CN108398464A - A kind of H2S sensors and preparation method thereof based on hollow spherical structure La doped indium oxide nano sensitive materials - Google Patents
A kind of H2S sensors and preparation method thereof based on hollow spherical structure La doped indium oxide nano sensitive materials Download PDFInfo
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- CN108398464A CN108398464A CN201810196908.2A CN201810196908A CN108398464A CN 108398464 A CN108398464 A CN 108398464A CN 201810196908 A CN201810196908 A CN 201810196908A CN 108398464 A CN108398464 A CN 108398464A
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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
Abstract
A kind of H based on hollow spherical structure La doped indium oxide nano sensitive materials2Sensor and preparation method thereof belongs to conductor oxidate gas sensor technical field.The Al of two parallel, cyclic annular and separate gold electrodes is carried by outer surface2O3Ceramic tube substrate is coated in Al2O3La doped indium oxides nano sensitive material on ceramic tube outer surface and gold electrode is placed in Al2O3Ni-Cd heating coil composition in ceramic tube.By in In2O3La elements are adulterated in hollow ball, are improved to H2The Monitoring lower-cut of the sensitivity of S, material is relatively low, and with quickly response resume speed and good repeatability, has broad application prospects in terms of detection level；The method of the invention has synthesis step simple, of low cost, small, the good characteristics for being suitable for producing in enormous quantities.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical fields, and in particular to one kind being based on hollow spherical structure La
The H of doped indium oxide nano sensitive material2Sensor and preparation method thereof.
Background technology
Hydrogen sulfide (H2S it is) colourless, has the poisonous gas of rotten egg smell.As the H containing 0.1% volume in air2When S,
It will cause people's headache, dizzy.As a large amount of H of sucking2It when S, can cause to go into a coma, or even dead.With H2S contact is more, can cause slow
Property poisoning, make to feel to degenerate, headache is become thin.H2S is industrially the important by-products of production oil, plastics, rubber, and
And be to belong to inflammable gas, explosive mixture can be formed by being mixed with air, encounter open fire, high thermal energy easily causes explosion.Work
In industry production, it is desirable that H in air2The content of S must not exceed 0.01 mg/litre.Therefore, H2The detection of S gases has particularly significant
Meaning.
In the gas sensor of huge number, using conductor oxidate as the resistor-type gas sensing utensil of sensitive material
Have the advantages that high sensitivity, Monitoring lower-cut are low, selectivity is good, respond and resume speed is fast, production method is simple, cost is relatively low,
It is one of current most widely used gas sensor.With the development of nanometer science and technology, by gas sensitive regulation and control at receiving
Rice structure can greatly improve the specific surface area of material, increase active site, gas-sensitive property can be made to be improved.In addition,
It is found that the semiconductor oxide composite adulterated by heterogeneous dopant can significantly improve the sensitivity of sensor
And selectivity.This, which is primarily due to doped metal ion, can improve the carrier mobility of sensing material, to improve it
" conversion function "；Secondly, some metal dopants can be used as catalyst to make to be happened at the corresponding oxygen in conductor oxidate surface
Change reduction reaction to be catalyzed, the selectivity of sensor can be improved, improved " identification function " of sensing material.Based on this
Point carries out designing and preparing for metal-doped oxide semiconductor, has for the application of enlargement gas sensor very heavy
The scientific meaning wanted.
Invention content
The object of the present invention is to provide a kind of H based on hollow spherical structure La doped indium oxide nano sensitive materials2S is sensed
Device and preparation method thereof.The present invention increases the sensitivity of sensor, improves sensor by being doped to semi-conducting material
Response speed improves the repeatability of sensor, promotes such sensor in H2The functionization of S field of gas detection.
The obtained sensor of the present invention has preferable selectivity, repeatability other than with higher sensitivity
And long-time stability.The sensor is to H2The Monitoring lower-cut of S is 1ppm, H as defined in European Union2S gas detections limit 500ppb~
10ppm.Therefore, inventive sensor can be used for H in atmospheric environment2The detection of S steam contents.It is of the present invention commercially available
Tubular structure sensor, manufacture craft is simple, small, is conducive to industrial batch production, therefore have important application value.
H of the present invention based on hollow spherical structure La doped indium oxide nano sensitive materials2Sensor, by appearance
Face carries the Al of two parallel, cyclic annular and separate gold electrodes2O3Ceramic tube substrate is coated in Al2O3Ceramic tube outer surface
With on gold electrode nano sensitive material, be placed in Al2O3Ni-Cd heating coil composition in ceramic tube；It is characterized in that：Nanometer is quick
Sense material is La doped indium oxides, and is prepared by following steps,
(1) by the In (NO of 0.22~0.26g3)3·4.5H2O, the La (NO of 2.2~11.1mg3)3·6H2O, 0.4~
The urea of 0.5g is dissolved in the in the mixed solvent of 30~40mL absolute ethyl alcohols and 2~5mL polyethylene glycol, it is sufficiently stirred 40~
60min, then 15~20min of ultrasound；
(2) solution for obtaining step (1) 10~12h of hydro-thermal reaction under the conditions of 160~170 DEG C；
(3) product that step (2) obtains is cooled to room temperature, then uses water and ethyl alcohol alternately centrifuge washing, will
To product be dried, finally at 450~550 DEG C calcine 2~3h, to obtain La adulterate In2O3Nano sensitive material.
Involved sensor uses heater-type structure, specific preparation process as follows in the present invention：
(1) La is taken to adulterate In2O3Nano sensitive material, with absolute ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform is mixed
Conjunction forms slurry；Slurry coating, which is dipped, with hairbrush carries two parallel, cyclic annular and separate gold electrodes on the surface
Al2O3Ceramic tube outer surface, makes it be completely covered on Al2O3The thickness of ceramic tube outer surface and gold electrode, nano sensitive material is
15~30um；Al2O3The internal diameter of ceramic tube is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；Single gold electricity
The width of pole is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm；Platinum filament wire, length are drawn on gold electrode
For 4~6mm；
(2) Al for having coated nano sensitive material for obtaining step (1)2O3Ceramic tube is sintered 1 at 350~450 DEG C~
Then the ni-Cd heating coil (the number of turns is 50~60 circles) that resistance value is 30~40 Ω is passed through Al by 3h2O3Ceramic tube inside leads to
Suitable operating temperature is provided for sensor with direct current, is then welded on heater-type hexagonal tube socket；
(3) device for obtaining step (2) aging 5~7 days in 200~400 DEG C of air environments, to obtain based on sky
The H of the La doped indium oxide nano sensitive materials of bulbus cordis structure2Sensor.
Operation principle：
When La adulterates In2O3H2When sensor is placed in air, the oxygen molecule in air will be from In2O3Capture electricity
Son and with O2 -、O-Or O2-Mode exist, material surface forms depletion layer, and resistance increases.When sensor is in certain suitable temperature
Lower contact H2When S gases, H2S gas molecules will be adsorbed on sensor surface, and release trapped electron returns to In2O3Conduction band, to make
In2O3Resistance declines.The sensitivity that we define sensor herein is S：S=Ra/Rg, wherein RaBetween sensor gold electrode
Resistance in air, RgH is contacted between sensor gold electrode2Resistance after S.
H based on hollow spherical structure La doped indium oxide sensitive materials prepared by the present invention2Sensor has following excellent
Point：
1. can prepare the material of hollow-core construction using simple hydro-thermal method, synthetic method is simple, of low cost；
2. by In2O3La elements are adulterated in hollow ball, are improved to H2The sensitivity of S, the Monitoring lower-cut of material compared with
It is low, and with quickly response resume speed and good repeatability, have broad application prospects in terms of detection level；
3. using commercially available tubular type sensor, device technology is simple, small, is suitable for producing in enormous quantities.
Description of the drawings
Fig. 1：La adulterates In2O3H2The structural schematic diagram of sensor；Left figure is sensor welded condition schematic diagram, right figure
For sensor sectional view.
Fig. 2：The stereoscan photograph of the sample of comparative example, embodiment 1, embodiment 2 and embodiment 3.
Fig. 3：Comparative example and embodiment 2 are at 200 DEG C to 10ppm H2Pair of 6 kinds of gas with various responses of S and 50ppm
Than figure.
Fig. 4：The H of comparative example, embodiment 1, embodiment 2 and embodiment 3 to 10ppm2The response of S gases and work temperature
The relation curve of degree.
Fig. 5：Comparative example and embodiment 2 are under optimum working temperature, to the H of various concentration2The response curve of S gases.
As shown in Figure 1, the names of the parts are：Platinum filament pin 1, nichrome heating coil 2, La adulterate In2O3Nanometer is sensitive
Material 3, annular gold electrode 4, Al2O3Ceramics pipe outer 5, pedestal 6；
Fig. 2 is the stereoscan photograph of the sample of comparative example, embodiment 1, embodiment 2 and embodiment 3.It can from figure
Go out, gained sample is the nanosphere with hollow-core construction.Also, with the increase of doping, form the nano particle of bouquet
Size is gradually reduced, and illustrates that the incorporation of La inhibits In2O3The growth of crystal grain.The picture of insertion is corresponding high power scanning electron microscope
Figure, by apparent hollow ball structure can be clearly seen in figure, and the thickness of hollow ball ball wall is substantially in 300~400nm.
Fig. 3 be comparative example and embodiment 2 at 200 DEG C to 10ppm H2Pair of 6 kinds of gas with various responses of S and 50ppm
Than figure.It can be seen from the figure that embodiment all has a certain upgrade to the response of most of gas compared to comparative example.
Fig. 4 is comparative example, embodiment 1, embodiment 2 and embodiment 3 to 10ppm H2The response of S gases and work
The relation curve of temperature.It can be seen from the figure that the optimum working temperature of four groups of samples is 200 DEG C.Wherein, the spirit of comparative example
Sensitivity is 3.71, and the sensitivity of embodiment 1 is 7.49, and the sensitivity of embodiment 2 is 17.8, and the sensitivity of embodiment 3 is 10.7.
Under optimum working temperature, the sensitivity highest of embodiment 2, about the 4.8 of comparative example sensitivity times.It can be seen that by mixing
The reaction efficiency of sensitive material and acetone can be improved by entering La ions, and then having obtained one, there is highly sensitive La to adulterate
In2O3Oxide semiconductor H2Sensor.
Fig. 5 is comparative example and embodiment 2 under optimum working temperature, to various concentration H2The response curve of S gases.It is sensitive
Spend test method：Sensor is put into gas cabinet first, resistance at this time is measured by the ammeter being connect with sensor, is passed
Aerial resistance value, that is, the R of sensora；Then microsyringe is used to inject the H of 1~200ppm into gas cabinet2S passes through survey
Sensor is measured in various concentration H2Resistance value, that is, R in Sg, according to the defined formula S=R of sensitivity Sa/Rg, pass through calculating
The sensitivity of various concentration lower sensor is obtained, H is finally obtained2The standard working curve (illustration) of S concentration-sensitivity.From figure
In as can be seen that the Monitoring lower-cut of 2 sensor of embodiment is 1ppm, sensitivity at this time is 2.48；Work as H2A concentration of 200ppm of S
When, the sensitivity of comparative example and embodiment 2 at this time is respectively 42.2 and 111.9, and response tends to be saturated.
R can be measured when practical measurement by above-mentioned methoda、Rg, obtain after Sensitirity va1ue with H2The mark of S concentration-sensitivity
Quasi- working curve is compared, to obtain the H in environment2S contents.
Specific implementation mode
Comparative example：
With In2O3Hollow ball makes heater-type H as sensitive material2Sensor, specific manufacturing process：
1. first by the In (NO of 0.26g3)3·4.5H2O, 0.5g urea are dissolved in 35mL absolute ethyl alcohols and the poly- second of 3mL two
The in the mixed solvent of alcohol is sufficiently stirred 50min, then ultrasound 20min；
2. above-mentioned solution is encased in 50mL water heating kettles, it is subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 12h；
3. obtained product water and ethyl alcohol alternately after reaction, are carried out centrifuge washing.Centrifuge parameters are set as
10000r/min, 10min.Product is dried after centrifugation.After drying, product at 500 DEG C is subjected to calcining 2h, obtained
In2O3Nano material.
4. taking appropriate In obtained2O3Nano material and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With
Hairbrush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, and making it that the gold electrode of outer surface be completely covered, (tubular ceramic serves as a contrast
The internal diameter at bottom is 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold being mutually parallel are come on its outer surface
Electrode, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 400 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, to obtain In2O3H2Sensor.
6. finally by sensor in 250 DEG C of air environments aging 6 days, to obtain In2O3The H of nano sensitive material2S
Sensor.
Embodiment 1：
With the molar ratio of La ions/In ions for 0.01:1 La adulterates In2O3Hollow ball makes indirect heat as sensitive material
Formula H2Sensor, manufacturing process are：
1. first by the In (NO of 0.26g3)3·4.5H2La (the NO of O, 2.2mg3)3·6H2O, 0.5g urea are dissolved in
The in the mixed solvent of 35mL absolute ethyl alcohols and 3mL polyethylene glycol is sufficiently stirred 50min, then ultrasound 20min；
2. above-mentioned solution is encased in 50mL water heating kettles, it is subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 12h；
3. obtained product water and ethyl alcohol alternately after reaction, are carried out centrifuge washing.Centrifuge parameters are set as
10000r/min, 10min.Product is dried after centrifugation.After drying, product at 500 DEG C is subjected to calcining 2h, obtained
In2O3Nano material.
4. taking appropriate In obtained2O3Nano material and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With
Hairbrush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, and making it that the gold electrode of outer surface be completely covered, (tubular ceramic serves as a contrast
The internal diameter at bottom is 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold being mutually parallel are come on its outer surface
Electrode, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 400 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, to obtain In2O3H2Sensor.
6. finally by sensor in 250 DEG C of air environments aging 6 days, to obtain In2O3The H of nano sensitive material2S
Sensor.
Embodiment 2：
With the molar ratio of La ions/In ions for 0.03:1 La adulterates In2O3Hollow ball makes indirect heat as sensitive material
Formula H2Sensor, manufacturing process are：
1. first by the In (NO of 0.26g3)3·4.5H2La (the NO of O, 6.6mg3)3·6H2O, 0.5g urea are dissolved in
The in the mixed solvent of 35mL absolute ethyl alcohols and 3mL polyethylene glycol is sufficiently stirred 50min, then ultrasound 20min；
2. above-mentioned solution is encased in 50mL water heating kettles, it is subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 12h；
3. obtained product water and ethyl alcohol alternately after reaction, are carried out centrifuge washing.Centrifuge parameters are set as
10000r/min, 10min.Product is dried after centrifugation.After drying, product at 500 DEG C is subjected to calcining 2h, obtained
In2O3Nano material.
4. taking appropriate In obtained2O3Nano material and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With
Hairbrush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, and making it that the gold electrode of outer surface be completely covered, (tubular ceramic serves as a contrast
The internal diameter at bottom is 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold being mutually parallel are come on its outer surface
Electrode, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 400 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, to obtain In2O3H2Sensor.
6. finally by sensor in 250 DEG C of air environments aging 6 days, to obtain In2O3The H of nano sensitive material2S
Sensor.
Embodiment 3：
With the molar ratio of La ions/In ions for 0.05:1 La adulterates In2O3Hollow ball makes indirect heat as sensitive material
Formula H2Sensor, manufacturing process are：
1. first by the In (NO of 0.26g3)3·4.5H2La (the NO of O, 11.1mg3)3·6H2O, 0.5g urea are dissolved in
The in the mixed solvent of 35mL absolute ethyl alcohols and 3mL polyethylene glycol is sufficiently stirred 50min, then ultrasound 20min；
2. above-mentioned solution is encased in 50mL water heating kettles, it is subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 12h；
3. obtained product water and ethyl alcohol alternately after reaction, are carried out centrifuge washing.Centrifuge parameters are set as
10000r/min, 10min.Product is dried after centrifugation.After drying, product at 500 DEG C is subjected to calcining 2h, obtained
In2O3Nano material.
4. taking appropriate In obtained2O3Nano material and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With
Hairbrush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, and making it that the gold electrode of outer surface be completely covered, (tubular ceramic serves as a contrast
The internal diameter at bottom is 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold being mutually parallel are come on its outer surface
Electrode, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 400 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, to obtain In2O3H2Sensor.
6. finally by sensor in 250 DEG C of air environments aging 6 days, to obtain In2O3The H of nano sensitive material2S
Sensor.
Claims (4)
1. a kind of H based on hollow spherical structure La doped indium oxide nano sensitive materials2Sensor, it is flat with two by outer surface
Row, cyclic annular and gold electrode separate Al2O3Ceramic tube substrate is coated in Al2O3On ceramic tube outer surface and gold electrode
Nano sensitive material is placed in Al2O3Ni-Cd heating coil composition in ceramic tube；It is characterized in that：Nano sensitive material is mixed for La
Miscellaneous indium oxide nano sensitive material, is prepared by following steps,
(1) by the In (NO of 0.22~0.26g3)3·4.5H2O, the La (NO of 2.2~11.1mg3)3·6H2O, 0.4~0.5g
Urea is dissolved in the in the mixed solvent of 30~40mL absolute ethyl alcohols and 2~5mL polyethylene glycol, is sufficiently stirred 40~60min, then
15~20min of ultrasound；
(2) solution for obtaining step (1) 10~12h of hydro-thermal reaction under the conditions of 160~170 DEG C；
(3) product that step (2) obtains is cooled to room temperature, water and ethyl alcohol alternately centrifuge washing is then used, by what is obtained
Product is dried, and 2~3h is finally calcined at 450~550 DEG C, and In is adulterated to obtain La2O3Nano sensitive material.
2. a kind of H based on hollow spherical structure La doped indium oxide nano sensitive materials as described in claim 12Sensor,
It is characterized in that：The thickness of nano sensitive material is 15~30um.
3. a kind of H based on hollow spherical structure La doped indium oxide nano sensitive materials as described in claim 12Sensor,
It is characterized in that：Al2O3The internal diameter of ceramic tube is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；Single gold
The width of electrode is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm；Platinum filament wire is drawn on gold electrode, is grown
Degree is 4~6mm.
4. a kind of described in claims 1 to 3 any one is based on hollow spherical structure La doped indium oxide nano sensitive materials
H2The preparation method of sensor, its step are as follows：
(1) La is taken to adulterate In2O3Nano sensitive material, with absolute ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform mixes shape
At slurry；The Al that slurry coating carries two parallel, cyclic annular and separate gold electrodes on the surface is dipped with hairbrush2O3
Ceramic tube outer surface, makes it be completely covered on Al2O3Ceramic tube outer surface and gold electrode；
(2) Al for having coated nano sensitive material for obtaining step (1)2O3Ceramic tube is sintered 1~3h at 350~450 DEG C,
Then the ni-Cd heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside passes to direct current to be carried for sensor
For suitable operating temperature, then it is welded on heater-type hexagonal tube socket；
(3) device for obtaining step (2) aging 5~7 days in 200~400 DEG C of air environments, to obtain being based on hollow ball
The H of structure La doped indium oxide nano sensitive materials2Sensor.
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