CN106896142A - Acetone sensor, the preparation method and applications of the Ce doped In_2O_3 nano sensitive materials based on graded structure - Google Patents
Acetone sensor, the preparation method and applications of the Ce doped In_2O_3 nano sensitive materials based on graded structure Download PDFInfo
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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 Ce doping In based on graded structure2O3The acetone sensor of nano sensitive material, preparation method and its application in terms of acetone steam is detected in environment indoors, belong to conductor oxidate gas sensor technical field.The Al with two parallel, ring-types and gold electrode separate by outer surface2O3Earthenware substrate, it is coated in Al2O3Nano sensitive material on ceramic tube outer surface and gold electrode, it is placed in Al2O3NI-G heating coil composition in earthenware.By in graduate In2O3Piece takes doping Ce elements, improves the sensitivity to acetone, and the Monitoring lower-cut of material is relatively low, and with quickly response resume speed and good repeatability, has broad application prospects in terms of detection level；Simple, with low cost, the small volume with synthetic method, is suitable to the good characteristics produced in enormous quantities.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical field, and in particular to a kind of based on graded structure
Ce doping In2O3The acetone sensor of nano sensitive material, preparation method and its in terms of detecting acetone steam in environment indoors
Using.
Background technology
Harm of the acetone gas to human body is mainly shown as the anesthetic effect of Central nervous system, and acute poisoning may occur in which weary
It is power, nausea, headache, dizziness, emotional.There is vomiting, out of breath, spasm, or even stupor in severe one.It is irritant to eye, nose, larynx.
Sensor, by the forward position in Information Technology Development, can widely be paid close attention to and be commercialized and be answered as the means of the information of acquisition
With.Although having been obtained for very big progress in the research of oxide semiconductor gas sensor, in order to meet its
The use requirement of each detection field, still needs to further improve the sensitivity of sensor, selectivity and reduces operating temperature.
In fact, deepen constantly always around the research for improving oxide-semiconductor sensor sensitivity, especially
It is that developing into for nanoscale science and technology improves sensor performance there is provided good opportunity.Research shows, the identification of gas sensitive
Function, translation function and sensitive body utilization rate decide the sensitivity of oxide-semiconductor sensor.It is found that by different
The semiconductor oxide composite of matter dopant doping can significantly improve sensitivity and the selectivity of sensor.This is main
Because doping dissimilar metal ion can improve the carrier mobility of sensing material, so as to improve its " translation function ",
Secondly, some dissimilar metal dopants can make generation anti-in the corresponding redox in conductor oxidate surface as catalyst
Should be catalyzed, the selectivity of sensor can be improved, be improved " identification function " of sensing material.Based on this point, carry out different
The design and preparation of the metal-doped oxide semiconductor of matter, have highly important section for the application of enlargement gas sensor
Learn meaning.
The content of the invention
It is an object of the invention to provide a kind of Ce doping In based on graded structure2O3The acetone of nano sensitive material is passed
Sensor, preparation method and its application in environment in terms of detection acetone steam indoors.The present invention enters by semi-conducting material
Row doping, increases the sensitivity of sensor, improves the response speed of sensor, improves the repeatability of sensor, promotes this kind of biography
Sensor is in the practical of field of gas detection.
Sensor obtained by the present invention except with it is higher it is sensitive be outside one's consideration, and with preferable selectivity, repeatability
And long-time stability.The Monitoring lower-cut of the sensor is 1ppm, can be used for the detection of acetone steam content in indoor environment.This hair
Bright used commercially available tubular structure sensor, manufacture craft is simple, small volume, beneficial to industrial batch production, therefore tool
There is important application value.
Ce doping In based on graded structure of the present invention2O3Acetone sensor, by outer surface with two put down
The Al of row, ring-type and gold electrode separate2O3Earthenware substrate, it is coated in Al2O3On ceramic tube outer surface and gold electrode
Nano sensitive material, it is placed in Al2O3NI-G heating coil composition in earthenware；It is characterized in that：Nano sensitive material is mixed for Ce
Miscellaneous In2O3, and prepared by following steps：
(1) by the InCl of 0.12~0.16g3·4H2Ce (the NO of O, 2~9.8mg3)3·6H2O, 0.8~1.2g urea and
The SDS (dodecyl sodium sulfate) of 0.1~0.15g is dissolved in the mixed solvent of 10mL ethanol and 30mL water, is sufficiently stirred for 30
~60min；
(2) by above-mentioned solution under the conditions of 150~170 DEG C 2~5h of hydro-thermal reaction；
(3) after reaction terminates, the product that will be obtained is cooled to room temperature, then with water and ethanol alternately centrifuge washing,
The product that will be obtained is dried, and 1~3h is finally calcined at 450~550 DEG C, so as to obtain Ce doping In2O3The sensitive material of nanometer
Material.
Involved sensor uses heater-type structure in the present invention, and concrete technology is as follows：
(1) Ce doping In is taken2O3Nano sensitive material, with ethanol in mass ratio 0.25~0.5：1 ratio uniform mixing shape
Into slurry；Slurry is dipped with hairbrush be coated on surface the Al with two parallel, ring-types and gold electrode separate2O3Ceramics
Tube outer surface, makes it be completely covered on Al2O3On ceramic tube outer surface and gold electrode；The thickness of nano sensitive material be 15~
30um；Al2O3The internal diameter of earthenware is 0.6~0.8mm, and external diameter is 1.0~1.5mm, and length is 4~5mm；Single gold electrode
Width is 0.4~0.5mm, and two spacing of gold electrode are 0.5~0.6mm；The platinum filament wire drawn on gold electrode, its length is
4~6mm；
(2) Al of nano sensitive material will have been coated2O3Earthenware sinters 1~3h at 350~450 DEG C, then by resistance
It is worth for the NI-G heating coil (number of turn is 50~60 circles) of 30~40 Ω passes through Al2O3Ceramic tube inside, passes to direct current and comes to pass
Sensor provides suitable operating temperature；The device that will finally prepare is welded on general heater-type hexagonal base；
(3) by above-mentioned device aging 5~7 days in 200~400 DEG C of air ambients, so as to obtain based on graded structure
Ce doping In2O3The acetone sensor of nano sensitive material.
Operation principle：
As Ce doping In2O3Acetone sensor is placed in when in air, and 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
During lower contact acetone gas, acetone gas molecule will be adsorbed in sensor surface, and release trapped electron returns to In2O3Conduction band, so that
Make In2O3Resistance declines.The sensitivity that we define sensor herein is S：S=Ra/Rg, wherein RaFor between sensor gold electrode
Resistance in air, RgTo contact the resistance after acetone between sensor gold electrode.
Ce based on graded structure doping In prepared by the present invention2O3Acetone sensor there is advantages below：
1. the composite construction of graduation nano material can be prepared using simple hydro-thermal method, and synthetic method is simple, cost
It is cheap；
2. by graduate In2O3Piece takes doping Ce elements, improves the sensitivity to acetone, the detection of material
Lower limit is relatively low, and with quickly response resume speed and good repeatability, has wide application preceding in terms of detection level
Scape；
3. commercially available tubular type sensor is used, device technology is simple, small volume, be suitable to produce in enormous quantities.
Brief description of the drawings
Fig. 1：Ce doping In2O3The structural representation of acetone sensor；Fig. 1 (a) is sectional view, and Fig. 1 (b) is welded condition
Schematic diagram；
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 in 250 DEG C of 8 kinds of comparison diagrams of the response of gas with various to 200ppm.
Fig. 4：The response and work temperature of comparative example, embodiment 1, embodiment 2 and embodiment 3 to 100ppm acetone gas
The relation curve of degree.
Fig. 5：Comparative example and embodiment 2 under optimum working temperature, to the response of various concentrations acetone gas.
As shown in figure 1, each component names are：Annular gold electrode 1, In2O3Nano sensitive material 2, Al2O3Ceramics pipe outer
3rd, nichrome heating coil 4, platinum filament pin 5；
Fig. 2 is the stereoscan photograph of the sample of comparative example, embodiment 1, embodiment 2 and embodiment 3.Can from figure
Go out, gained sample is graded structure (the graduation three-dimensional manometer assembled as construction unit by low-dimensional nano structure
Structure) bouquet.Also, as the increase of doping, the nanoparticle size for constituting bouquet are gradually reduced, illustrate the incorporation of Ce
Inhibit In2O3The growth of crystal grain.
Fig. 3 is comparative example and embodiment 2 in 250 DEG C of 8 kinds of comparison diagrams of the response of gas with various to 100ppm.From figure
In as can be seen that embodiment compared to comparative example, the response to most of gas all has a certain upgrade.
Fig. 4 is the response and work of comparative example, embodiment 1, embodiment 2 and embodiment 3 to 100ppm acetone gas
The relation curve of temperature.It can be seen that the optimum working temperature of four groups of samples is 250 DEG C.Wherein, the spirit of comparative example
Sensitivity is 6.3, and the sensitivity of embodiment 1 is 17.8, and the sensitivity of embodiment 2 is 27.5, and the sensitivity of embodiment 3 is 22.6.
Under optimum working temperature, the sensitivity highest of embodiment 2, about the 4.4 of comparative example sensitivity times.As can be seen here, by mixing
Entering Ce ions can improve the reaction efficiency of sensitive material and acetone, and then obtain one with highly sensitive Ce doping
In2O3Oxide semiconductor acetone sensor.
Fig. 5 be comparative example and embodiment 2 under optimum working temperature, to the response curve of various concentrations acetone gas.Spirit
Sensitivity method of testing：Sensor is put into gas cabinet first, now resistance is measured by the ammeter being connected with sensor, obtained
The aerial resistance value of sensor is Ra；Then led to the acetone that 1~100ppm is injected in gas cabinet using microsyringe
Cross measurement and obtain the i.e. R of resistance value of the sensor in various concentrations acetoneg, the defined formula S=R according to sensitivity Sa/Rg, lead to
The sensitivity for being calculated various concentrations lower sensor is crossed, the standard working curve of acetone concentration-sensitivity is finally given.From
As can be seen that the Monitoring lower-cut of the sensor of embodiment 2 is 1ppm in figure, sensitivity now is 1.2；When acetone concentration is
During 200ppm, the now sensitivity of comparative example and embodiment 2 is respectively 14.4 and 41.8, and response tends to saturation.
R can be measured by above-mentioned method during actual measurementa、Rg, obtain the mark with acetone concentration-sensitivity after Sensitirity va1ue
Quasi- working curve is contrasted, and so as to obtain the content of acetone in environment, this feature enables this kind of acetone sensor fine
The detection that can be applied to acetone gas in indoor environment.
Specific embodiment
Comparative example：
With In2O3Bouquet makes heater-type acetone sensor, its specific manufacturing process as sensitive material：
1. first by the InCl of 0.13g3·4H2The SDS (dodecyl sodium sulfate) of O, 1g urea and 0.13g is dissolved in mixed
(ethanol in bonding solvent：Water=10mL:30mL), it is sufficiently stirred for 60min：
2. above-mentioned solution is encased in 50mL water heating kettles, be subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 3h；
3. after reaction terminates, the product that will be obtained alternately carries out centrifuge washing with water and ethanol.Centrifuge parameters are set to
10000r/min, 10min.Product is dried after centrifugation.After drying terminates, product is carried out into calcining 2h at 500 DEG C, obtained
In2O3Nano material.
4. appropriate obtained In is taken2O3Nano material and ethanol 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, makes its gold electrode (tubular ceramic lining that outer surface is completely covered
The internal diameter at bottom is 0.7mm, and external diameter is 1.1mm, and length is 4.5mm；Two ring-type gold being parallel to each other are come with its outer surface
Electrode, the single width of two electrodes is 0.4mm, and spacing is 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated earthenware is sintered into 2h at 400 DEG C, 35 Ω NI-Gs heating coils are then passed through into Al2O3Ceramics
Inside pipe, pass to direct current to provide operating temperature.Earthenware is welded on general heater-type hexagonal finally by platinum filament wire
On base, so as to obtain In2O3Acetone sensor.
6. finally by sensor aging 6 days in 250 DEG C of air ambients, so as to obtain In2O3The acetone of nano sensitive material
Sensor.
Embodiment 1：
Mol ratio with Ce ions/In ions is 0.01：1 Ce doping In2O3Oxide semiconductor is used as sensitive material system
Make acetone sensor, its manufacturing process is
1. first by the InCl of 0.13g3·4H2Ce (the NO of O, 2mg3)3·6H2The SDS (12 of O, 1g urea and 0.13g
Sodium alkyl sulfonate) it is dissolved in (ethanol in mixed solvent：Water=10mL:30mL), it is sufficiently stirred for 60min；
2. above-mentioned solution is encased in 50mL water heating kettles, be subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 3h；
3. after reaction terminates, the product that will be obtained alternately carries out centrifuge washing with water and ethanol.Centrifuge parameters are set to
10000r/min, 10min.Product is dried after centrifugation.After drying terminates, product is carried out into calcining 2h at 500 DEG C, obtained
Ce doping In2O3Nano material；
4. appropriate obtained Ce doping In is taken2O3Nano material and ethanol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry
Material.Appropriate slurry is dipped with hairbrush and be coated in commercially available ceramic tube outer surface, make its gold electrode (tubulose pottery that outer surface is completely covered
The internal diameter at ceramic liner bottom is 0.7mm, and external diameter is 1.1mm, and length is 4.5mm；Two rings being parallel to each other are come with its outer surface
Shape gold electrode, the single width of two electrodes is 0.4mm, and spacing is 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated earthenware is sintered into 2h at 400 DEG C, 35 Ω NI-Gs heating coils are then passed through into Al2O3Ceramics
Inside pipe, pass to direct current to provide operating temperature.Earthenware is welded on general heater-type hexagonal finally by platinum filament wire
It is 0.01 so as to obtain mol ratio on base:1Ce doping In2O3Acetone sensor.
6., finally by sensor aging 6 days in 250 DEG C of air ambients, adulterated so as to obtain the Ce based on graded structure
In2O3The acetone sensor of nano sensitive material.
Embodiment 2：
Mol ratio with Ce ions/In ions is 0.03：1 Ce doping In2O3Oxide semiconductor is used as sensitive material system
Make acetone sensor, its manufacturing process is
1. first by the InCl of 0.13g3·4H2Ce (the NO of O, 5.9mg3)3·6H2The SDS (ten of O, 1g urea and 0.13g
Dialkyl sulfonates) it is dissolved in (ethanol in mixed solvent：Water=10mL:30mL), it is sufficiently stirred for 60min；
2. above-mentioned solution is encased in 50mL water heating kettles, be subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 3h；
3. after reaction terminates, the product that will be obtained alternately carries out centrifuge washing with water and ethanol.Centrifuge parameters are set to
10000r/min, 10min.Product is dried after centrifugation.After drying terminates, product is carried out into calcining 2h at 500 DEG C.
4. appropriate obtained nano material and ethanol 0.4mg in mass ratio are taken:1mg is uniformly mixed to form slurry.Use hairbrush
Dip appropriate slurry and be coated in commercially available ceramic tube outer surface, the gold electrode for making it that outer surface is completely covered.(tubular ceramic substrate
Internal diameter is 0.7mm, and external diameter is 1.1mm, and length is 4.5mm；Two ring-type gold electrodes being parallel to each other are come with its outer surface,
The single width of two electrodes is 0.4mm, and spacing is 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm.)
5. coated earthenware is sintered into 2h at 400 DEG C, 35 Ω NI-Gs heating coils are then passed through into Al2O3Ceramics
Inside pipe, pass to direct current to provide operating temperature.Earthenware is welded on general heater-type hexagonal finally by platinum filament wire
It is 0.03 so as to obtain mol ratio on base:1Ce doping In2O3Acetone sensor.
6., finally by sensor aging 6 days in 250 DEG C of air ambients, adulterated so as to obtain the Ce based on graded structure
In2O3The acetone sensor of nano sensitive material.
Embodiment 3：
Mol ratio with Ce ions/In ions is 0.05：1 Ce doping In2O3Oxide semiconductor is used as sensitive material system
Make acetone sensor, its manufacturing process is
1. first by the InCl of 0.13g3·4H2Ce (the NO of O, 9.8mg3)3·6H2The SDS (ten of O, 1g urea and 0.13g
Dialkyl sulfonates) it is dissolved in (ethanol in mixed solvent：Water=10mL:30mL), it is sufficiently stirred for 60min；
2. above-mentioned solution is encased in 50mL water heating kettles, be subsequently placed into hydro-thermal baking oven, baking oven parameter setting is 160
DEG C, 3h；
3. after reaction terminates, the product that will be obtained alternately carries out centrifuge washing with water and ethanol.Centrifuge parameters are set to
10000r/min, 10min.Product is dried after centrifugation.After drying terminates, product is carried out into calcining 2h at 500 DEG C.
4. appropriate obtained nano material and ethanol 0.4mg in mass ratio are taken:1mg is uniformly mixed to form slurry.Use hairbrush
Dip appropriate slurry and be coated in commercially available ceramic tube outer surface, make gold electrode that it is completely covered outer surface (tubular ceramic substrate
Internal diameter is 0.7mm, and external diameter is 1.1mm, and length is 4.5mm；Two ring-type gold electrodes being parallel to each other are come with its outer surface,
The single width of two electrodes is 0.4mm, and spacing is 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated earthenware is sintered into 2h at 400 DEG C, 35 Ω NI-Gs heating coils are then passed through into Al2O3Ceramics
Inside pipe, pass to direct current to provide operating temperature.Earthenware is welded on general heater-type hexagonal finally by platinum filament wire
It is 0.05 so as to obtain mol ratio on base:1Ce doping In2O3Acetone sensor.
6., finally by sensor aging 6 days in 250 DEG C of air ambients, adulterated so as to obtain the Ce based on graded structure
In2O3The acetone sensor of nano sensitive material.
Claims (5)
1. it is a kind of based on graded structure Ce doping In2O3The acetone sensor of nano sensitive material, two are carried by outer surface
The Al of parallel, ring-type and gold electrode separate2O3Earthenware substrate, it is coated in Al2O3On ceramic tube outer surface and gold electrode
Nano sensitive material, be placed in Al2O3NI-G heating coil composition in earthenware, the platinum filament wire drawn on gold electrode；Its
It is characterised by：Nano sensitive material is Ce doping In2O3, and prepared by following steps,
(1) by the InCl of 0.12~0.16g3·4H2Ce (the NO of O, 2~9.8mg3)3·6H2O, 0.8~1.2g urea and 0.1~
0.15g dodecyl sodium sulfates are dissolved in the mixed solvent of 10mL ethanol and 30mL water, are sufficiently stirred for 30~60min；
(2) above-mentioned solution is existedUnder the conditions of 2~5h of hydro-thermal reaction；
(3) after reaction terminates, the product that will be obtained is cooled to room temperature, then with water and ethanol alternately centrifuge washing, will
To product be dried, finally at 450~550 DEG C calcine 1~3h, so as to obtain Ce doping In2O3Nano sensitive material.
2. a kind of Ce doping In based on graded structure as claimed in claim 12O3The acetone sensing of nano sensitive material
Device, it is characterised in that：The thickness of nano sensitive material is 15~30um.
3. a kind of Ce doping In based on graded structure as claimed in claim 12O3The acetone sensing of nano sensitive material
Device, it is characterised in that：Al2O3The internal diameter of earthenware is 0.6~0.8mm, and external diameter is 1.0~1.5mm, and length is 4~5mm；It is single
The width of gold electrode is 0.4~0.5mm, and two spacing of gold electrode are 0.5~0.6mm；The platinum filament wire drawn on gold electrode,
Its length is 4~6mm.
4. described in claims 1 to 3 any one based on graded structure Ce doping In2O3The acetone of nano sensitive material
The preparation method of sensor, its step is as follows：
(1) Ce doping In is taken2O3Nano sensitive material, with ethanol in mass ratio 0.25~0.5：1 ratio uniform is mixed to form slurry
Material；Slurry is dipped with hairbrush be coated on surface the Al with two parallel, ring-types and gold electrode separate2O3Outside earthenware
Surface, makes it be completely covered on Al2O3On ceramic tube outer surface and gold electrode；
(2) Al of nano sensitive material will have been coated2O3Earthenware sinters 1~3h at 350~450 DEG C, is then by resistance value
The NI-G heating coil of 30~40 Ω passes through Al2O3Ceramic tube inside, passes to direct current to provide suitable work temperature for sensor
Degree；The device that will finally prepare is welded on general heater-type hexagonal base；
(3) by above-mentioned device aging 5~7 days in 200~400 DEG C of air ambients, so as to obtain the Ce based on graded structure
Doping In2O3The acetone sensor of nano sensitive material.
5. described in claims 1 to 3 any one based on graded structure Ce doping In2O3The acetone of nano sensitive material
Sensor detects the application in terms of acetone steam in environment indoors.
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| CN113219010A (en) * | 2021-05-19 | 2021-08-06 | 吉林大学 | Ethanol sensor of ZnO double-shell hollow structure microsphere sensitive material and preparation |
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