CN108508062A - One kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and applications - Google Patents
One kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and applications Download PDFInfo
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- CN108508062A CN108508062A CN201810255079.0A CN201810255079A CN108508062A CN 108508062 A CN108508062 A CN 108508062A CN 201810255079 A CN201810255079 A CN 201810255079A CN 108508062 A CN108508062 A CN 108508062A
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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
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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
Abstract
One kind being based on MoO3Triethylamine sensor, preparation method and its application in complex environment in terms of detection Triethylamine gas of nano sensitive material, belong to conductor oxidate gas sensor technical field.Sensor is heater-type structure, and the Al of two parallel, cyclic annular and separate gold electrodes is carried by outer surface2O3Ceramic tube substrate, coated in the MoO on ceramic tube outer surface and gold electrode3Nano sensitive material and the ni-Cd heating coil composition being placed in ceramic tube.The present invention utilizes the MoO for preparing simple, size uniformity3Nanometer sheet sensitive material has developed Triethylamine gas sensor with high performance to the recovery of triethylamine quick response, excellent selectivity, has good detection performance in complex environment environment, there is good application prospect.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical fields, and in particular to one kind being based on MoO3Nanometer is sensitive
Triethylamine sensor, preparation method and its application in complex environment in terms of detection Triethylamine gas of material.
Background technology
With the development of information technology, sensor is in the forward position of Information Technology Development as the means for obtaining information, will
It commercially produces by extensive concern and further.In recent years, atmosphere pollution is continuously increased, industry, household safe accident
Frequently occur, and the industries such as food security, health care, the chemical industry energy, military affairs, space flight there is an urgent need to.Therefore, it excavates
New gas sensor is detected pollution gas is of great significance in turn.
Triethylamine (TEA) is a kind of volatile organic matter compound (VOC), is widely used as catalyst, preservative, has
Solvent and synthetic dyestuffs, and a kind of industrial critically important raw material.But it has toxicity and volatility, it is inflammable and explosive
It is fried, if being compromised out in industrial processes, it is easy to damage environment and the mankind；Triethylamine can also be in dead fish
It is secreted in other marine organisms.Due to its toxicity and volatility, can cause to the strong of esophagus and stomach after mankind's sucking
Irritation may cause pulmonary edema even dead.Therefore, it is necessary to prepare the good material of selectivity, high sensitivity sensor,
Micro triethylamine is quickly detected with fast under industrial process and fish processing industry and more complicated environmental condition.
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.Many metal oxide semiconductors known to us, such as ZnO, SnO2、
WO3、Fe2O3And In2O3, it is obtained for extensive research, they show splendid sensitivity and response speed.However, more
This poor disadvantage of selectivity may limit their application under the conditions of complex environment.Sensitivity material used in the present invention
Expect MoO3It is a kind of typical n-type semiconductor, after being contacted with gas triethylamine, resistance declines rapidly；It is contacted with other gases
Resistance variations are little afterwards, i.e., the variation of gaseous environment are converted into detectable, distinguishing electric signal.Therefore exploitation has
High-performance, highly selective MoO3Base triethylamine sensor has a very important significance in every field such as environmental monitorings.
Invention content
The object of the present invention is to provide one kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and its
The application in terms of Triethylamine gas is detected in complex environment.
Heretofore described one kind being based on MoO3The Triethylamine gas sensor of nano sensitive material is heater-type knot
Structure is carried the Al of two parallel, cyclic annular and separate gold electrodes by outer surface2O3Ceramic tube substrate is coated in ceramic tube
Nano sensitive material on outer surface and gold electrode is formed with the ni-Cd heating coil being placed in ceramic tube, it is characterised in that：It receives
Rice sensitive material is MoO3Nano sensitive material.Sensor passes to direct current to provide biography at work, to ni-Cd heating coil
The operating temperature of sensor, D.C. resistance resistance value when by measuring in different atmosphere between two gold electrodes realize that measurement triethylamine is dense
The purpose of degree.Commercially available tubular structure sensor of the present invention, manufacture craft is simple, small, is conducive to industrial batch
Amount production, therefore there is important application value.Wherein, MoO3Nano sensitive material is prepared by following steps：
(1) first by 0.08g~0.09g (NH4)6Mo7O24·4H2O is dissolved in 20~40mL deionized waters, stirring 15
After~30min, then by the HNO of 3~5mL PEG-400 (polyethylene glycol) and 3~5mL, mass fraction 65%3It instills dropwise above-mentioned
In solution, continue 15~30min of stirring；
(2) above-mentioned solution is encased in water heating kettle, is subsequently placed into baking oven, 20~25h is reacted at 170~190 DEG C；
(3) after reaction, obtained product water and ethyl alcohol are alternately subjected to centrifuge washing, then dried, it is dry
1.5~3h of calcining is carried out at 450~550 DEG C afterwards, to obtain MoO3Nano sensitive material.
Involved sensor uses heater-type structure, specific preparation method as follows in the present invention：
(1) MoO is taken3Nano sensitive material, with ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform is mixed to form slurry
Material dips the Al that slurry coating carries two gold electrodes parallel, cyclic annular and separate on the surface with fine, soft fur brush2O3Ceramic tube
Outer surface makes it that gold electrode be completely covered；The thickness of the nano sensitive material of ceramic tube outer surface is 15~30 μm；Al2O3Ceramics
The internal diameter of pipe is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；The width of single gold electrode is 0.4~
The spacing of 0.5mm, two gold electrodes are 0.5~0.6mm；The platinum filament wire drawn on gold electrode, the length of 4~6mm；
(2) coated ceramic tube is sintered to 1.5~3h at 350~450 DEG C, is then 30~40 Ω's by resistance value
Ni-Cd heating coil (the number of turns is 50~60 circles) passes through Al2O3Ceramic tube inside passes to direct current to be provided suitably for sensor
Ceramic tube is welded on heater-type hexagonal tube socket by operating temperature finally by platinum filament wire；
(3) device for finally obtaining step (2) aging 5~7 days in 200~400 DEG C of air environments, to obtain base
In MoO3The triethylamine sensor of nano sensitive material.
Operation principle：
When based on MoO3When the triethylamine sensor of nano sensitive material is placed in air, the oxygen molecule in air is inhaled
It is attached on the sensor surface and by from MoO3The conduction band electron of nano sensitive material ionize with formed the oxonium ion of absorption with
O2-, O-Or O2-Mode exist.Since the concentration of free electron in conduction band is relatively low in air, so MoO3Sensor
Measurement resistance will increase.When sensor contacts Triethylamine gas under certain suitable temperature, oxygen species and object gas it
Between react, lead to capture the electronics in Ionized oxygen species and be released back into MoO3In nano sensitive material conduction band.It exhausts
Layer potential barrier reduces, and the conductance of sensor increases, to measure resistance reduction.Herein, we define the sensitivity S of sensor：S
=Ra/Rg, wherein RaFor the aerial resistance of sensor, RgFor the resistance after sensor contacts triethylamine.
Advantage of the present invention：
1. being prepared for the MoO of Nano grade using simple hydro-thermal method3Nano sensitive material has uniform size point
Cloth, synthetic method is simple, of low cost, and a kind of effective sensitive material is provided for exploitation high-performance triethylamine sensor.
2. the MoO that the present invention uses3Sensitive material is to triethylamine high sensitivity, and the sensor stability of exploitation is good, reliably
Property is strong.
3. the present invention make based on MoO3The triethylamine sensor manufacturing process of nano sensitive material is simple, preparation method
Step is easy, of low cost, small, is suitble to industrial batch production.
Description of the drawings
Fig. 1：It is of the present invention to be based on MoO3It the structural schematic diagram (1) of the triethylamine sensor of nano sensitive material and cuts open
View (2).
Fig. 2：The SEM of nano sensitive material prepared by the present invention schemes.(Fig. 2 a- Fig. 2 c are MoO prepared by the present invention3Material
The presoma MoO of material2High low power SEM figure；Fig. 2 d, 2e are the MoO prepared by the present invention3The low power SEM figures of sensitive material；Figure
2f is MoO3The high power SEM figures of sensitive material).
Fig. 3：The MoO of material prepared of the present invention3The TEM of nano sensitive material schemes, and HRTEM figures and SAED scheme (Fig. 3 a
For MoO prepared by the present invention3The presoma MoO of material2The TEM figures of single ball；Fig. 3 b are MoO prepared by the present invention3Material
TEM schemes；Fig. 3 c are MoO3The HRTEM of material schemes, and illustration is schemed for constituency SAED；Fig. 3 d- Fig. 3 f are prepared MoO3The member of material
Plain mapping graph).
Fig. 4：It is of the invention based on MoO under 275 DEG C of operating temperature3The triethylamine sensor of nano sensitive material 5~
(its illustration is the letter under 5~100ppm concentration to functional relation between 1000ppm triethylamine atmosphere medium sensitivities and gas concentration
Number relational graph).
Fig. 5：It is of the invention based on MoO under 275 DEG C of operating temperature38 kinds of the triethylamine sensor pair of nano sensitive material
Response comparison diagram of the gas under 100ppm concentration.
As shown in Figure 1, the names of the parts are：Al2O3Ceramics pipe outer 1, platinum line 2, annular gold electrode 3, nickel-cadmium coil
4, MoO3Nano sensitive material 5；
As shown in Fig. 2, presoma MoO2With the MoO prepared by the present invention3Scantling is than more uniform, each MoO2Nanometer
A diameter of 80~90nm of ball, single MoO3The length of nanometer sheet is 2~3 μm.Fig. 2 (c) and (f) are set forth one individually
MoO2Nanosphere and single MoO3Nanometer sheet.We can also be observed that MoO simultaneously2Nanosphere is by some nano particle groups
At, and MoO3Sensitive material is made of being accumulated by numerous nanometer sheets.
As shown in figure 3, sphere shows apparent comparison of light and shade and demonstrates MoO in Fig. 3 (a)2The solid knot of nanosphere
Structure.Fig. 3 (b) further demonstrates MoO3Sensitive material is really accumulated by the nanometer sheet of numerous size uniformities.Again to individual
One nanometer sheet has carried out HRTEM tests (Fig. 2 (c)), and can calculate the distance on a direction between adjacent crystal planes is
0.346nm corresponds to MoO3(JCPDS card number .35-609) (040) crystal face.The neat dot matrix of selective electron diffraction also discloses
These compositions MoO3The single crystal intrinsic of nano sensitive material.
As shown in figure 4, in the case where operating temperature is 275 DEG C, MoO3Triethylamine (5 of the base triethylamine sensor to various concentration
~1000ppm) sensitivity relation under atmosphere.With the raising of triethylamine concentration, sensitivity increases, obtains it is to be noted that sensor
When detecting triethylamine concentration and being 400ppm already close to saturation.
Fig. 5 is the MoO in the case where operating temperature is 275 DEG C38 kinds of gases of base triethylamine sensor pair are under 100ppm concentration
Response comparison diagram.It can be seen from the figure that MoO3Response of the base triethylamine sensor to the interference gas other than triethylamine
Respectively less than 5, but to the detection of triethylamine response up to 27.1, about the 6~27 of other gases times, show the sensor pair three
Ethamine has excellent selectivity.
Table 1：Based on MoO3The Triethylamine gas sensor of nano sensitive material is in 100ppm triethylamine atmosphere, sensitivity
With the data of operating temperature
| Senor operating temperature (DEG C) | Sensitivity (Ra/Rg) | |
| Embodiment 1 | 200 | 5.3 |
| Embodiment 2 | 225 | 6.4 |
| Embodiment 3 | 250 | 17.7 |
| Embodiment 4 | 275 | 27.1 |
| Embodiment 5 | 300 | 8.6 |
| Embodiment 6 | 325 | 5.3 |
Specific implementation mode
Embodiment 1
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 200 DEG C.
Embodiment 2
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 225 DEG C.
Embodiment 3
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 250 DEG C.
Embodiment 4
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 275 DEG C.
Embodiment 5
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 300 DEG C.
Embodiment 6
With MoO3Nanometer sheet makes heater-type triethylamine sensor, specific manufacturing process as sensitive material：
First by 0.087g (NH4)6Mo7O24·4H2O is dissolved in 30mL deionized waters.After stirring 20min, successively will
The dense HNO of 3mL PEG-400 and 3mL3(65%) it instills dropwise in above-mentioned solution, continues to stir 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 180
DEG C, for 24 hours；
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 is subjected to calcining 2h at 500 DEG C.
4. taking appropriate nano material obtained and ethyl alcohol 0.3mg in mass ratio:1mg is uniformly mixed to form slurry.Use hairbrush
It dips appropriate slurry and is coated in commercially available ceramic tube outer surface, make it that the gold electrode of outer surface be completely covered.MoO3The sensitive material of nanometer
The thickness of material is 20 μm, and (internal diameter of tubular ceramic substrate is 0.7mm, outer diameter 1.1mm, length 4.5mm；On its outer surface certainly
The cyclic annular gold electrode being mutually parallel with two, the single width of two electrodes are 0.4mm, spacing 0.5mm；It is drawn on gold electrode
Platinum filament wire length is 5mm).
5. coated ceramic tube is sintered 2h at 450 DEG C, then the ni-Cd heating coil that resistance value is 35 Ω is worn
Cross Al2O3Ceramic tube inside passes to direct current to provide operating temperature.Ceramic tube is welded on finally by platinum filament wire general
On heater-type hexagonal tube socket, to obtain MoO3Base oxide semiconductor triethylamine sensor.
6. finally by sensor in 300 DEG C of air environments aging 6 days, for use.
7. testing sensitivity of the sensor to 100ppm triethylamines at 325 DEG C.
Claims (5)
1. one kind being based on MoO3The triethylamine sensor of nano sensitive material, it is parallel, cyclic annular and divide each other with two by outer surface
The Al of vertical gold electrode2O3Ceramic tube substrate is coated in Al2O3Nano sensitive material on ceramic tube outer surface and gold electrode is set
In Al2O3Ni-Cd heating coil composition in ceramic tube, the platinum filament wire drawn on gold electrode；It is characterized in that：Nanometer is sensitive
Material is MoO3Nano sensitive material, and be prepared by following steps,
(1) first by 0.08g~0.09g (NH4)6Mo7O24·4H2O is dissolved in 20~40mL deionized waters, and stirring 15~
After 30min, then by the HNO of 3~5mL PEG-400 (polyethylene glycol) and 3~5mL, mass fraction 65%3It instills dropwise above-mentioned molten
In liquid, continue 15~30min of stirring；
(2) above-mentioned solution is encased in water heating kettle, is subsequently placed into baking oven, 20~25h is reacted at 170~190 DEG C；
(3) after reaction, obtained product water and ethyl alcohol are alternately subjected to centrifuge washing, then dried, it is dry after
1.5~3h of calcining is carried out at 450~550 DEG C, to obtain MoO3Nano sensitive material.
2. as described in claim 1 a kind of based on MoO3The triethylamine sensor of nano sensitive material, it is characterised in that：MoO3
The thickness of nano sensitive material is 15~30 μm.
3. as described in claim 1 a kind of based on MoO3The triethylamine sensor of nano sensitive material, it is characterised in that：Al2O3
The internal diameter of ceramic tube is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；The width of single gold electrode is 0.4
The spacing of~0.5mm, two gold electrodes are 0.5~0.6mm；The platinum filament wire drawn on gold electrode, the length of 4~6mm.
4. described in claim 1 a kind of based on MoO3The preparation method of the triethylamine sensor of nano sensitive material, step is such as
Under：
(1) MoO is taken3Nano sensitive material, with ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform is mixed to form slurry, with thin
Hairbrush dips the Al that slurry coating carries two gold electrodes parallel, cyclic annular and separate on the surface2O3Ceramic tube outer surface,
Make it that gold electrode be completely covered；
(2) coated ceramic tube is sintered to 1.5~3h at 350~450 DEG C, is then the ni-Cd of 30~40 Ω by resistance value
Heating coil passes through Al2O3Ceramic tube inside passes to direct current to provide suitable operating temperature for sensor, finally by platinum
Ceramic tube is welded on heater-type hexagonal tube socket by silk conducting wire；
(3) device for obtaining step (2) aging 5~7 days in 200~400 DEG C of air environments, to obtain being based on MoO3It receives
The triethylamine sensor of rice sensitive material.
5. described in claims 1 to 3 any one based on MoO3The triethylamine sensor of nano sensitive material is in complex environment
Detect the application in terms of Triethylamine gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810255079.0A CN108508062A (en) | 2018-03-27 | 2018-03-27 | One kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and applications |
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|---|---|---|---|
| CN201810255079.0A CN108508062A (en) | 2018-03-27 | 2018-03-27 | One kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and applications |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109470744A (en) * | 2018-11-09 | 2019-03-15 | 吉林大学 | One kind being based on MoO3/In2O3Acetone sensor, the preparation method and applications of composite sensitive material |
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| CN109594059A (en) * | 2018-10-31 | 2019-04-09 | 青岛大学 | A kind of atomic layer deposition preparation method of the heterogeneous sensitive thin film for triethylamine detection |
| CN109470744A (en) * | 2018-11-09 | 2019-03-15 | 吉林大学 | One kind being based on MoO3/In2O3Acetone sensor, the preparation method and applications of composite sensitive material |
| CN109470744B (en) * | 2018-11-09 | 2020-02-21 | 吉林大学 | Acetone sensor based on composite sensitive material, preparation method and application thereof |
| CN109884132A (en) * | 2019-03-01 | 2019-06-14 | 吉林大学 | MoO is adulterated based on bobbles shape Ni3The dimethylbenzene sensor of nano sensitive material, preparation method and applications |
| CN113125519A (en) * | 2021-04-19 | 2021-07-16 | 江南大学 | In2O3/α-Fe2O3Nanowire, triethylamine sensor and preparation method thereof |
| CN113125519B (en) * | 2021-04-19 | 2022-03-01 | 江南大学 | In2O3/α-Fe2O3Nanowire, triethylamine sensor and preparation method thereof |
| CN113671010A (en) * | 2021-08-18 | 2021-11-19 | 吉林大学 | In based on mesoporous2O3Triethylamine gas sensor of-NiO sensitive material and preparation method thereof |
| CN113671010B (en) * | 2021-08-18 | 2022-04-01 | 吉林大学 | In based on mesoporous2O3Triethylamine gas sensor of-NiO sensitive material and preparation method thereof |
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