CN109001264A - One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material - Google Patents
One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material Download PDFInfo
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- CN109001264A CN109001264A CN201810646930.2A CN201810646930A CN109001264A CN 109001264 A CN109001264 A CN 109001264A CN 201810646930 A CN201810646930 A CN 201810646930A CN 109001264 A CN109001264 A CN 109001264A
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- sensitive material
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- microballoon
- ufe
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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
One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material, belongs to conductor oxidate gas sensor technical field.Sensor is tubular structure, the Al of gold electrode parallel with two, cyclic annular and separate by outer surface2O3Ceramic tube substrate is coated in Al2O3Porous C uFe on ceramic tube outer surface and gold electrode2O4Microballoon sensitive material passes through Al2O3The nichrome heating coil of ceramic tube inside forms.The present invention prepares porous C uFe using one step hydro thermal method2O4Microballoon sensitive material, CuFe2O4The size of porous microsphere is 150~200nm.Sensor of the present invention has integrated level height, structure simple, cheap, small in size, is suitable for producing in enormous quantities.And the sensor with having faster response and good long-time stability, has broad application prospects to acetone in content of acetone context of detection.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical fields, and in particular to one kind is based on porous C uFe2O4It is micro-
The acetone gas sensor and preparation method thereof of ball sensitive material.
Background technique
Acetone is as a kind of common organic solvent, with colourless, transparent, active, inflammable, volatile and have pungent gas
The liquid of taste.Acetone Central nervous system has inhibition and anesthetic effect, can cause when VOC reaches a certain concentration in air
The symptoms such as headache, nauseous, out of strength even cause twitch, stupor, cause sternly to liver, kidney, brain and nervous system when serious
Grievous hurt simultaneously causes the serious consequences such as failure of memory.Acetone with other organic solvents equally meet open fire, high fever easily burn it is quick-fried
It is fried, and explosion limit is 2.55%~12.8%, therefore the detection of acetone gas is had a very important significance.
Conductor oxidate gas sensor is the resistor-type gas sensor using conductor oxidate as sensitive material, with
Other types of sensor is compared, and conductor oxidate type gas sensor has that high sensitivity, Monitoring lower-cut be low, response restores
Speed it is fast and it is at low cost a little, be one of current most widely used gas sensor.With nanometer science and technology
Development can greatly improve the specific surface area of material by the way that gas sensitive is regulated and controled formation of nanostructured, it is living to increase surface
Property site, improves the gas-sensitive property of material.
CuFe2O4It is a kind of conductor oxidate with inverse spinel structure, is readily synthesized that there is low toxicity and height
Thermal stability be considered to have one of sensitive material of development potentiality.In addition, CuFe2O4Also show excellent catalytic
Can, magnetic and electronic conductivity energy, however CuFe2O4The report that material is applied to gas sensor is considerably less.Thus it is necessary to
Develop a kind of simple method preparation CuFe2O4Sensitive material simultaneously regulates and controls its micro-nano structure, obtains high performance gas sensor.
Summary of the invention
The object of the present invention is to provide one kind to be based on porous C uFe2O4The acetone gas sensor of microballoon sensitive material and its
Preparation method.
The present invention is with porous C uFe2O4Microballoon is as sensitive material, one side CuFe2O4As semiconductor oxide materials
Have the characteristics that nontoxic, resourceful；On the other hand, porous C uFe2O4Microballoon has graded structure, has relatively large
Specific surface area, it is loose porous, it can be improved the reaction efficiency of under test gas Yu sensitive material surface, to further increase material
Sensitivity.
It is of the present invention a kind of based on porous C uFe2O4The acetone gas sensor of microballoon sensitive material is tubular structure,
The Al of Au electrode parallel with two, cyclic annular and separate by outer surface2O3Ceramic tube substrate is coated in Al2O3Ceramic tube
Conductor oxidate sensitive material on outer surface and gold electrode passes through Al2O3The nichrome heating coil group of ceramic tube inside
At, it is characterised in that: conductor oxidate sensitive material is porous C uFe2O4Microballoon sensitive material, and it is as follows by following steps
It is prepared:
(1) by 3~5mmol CuCl2·2H2O and 6~10mmol FeCl3·6H2O is dissolved in the ratio of molar ratio 1:2
In 60~80mL ethylene glycol solution, 10~20min of magnetic agitation；
(2) by the sodium acetate ((CH of 1.5~1.7g3COONa)·3H2O) powder is added in the solution that step (1) obtains,
Continue 15~20min of magnetic agitation；
(3) 0.9~1.1g dodecyl trimethyl ammonium bromide is added in the solution of step (2), continues magnetic agitation
15~20min；
(4) solution for obtaining step (3) 10~14h of isothermal reaction at 180~200 DEG C, then naturally cools to room
Temperature is dried in vacuo after washing 3~5 times respectively with deionized water and ethyl alcohol in 70~90 DEG C；
(5) material for obtaining step (4) obtains porous C uFe in 350~450 DEG C of 1~2h of calcining2O4Microballoon sensitivity material
Feed powder end.
One kind being based on porous C uFe2O4The preparation method of the acetone gas sensor of microballoon sensitive material, sensor are indirect heat
Formula structure, preparation step are as follows:
By porous C uFe2O4The mixing of the ratio of microballoon sensitive material powder and deionized water 1~3:1 in mass ratio, and grind
At pasty slurry, then dipping a small amount of slurry with hairbrush, to be uniformly coated on outer surface parallel with two, cyclic annular and divide each other
The Al of vertical gold electrode2O3Ceramic pipe surface, forms the sensitive material film of 100~200 μ m-thicks, and covers sensitive material completely
Bezel ring, shape gold electrode；A length of 4~4.5mm of ceramic tube, outer diameter are 1.2~1.5mm, and internal diameter is 0.8~1.0mm；Annular gold electricity
The width of pole is 0.7~0.9mm, and the spacing of two electrodes is 1.7~1.9mm；Then it is toasted 30~45 minutes under infrared lamp,
After sensitive material is dry, Al2O3Ceramic tube is calcined 2~3 hours at 400~450 DEG C；It then is 30~40 by resistance value
The nichrome heating coil of Ω passes through Al2O3Ceramic tube inside is finally welded according to heater-type gas sensor as heater strip
It connects and encapsulates, to obtain based on porous C uFe2O4The acetone gas sensor of microballoon sensitive material.
The present invention has the advantages that
(1) porous C uFe is prepared using a step solvent thermal process2O4Microballoon sensitive material powder, material obtained are
The graded structure porous C uFe being made of nano particle2O4Microballoon, pattern are unique, uniform；
(2) the porous C uFe prepared by2O4Microballoon sensitive material has excellent gas-sensitive property to acetone, including high spirit
Sensitivity and selectivity, quickly respond recovery characteristics；
(3) present invention make based on porous C uFe2O4Microballoon sensitive material acetone gas sensor manufacture craft is simple,
It is low in cost, it is small in size, it is suitble to industrial batch production.
Detailed description of the invention
Fig. 1 (a-c) is the porous C uFe of preparation of the embodiment of the present invention2O4The SEM of microballoon sensitive material schemes.Wherein (a) figure
Enlargement ratio is 80000, and (b) enlargement ratio of figure is 200000 times, and (c) enlargement ratio of figure is 300000 times；
Fig. 2 is of the present invention based on porous C uFe2O4The structural representation of the acetone gas sensor of microballoon sensitive material
Figure；
Fig. 3 is that the sensor of embodiment preparation is bent to the response (sensitivity) of 100ppm acetone at a temperature of different operating
Line；
Fig. 4 is choosing of the sensor of embodiment preparation at 250 DEG C to 100ppm acetone, ethyl alcohol, methanol, formaldehyde, toluene
Selecting property column diagram.
Fig. 5 is for embodiment to the transient response curve of various concentration acetone gas under optimum working temperature.
As shown in Figure 1, it can be seen that prepared CuFe from figure a and b2O4Material is in spherical and well dispersed, shape
It is uniform.It can be seen that CuFe from figure c2O4Microballoon is made of the nano particle of 10~15nm, be in porous structure, ball it is straight
Diameter is about 150~200nm；
As shown in Fig. 2, the names of the parts are Al2O3Ceramic tube 1, semiconductor sensitive material 2, nichrome heating coil 3,
Annular gold electrode 4, platinum filament pin 5；
As shown in figure 3, for embodiment in the present invention to the response curve of 100ppm acetone at a temperature of different operating.It can be with
The optimum working temperature for seeing embodiment is 250 DEG C, at this time the sensitivity of device most preferably 20.6.
As shown in figure 4, for comparative example of the present invention and embodiment at 250 DEG C of optimum working temperature to 100ppm not
With the selective column diagram of gas, it can be seen that embodiment embodies preferably selective to acetone.
As shown in figure 5, bent to the response of various concentration acetone under optimum working temperature for embodiment of the present invention
Line, it can be seen that with the increase of acetone concentration, the response for implementing ratio sensor is gradually increased, Monitoring lower-cut 1ppm.
Specific embodiment
Embodiment 1:
1. by 3mmol CuCl2·2H2O and 6mmol FeCl3·6H2O is dissolved in 70mL second two with the ratio of molar ratio 1:2
In alcoholic solution, magnetic agitation 15min；
2. by the sodium acetate ((CH of 1.6g3COONa)·3H2O it) is added in the solution that step (1) obtains, continues magnetic force and stir
Mix 15min；
3. 1.0g dodecyl trimethyl ammonium bromide is added in the solution of step (2), continue magnetic agitation 15min；
4. the solution that step (3) is obtained isothermal reaction 12h at 200 DEG C, then cooled to room temperature, uses deionization
Water and ethyl alcohol are dried in vacuo after washing 3 times respectively in 80 DEG C；
5. the material that step (3) is obtained obtains porous C uFe in 400 DEG C of calcining 2h2O4Microballoon sensitive material powder produces
Amount of substance is about 300mg；
6. by sensitive material porous C uFe2O4Microballoon sensitive material powder is mixed and is ground according to mass ratio 3:1 with deionized water
Wear into pasty slurry, then with hairbrush by above-mentioned slurry be uniformly coated in commercially available outer surface it is parallel with two, it is cyclic annular and
The Al of gold electrode separate2O3Ceramic pipe surface, forms the sensitive material film of 100 μm of left and right thicknesses, and makes sensitive material
Cover all annular gold electrode, wherein the length of ceramic tube is 4mm, outer diameter 1.2mm, internal diameter 0.8mm, two annulars
The width of gold electrode is 0.8mm, and the spacing of two electrodes is 1.8mm.Two platinum filaments are respectively connected on each electrode as pin,
The length of platinum filament is about 9mm；
7. the alumina ceramic tube for being coated with sensitive material is toasted 30min under infrared lamp, it is completely dried to sensitive material
Afterwards, alumina ceramic tube is put into Muffle furnace at 400 DEG C and calcines 2h, be then 30 Ω or so, the number of turns by a resistance value
Nichrome heating coil for 40 circles is pierced by from ceramic tube inside as heater strip, finally by above-mentioned device according to heater-type gas
Quick element is welded and is encapsulated, and is obtained based on porous C uFe2O4The acetone gas sensor of microballoon sensitive material.
Claims (3)
1. one kind is based on porous C uFe2O4The acetone gas sensor of microballoon sensitive material has two parallel, rings by outer surface
The Al of shape and Au electrode separate2O3Ceramic tube substrate is coated in Al2O3Partly leading on ceramic tube outer surface and Au electrode
Oxide body sensitive material is placed in Al2O3Nichrome coil composition in ceramic tube；It is characterized by: conductor oxidate is quick
Sense material is porous C uFe2O4Microballoon sensitive material, and it is prepared by following steps,
(1) by 3~5mmol CuCl2·2H2O and 6~10mmol FeCl3·6H2O is dissolved in 60 with the ratio of molar ratio 1:2~
In 80mL ethylene glycol solution, 10~20min of magnetic agitation；
(2) sodium acetate of 1.5~1.7g is added in the solution that step (1) obtains, continues 15~20min of magnetic agitation；
(3) 0.9~1.1g dodecyl trimethyl ammonium bromide is added in the solution of step (2), continuation magnetic agitation 15~
20min；
(4) solution for obtaining step (3) 10~14h of isothermal reaction at 180~200 DEG C, then cooled to room temperature, is used
Deionized water and ethyl alcohol are dried in vacuo after washing 3~5 times respectively in 70~90 DEG C；
(5) material for obtaining step (4) obtains porous C uFe in 350~450 DEG C of 1~2h of calcining2O4Microballoon sensitive material powder
End.
2. described in claim 1 a kind of based on porous C uFe2O4The preparation side of the acetone gas sensor of microballoon sensitive material
Method, its step are as follows:
(1) by porous C uFe2O4Microballoon sensitive material powder and deionized water are mixed with the ratio of 1~3:1 of mass ratio, and are ground
At pasty slurry, then with brush dip a small amount of slurry be uniformly coated on commercially available outer surface it is parallel with two, it is cyclic annular and
The Al of gold electrode separate2O3Ceramic pipe surface, forms the sensitive material film of 100~200 μ m-thicks, and makes sensitive material
Annular gold electrode is completely covered；
(2) it is toasted 30~45 minutes under infrared lamp, after sensitive material is dry, Al2O3Ceramic tube is forged at 400~450 DEG C
It burns 2~3 hours；Then the nichrome heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside is as heating
Silk, is finally welded and is encapsulated according to heater-type gas sensor, to obtain based on porous C uFe2O4Microballoon sensitive material
Acetone gas sensor.
3. as claimed in claim 2 a kind of based on porous C uFe2O4The preparation side of the acetone gas sensor of microballoon sensitive material
Method, it is characterised in that: Al2O3A length of 4~4.5mm of ceramic tube, outer diameter are 1.2~1.5mm, and internal diameter is 0.8~1.0mm；Annular
The width of gold electrode is 0.7~0.9mm, and the spacing of two electrodes is 1.7~1.9mm.
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| CN110006977A (en) * | 2019-05-15 | 2019-07-12 | 北京理工大学 | A kind of CuFe2O4The preparation of nanosphere electrochemical sensor and detection method to lysozyme |
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| CN112255279A (en) * | 2020-09-29 | 2021-01-22 | 沈阳化工大学 | Flower-shaped V2O5Preparation of microsphere and application of microsphere in acetone gas sensor |
| CN113514506A (en) * | 2021-07-13 | 2021-10-19 | 吉林大学 | Based on porous LaFeO3Acetone gas sensor of microsphere nano sensitive material and preparation method thereof |
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