superior moisture resistance
Energy.
As shown in figure 5, for the sensor of embodiment 1 in toluene, the resistance of semiconductor becomes big, this characteristic with
The gas-sensitive property of p-type oxide semiconductor is consistent, and sensor shows excellent response and extensive to the toluene of various concentrations
Multiple characteristic.When the device of embodiment 1 is in the case where operating temperature is 250 DEG C, the sensitivity of device increases with the increase of toluene concentration,
In addition, the Monitoring lower-cut of the sensor of embodiment 1 is relatively low, ppb ranks can be reached, the sensitivity to 10ppb toluene is 1.2, table
SnO in bright embodiment 12The NiO sensors of modification can be used for the detection of trace toluene pollutant in environment.
As shown in fig. 6, for sensor in comparative example 1, with the increase of toluene gas concentration, in embodiment 1
Sensor sensitivity enhancement it is obvious, and preferable linear increase relation is shown between sensitivity and concentration.And
In 20 days of follow-on test, the aerial initial resistance of sensor and its phase that are operated in the embodiment 1 at a temperature of 250 DEG C
The fluctuation of the sensitivity curve in 100ppm toluene gas answered is smaller, shows its good long-time stability.
Note：Found during actual test, the gas-sensitive property of sensor is best in embodiment 1, hence it is evident that better than embodiment 2 and in fact
The gas sensor in example 3 is applied, it is more representative.So as shown in Figures 1 to 6, emphasis is to embodiment 1 and right in this patent
The gas-sensitive property of sensor carries out comparative study in ratio 1, hence it is evident that and representative show the SnO synthesized by hydro-thermal method2
The remarkable toluene gas that the NiO nanostructureds sensitive material of modification is shown relative to unmodified NiO sensitive materials senses
Characteristic.In addition, the sensitivity (P-type semiconductor) for device is being defined as it in tested gas in testing reducibility gas
Resistance value (Rg) with resistance value (R in atmosphereaThe ratio between) size, as S=Rg/Ra.In test process, static test is used
System is tested, and device is placed in 50~80L gas tank, inwardly injects a certain amount of under test gas, is observed and is recorded it
Change in resistance, by the way that corresponding sensitivity number is calculated.
Embodiment
Comparative example 1：
Toluene Gas Sensor is made by the use of unmodified NiO graded structures nanometer bouquet as sensitive material, its specific making
Process：
(1) 30mL deionized waters are measured first, are poured into beaker, and are constantly stirred；
(2) by 0.47g NiCl2·6H2O and 0.28g HMT (hexa) are added to equipped with deionized water
In beaker, and constantly stirring is kept until it all dissolves, then adds 2mL monoethanolamines to it；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 12 hours at 160 DEG C, naturally cool to room temperature
Afterwards by the multiple eccentric cleaning of precipitation deionized water and ethanol of generation, 2 are calcined at 400 DEG C again after being then dried at room temperature for
Hour, so as to obtain unmodified NiO graded structure nanometer bouquet powder；
(4) the unmodified NiO graded structures nanometer bouquet powder prepared in right amount with hydro-thermal method is taken to be mixed with deionized water,
And grind and form pasty slurry, then dip a small amount of slurry and be uniformly coated on outer surface and come with 2 annular gold electrodes
Al2O3Ceramic pipe surface, sensitive material film is formed, and make sensitive material that annular gold electrode be completely covered, sensitive material film
Thickness is 45 μm；
(5) toasted 30 minutes under infrared lamp, after sensitive material drying, Al2O3It is small that earthenware calcines 2 at 400 DEG C
When；Then the nichrome heating coil that resistance value is 32 Ω is passed through into Al2O3Ceramic tube inside, finally will be upper as heater strip
State device to be welded and encapsulated according to general heater-type gas sensor, so as to obtain receiving based on unmodified NiO graded structures
The toluene gas sensor of popped rice ball sensitive material.
Embodiment 1：
Use SnO2The NiO nanostructureds of modification make hypersensitive toluene gas sensor as sensitive material, and its is specific
Manufacturing process：
(1) 30mL deionized waters are measured first, are poured into beaker, and are constantly stirred；
(2) by 0.17g SnCl4.5H2O, 0.47g NiCl2·6H2O and 0.28g HMT (hexa) are added
Into the beaker equipped with deionized water, and constantly stirring is kept until it all dissolves, then adds 2mL monoethanolamines to it；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 12 hours at 160 DEG C, naturally cool to room temperature
Afterwards by the multiple eccentric cleaning of precipitation deionized water and ethanol of generation, 2 are calcined at 400 DEG C again after being then dried at room temperature for
Hour, so as to obtain SnO2The NiO nanostructured powders of modification, product quality 0.14g；
(4) SnO prepared in right amount with hydro-thermal method is taken2The NiO nanostructured powders (12.6mg) of modification and deionized water (50
μ L) mixing, and grind form pasty slurry, then dip a small amount of slurry be uniformly coated on outer surface come with 2 annular gold
The Al of electrode2O3Ceramic pipe surface, sensitive material film is formed, and make sensitive material that annular gold electrode, sensitive material be completely covered
The thickness of film is 58 μm；
(5) toasted 30 minutes under infrared lamp, after sensitive material drying, Al2O3It is small that earthenware calcines 2 at 400 DEG C
When；Then the nichrome heating coil that resistance value is 32 Ω is passed through into Al2O3Ceramic tube inside, finally will be upper as heater strip
State device to be welded and encapsulated according to general heater-type gas sensor, so as to obtain being based on SnO2The NiO nanostructureds of modification
The hypersensitive toluene gas sensor of sensitive material.
Wherein, Al2O3A length of 4.2mm of earthenware, external diameter 1.3mm, internal diameter 0.9mm.
Embodiment 2：
Use SnO2The NiO nanostructureds of modification make toluene gas sensor as sensitive material, and it specifically made
Journey：
(1) 40mL deionized waters are measured first, are poured into beaker, and are constantly stirred；
(2) by 0.4g SnCl4.5H2O, 0.67g NiCl2·6H2O and 0.38g HMT (hexa) are added
Into the beaker equipped with deionized water, and constantly stirring is kept until it all dissolves, then adds 4 mL monoethanolamines to it；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 14 hours at 200 DEG C, naturally cool to room temperature
Afterwards by the multiple eccentric cleaning of precipitation deionized water and ethanol of generation, 3 are calcined at 500 DEG C again after being then dried at room temperature for
Hour, so as to obtain SnO2The NiO nanostructured powders of modification, product quality 0.23g；
(4) SnO prepared in right amount with hydro-thermal method is taken2The NiO nanostructured powders (12.6mg) of modification and deionized water (50
μ L) mixing, and grind form pasty slurry, then dip a small amount of slurry be uniformly coated on outer surface come with 2 annular gold
The Al of electrode2O3Ceramic pipe surface, sensitive material film is formed, and make sensitive material that annular gold electrode, sensitive material be completely covered
The thickness of film is 62 μm；
(5) toasted 40 minutes under infrared lamp, after sensitive material drying, Al2O3It is small that earthenware calcines 3 at 500 DEG C
When；Then the nichrome heating coil that resistance value is 36 Ω is passed through into Al2O3Ceramic tube inside, finally will be upper as heater strip
State device to be welded and encapsulated according to general heater-type gas sensor, so as to obtain being based on SnO2The NiO nanostructureds of modification
The toluene gas sensor of sensitive material.
Wherein, Al2O3A length of 4.2mm of earthenware, external diameter 1.3mm, internal diameter 0.9mm.
Embodiment 3：
Use SnO2The NiO nanostructureds of modification make toluene gas sensor as sensitive material, and it specifically made
Journey：
(1) 20mL deionized waters are measured first, are poured into beaker, and are constantly stirred；
(2) by 0.1g SnCl4.5H2O, 0.4g NiCl2·6H2O and 0.2g HMT (hexa) are added to
In beaker equipped with deionized water, and constantly stirring is kept until it all dissolves, then adds 1 mL monoethanolamines to it；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 10 hours at 140 DEG C, naturally cool to room temperature
It is small that at 300 DEG C 1 is forged afterwards by the multiple eccentric cleaning of precipitation deionized water and ethanol of generation, after being then dried at room temperature for again
When, so as to obtain SnO2The NiO nanostructured powders of modification, product quality 0.08g；
(4) SnO prepared in right amount with hydro-thermal method is taken2The NiO nanostructured powders (12.6mg) of modification and deionized water (50
μ L) mixing, and grind form pasty slurry, then dip a small amount of slurry be uniformly coated on outer surface come with 2 annular gold
The Al of electrode2O3Ceramic pipe surface, sensitive material film is formed, and make sensitive material that annular gold electrode, sensitive material be completely covered
The thickness of film is 64 μm；
(5) toasted 30 minutes under infrared lamp, after sensitive material drying, Al2O3It is small that earthenware calcines 1 at 300 DEG C
When；Then the nichrome heating coil that resistance value is 33 Ω is passed through into Al2O3Ceramic tube inside, finally will be upper as heater strip
State device to be welded and encapsulated according to general heater-type gas sensor, so as to obtain being based on SnO2The NiO nanostructureds of modification
The toluene gas sensor of sensitive material.
Wherein, Al2O3A length of 4.2mm of earthenware, external diameter 1.3mm, internal diameter 0.9mm.
Claims (3)
1. one kind is based on SnO2The hypersensitive toluene gas sensor of the NiO nanostructured sensitive materials of modification, is carried by outer surface
The Al of two parallel, ring-types and gold electrode separate2O3Earthenware substrate, coated in Al2O3Ceramic tube outer surface and gold electricity
Sensitive material on extremely, it is placed in Al2O3Nichrome heating coil composition in earthenware；It is characterized in that：Sensitive material is
SnO2The NiO nano structural materials of modification, and be prepared by following steps,
(1) by 0.1~0.4g SnCl4.5H2O, 0.4~0.7g NiCl2·6H2O and 0.2~0.4g hexas add
Enter into 20~40mL deionized waters, be stirred continuously until it all dissolves, then adds 1~4mL monoethanolamines thereto；
(2) above-mentioned solution is transferred in water heating kettle, hydro-thermal reaction is taken out after 10~14 hours at 140~200 DEG C, naturally cold
But to after room temperature by the multiple eccentric cleaning of precipitation deionized water and ethanol of generation, again 300 after being then dried at room temperature for
Calcined 1~3 hour at~500 DEG C, so as to obtain SnO2The NiO nano structural material powder of modification.
2. one kind described in claim 1 is based on SnO2The hypersensitive toluene gas sensing of the NiO nanostructured sensitive materials of modification
The preparation method of device, its step are as follows：
(1) SnO is taken2NiO 10~20mg of nano structural material powder of modification mix with 40~100 μ L deionized waters, and grind shape
Into pasty slurry, then dip a small amount of slurry and be uniformly coated on outer surface and carry two parallel, ring-types and gold separate
The Al of electrode2O3Earthenware substrate surface, sensitive material film is formed, and make sensitive material that annular gold electrode be completely covered；
(2) toasted 30~45 minutes under infrared lamp, after sensitive material drying, Al2O3Earthenware is forged at 300~500 DEG C
Burn 1~3 hour；Then the nichrome heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside is as heating
Silk, above-mentioned device is finally welded and encapsulated according to general heater-type gas sensor, so as to obtain being based on SnO2Modification
The hypersensitive toluene gas sensor of NiO nanostructured sensitive materials.
3. one kind as claimed in claim 2 is based on SnO2The hypersensitive toluene gas of the NiO nanostructured sensitive materials of modification passes
The preparation method of sensor, it is characterised in that：Al2O3A length of 4~4.5mm of earthenware, external diameter are 1.2~1.5mm, internal diameter 0.8
~1.0mm.
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