CN108828017A - A kind of gas sensor and preparation method thereof towards acetone gas detection - Google Patents
A kind of gas sensor and preparation method thereof towards acetone gas detection Download PDFInfo
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- CN108828017A CN108828017A CN201810227320.9A CN201810227320A CN108828017A CN 108828017 A CN108828017 A CN 108828017A CN 201810227320 A CN201810227320 A CN 201810227320A CN 108828017 A CN108828017 A CN 108828017A
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000001514 detection method Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010931 gold Substances 0.000 claims abstract description 5
- 229910052737 gold Inorganic materials 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 16
- 239000003960 organic solvent Substances 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000002070 nanowire Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000004005 microsphere Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002127 nanobelt Substances 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 239000002071 nanotube Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims 1
- 238000010422 painting Methods 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 16
- 206010012601 diabetes mellitus Diseases 0.000 abstract description 7
- 238000012544 monitoring process Methods 0.000 abstract description 5
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 56
- 239000012528 membrane Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 230000036541 health Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000007970 homogeneous dispersion Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of gas sensors and preparation method thereof towards acetone gas detection, which utilizes the Fe of nanotopography structure from the interaction of material and object gas2O3Material is as gas sensitive material, it is deposited in the ceramic pipe surface for studding with gold electrode by the method for spin coating, it is assembled into a gas sensor, improve its response performance to acetone gas by optimizing sensitive thicknesses of layers, obtained gas sensor has good response to acetone gas, and detectable actual concentrations are down to 1 ppm.Meanwhile the ability that the sensor also resists other organic gas to interfere, there is preferable selective response to acetone gas, can be used as a kind of tool for clinically monitoring diabetes patient's state of an illness in real time.
Description
Technical field
The invention belongs to oxide gas sensor technical fields, and in particular to a kind of gas towards acetone gas detection
Sensor and preparation method thereof.
Background technique
Studies have shown that the content of acetone in diabetes patient's exhaled gas is up to 1.8 ppm, therefore for the height of acetone gas
Sensitivity selective enumeration method has great importance in terms of the health monitoring of diabetic.It is with metal oxide semiconductor
The gas sensor on basis has been widely used in industry, environment due to the advantages that its is small in size, low energy consumption, stability is good
The multiple fields such as monitoring, food inspection.However due to the limitation of gas sensing mechanism, most metals oxide gas sensor is almost
There is response to multiple gases, in the case where detecting mixed gas or with the presence of interference gas etc., is difficult effectively to identify and examine
Measure target components.
The key for developing high performance sensor is to develop the sensitive material of highly selective high sensitivity.According to correlation
Literature survey discovery, acetone molecules can be in Fe2O3Catalytic oxidation occurs for material surface, and can pass through crystal face, hole
Regulations are waited to promote the single-minded selective degree of catalysis reaction.Therefore it is expected to the Fe prepared with this2O3Material comes as sensitive body
Gas sensor is prepared, to realize the efficient detection to acetone gas in expiration.
Nevertheless, the performance of sensor is also greatly limited by preparation process, the ginseng such as thickness of especially sensitive film layer
Number.Therefore, obtain be suitble to thickness, equally distributed sensitive membrane for improving performance be very it is necessary to.
Summary of the invention
The object of the invention is that in order to overcome drawbacks described above existing in the prior art, provide it is a kind of towards
The gas sensor and preparation method thereof of acetone gas detection.
The present invention is achieved through the following technical solutions above-mentioned purpose, a kind of gas sensing towards acetone gas detection
Device, the gas sensor is with Fe2O3Material is applied on ceramic pipe electrode as gas sensitive material by the method for spin coating, real
Now to the highly selective detection for the acetone gas that concentration is 1ppm.
It is prepared by the method that the gas sensor of above-mentioned single acetone gas monitoring is all made of spin coating, the specific steps are：
A. the Fe of 5-100mg is taken2O3Material is evenly spread in the organic solvent of 1-50mL；
B. scattered Fe described in certain volume step a is taken2O3Sensitive material drips on the surface of N number of ceramic tube, then
Ceramic tube is connected on a rotary axis, shaft rotates on one side, and organic solvent volatilizees on one side, until volatilization completely,
Fe2O3Sensitive material can be uniformly deposited on ceramic pipe surface, form one layer of air-sensitive film；It is added dropwise on different ceramic tubes different
The Fe of number2O3Dispersion liquid obtains multiple with different-thickness Fe2O3The sensor of sensitive membrane.
C. the both ends of each of described ceramic pipe surface tumble in a pair of of gold electrode respectively in stepb, then weld respectively again
A platinum filament is connect as lead, lead need to be contacted with air-sensitive film, in ceramic tube pass through a heater strip, two conducting wires respectively with
Measuring circuit connection, heater strip are connect with heater circuit, and sensor works under 200-350 °C, and resistance is in 5-500 K
Ω。
D. the acetone performance of different film thickness gas sensors is tested, and the optimal gas sensor of performance is selected with this, is used
In the detection of low concentration (1 ppm) acetone.
In above-mentioned technical proposal, the Fe2O3The structure and morphology of material be nanoparticle, nano wire, nanobelt, nanotube,
One or more of nanocube, flower-like microsphere.
In above-mentioned technical proposal, organic solvent that the preparation method uses for ethyl alcohol, methanol, acetone, acetonitrile, toluene,
One of ethylene glycol, n-hexane, butanone or a variety of mixtures.
In above-mentioned technical proposal, the revolving speed of the gas sensor preparation process rotation axis is 10-200r/min.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can achieve following has
Beneficial effect：
1, from the interaction of material and object gas, the Fe of nanotopography structure is utilized2O3Material is as gas sensitization
Material realizes the detection to low concentration acetone gas so that response characteristic is more obvious；
2, Fe is completed using spinning movement2O3Sensitive material optimizes air-sensitive film thickness, changes in the uniform smearing of ceramic pipe surface
It has been apt to the selective response degree for object gas acetone.
Detailed description of the invention
Specific embodiments of the present invention are further described in detail with reference to the accompanying drawing, wherein：
Fig. 1 is Fe of the present invention2O3The scanning electron microscopy picture of nano wire；
Fig. 2 is the response curve of gas sensor test 1ppm acetone gas in the first embodiment of the invention；
Fig. 3 is Fe of the present invention2O3The scanning electron microscopy picture of microballoon；
Fig. 4 is the response curve of gas sensor test 1ppm acetone gas in second of embodiment of the invention.
Specific embodiment
Single gas sensor disclosed by the invention is all made of Fe2O3Material is as sensitive membrane, Fe2O3The structure of material
Pattern can be one or more of nanoparticle, nano wire, nanobelt, nanotube, nanocube, flower-like microsphere,
The thickness of sensing membrane is different in each sensor, responds difference to acetone gas, quick come the acetone for optimizing sensor with this
Perceptual energy is realized and is detected to the high sensitivity of low concentration (1 ppm) acetone gas.
It is prepared by the method that the gas sensor of single acetone gas monitoring is all made of spin coating, the specific steps are：
Step 1：Take the Fe of 5-100mg2O3Sensitive material is evenly spread in the organic solvent of 1-50mL, which can
Think ethyl alcohol, methanol, acetone, acetonitrile, toluene, ethylene glycol, n-hexane, one of butanone or a variety of mixtures；
Step 2：Take certain volume scattered Fe described in step 12O3Sensitive material drips on the surface of N number of ceramic tube
On, ceramic tube, around axial rotation, makes Fe with 10-200 r/min revolving speed2O3Sensitive material homogeneous dispersion is spin-coated on its surface, directly
It volatilizees completely to organic solvent, constitutes one layer of Fe2O3Sensitive membrane；The Fe of different numbers is added dropwise on different ceramic tubes2O3Dispersion liquid,
It obtains multiple with different-thickness Fe2O3The sensor of sensitive membrane；
Step 3：Sensor works at 200-350 DEG C, and resistance is in 5-500 K Ω；
Step 4：The acetone performance of different film thickness gas sensors is tested, and the optimal gas sensor of performance is selected with this, is used
In the detection of low concentration (1 ppm) acetone.
Embodiment 1：
1）By the Fe of 10 mg2O3Nano wire is evenly spread in the ethyl alcohol of 20 mL by ultrasound, Fe2O3The pattern knot of nano wire
Structure is as shown in Figure 1；
2）Take the 5 scattered Fe of μ L2O3Nano wire ethanol solution drips in the ceramic pipe surface for studding with gold electrode at 1, ceramics
Pipe, around axial rotation, makes Fe with 20 r/min revolving speeds2O3Nanowire dispersion is uniformly spin-coated on its surface, until organic solvent is complete
Full volatilization, constitutes layer of semiconductor Fe2O3Air-sensitive film；5 μ L semiconductor Fe of different numbers are added dropwise on different ceramic tubes2O3Nanometer
Line dispersion liquid obtains Fe with different thickness2O3N sensor of air-sensitive film；
3）Sensor works under 200-350 °C, and resistance is in 5-500 K Ω；
The response for defining sensor is S=Ra/Rg, and wherein Ra is the aerial resistance of sensor, and Rg is sensor to be measured
Resistance in gas.
The test of acetone response performance is carried out to N gas sensor of above-mentioned preparation, and best with this optimization performance
Gas sensor.Sensitive body is best to acetone response at spin coating 10 times or so.Acetone in diabetic's exhaled gas
Gas content is higher than 1.8 ppm, and acetone gas content is generally below 1 ppm in normal person's expiration.Therefore it is required that sensor
Recognition capability is in 1 ppm or less.As shown in Fig. 2, the sensor after optimizing film thickness is with higher to 1 ppm acetone gas
Response can be realized the health detection to diabetic.
Embodiment 2：
1）By the Fe of 5 mg2O3Microballoon is evenly spread in the ethyl alcohol of 5 mL by ultrasound, Fe2O3The appearance structure of microballoon such as Fig. 3
It is shown；
2）Take the 5 scattered Fe of μ L2O3Micron ball ethanol solution drips in the ceramic pipe surface for studding with gold electrode at 1, ceramics
Pipe, around axial rotation, makes Fe with 10 r/min revolving speeds2O3Micron ball homogeneous dispersion is spin-coated on its surface, until organic solvent is complete
Full volatilization, constitutes layer of semiconductor Fe2O3Air-sensitive film；10 μ L semiconductor Fe of different numbers are added dropwise on different ceramic tubes2O3It receives
Rice noodles dispersion liquid obtains Fe with different thickness2O3N sensor of air-sensitive film；
3）Sensor works under 200-350 °C, and resistance is in 5-500 K Ω；
The response for defining sensor is S=Ra/Rg, and wherein Ra is the aerial resistance of sensor, and Rg is sensor to be measured
Resistance in gas.
The test of acetone response performance is carried out to N gas sensor of above-mentioned preparation, and best with this optimization performance
Gas sensor.Sensitive body is best to acetone response at spin coating 6 times or so.Acetone in diabetic's exhaled gas
Gas content is higher than 1.8 ppm, and acetone gas content is generally below 1 ppm in normal person's expiration.Therefore it is required that sensor
Recognition capability is in 1 ppm or less.As shown in figure 4, the sensor after optimizing film thickness is with higher to 1 ppm acetone gas
Response can be realized the health detection to diabetic.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (5)
1. a kind of gas sensor towards acetone gas detection, it is characterised in that：The gas sensor is with Fe2O3Material conduct
Gas sensitive material is applied on ceramic pipe electrode by the method for spin coating, realizes the height to the acetone gas that concentration is 1ppm
Selective enumeration method.
2. a kind of gas sensor towards acetone gas detection according to claim 1, it is characterised in that：The Fe2O3
The structure and morphology of material be one of nanoparticle, nano wire, nanobelt, nanotube, nanocube, flower-like microsphere or
It is a variety of.
3. a kind of preparation method of gas sensor as described in claim 1, it is characterised in that：Single sensor is all made of rotation
Prepared by the method for painting, specific step is as follows：
A. the Fe of 5-100mg is taken2O3Sensitive material is evenly spread in the organic solvent of 1-50mL by ultrasound；
B. scattered Fe described in certain volume step a is taken2O3Sensitive material drips on the surface of ceramic tube, then will pottery
Porcelain tube is connected on a rotary axis, and shaft rotates on one side, and organic solvent volatilizees on one side, until volatilization completely, Fe2O3
Sensitive material can be uniformly deposited on ceramic pipe surface, form one layer of air-sensitive film；
C. the both ends of each of described ceramic pipe surface tumble in a pair of of gold electrode respectively in stepb, and one is then respectively welded again
Root platinum filament need to be contacted as lead, lead with air-sensitive film, in ceramic tube pass through a heater strip, two conducting wires respectively with measurement
Circuit connection, heater strip are connect with heater circuit, and sensor works under 200 ~ 350 °C, and resistance is in 5-500 K Ω.
4. the preparation method of gas sensor according to claim 3, it is characterised in that：The organic solvent be ethyl alcohol,
One of methanol, acetone, acetonitrile, toluene, ethylene glycol, n-hexane, butanone or a variety of mixtures.
5. the preparation method of gas sensor according to claim 3, it is characterised in that：The revolving speed of the shaft is 10-
200r/min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810227320.9A CN108828017A (en) | 2018-03-20 | 2018-03-20 | A kind of gas sensor and preparation method thereof towards acetone gas detection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810227320.9A CN108828017A (en) | 2018-03-20 | 2018-03-20 | A kind of gas sensor and preparation method thereof towards acetone gas detection |
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| CN108828017A true CN108828017A (en) | 2018-11-16 |
Family
ID=64154152
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| CN201810227320.9A Pending CN108828017A (en) | 2018-03-20 | 2018-03-20 | A kind of gas sensor and preparation method thereof towards acetone gas detection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109946348A (en) * | 2019-03-18 | 2019-06-28 | 中国药科大学 | A kind of foamed metal oxide is preparing the application in gas sensor |
| CN111579616A (en) * | 2020-05-29 | 2020-08-25 | 吉林大学 | Based on YSZ and Fe2TiO5-TiO2Acetone sensor of sensitive electrode, preparation method and application thereof |
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| US20150301020A1 (en) * | 2012-04-30 | 2015-10-22 | Council Of Scientific & Industrial Reasearch | A sensor composition for acetone detection in breath |
| CN106093137A (en) * | 2016-06-20 | 2016-11-09 | 吉林大学 | A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof |
| CN106770494A (en) * | 2016-11-29 | 2017-05-31 | 中华人民共和国龙岩出入境检验检疫局 | A kind of novel acetone sensor with ultra-fine tungsten oxide nano wire as sensitive material |
| CN106770497A (en) * | 2017-01-09 | 2017-05-31 | 吉林大学 | One kind is based on Pt/ α Fe2O3Acetone gas sensor of porous nanoparticles sensitive material and preparation method thereof |
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2018
- 2018-03-20 CN CN201810227320.9A patent/CN108828017A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150301020A1 (en) * | 2012-04-30 | 2015-10-22 | Council Of Scientific & Industrial Reasearch | A sensor composition for acetone detection in breath |
| CN104931540A (en) * | 2014-03-20 | 2015-09-23 | 中国科学院大连化学物理研究所 | Gas sensor array and preparation method thereof |
| CN106093137A (en) * | 2016-06-20 | 2016-11-09 | 吉林大学 | A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof |
| CN106770494A (en) * | 2016-11-29 | 2017-05-31 | 中华人民共和国龙岩出入境检验检疫局 | A kind of novel acetone sensor with ultra-fine tungsten oxide nano wire as sensitive material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109946348A (en) * | 2019-03-18 | 2019-06-28 | 中国药科大学 | A kind of foamed metal oxide is preparing the application in gas sensor |
| CN111579616A (en) * | 2020-05-29 | 2020-08-25 | 吉林大学 | Based on YSZ and Fe2TiO5-TiO2Acetone sensor of sensitive electrode, preparation method and application thereof |
| CN111579616B (en) * | 2020-05-29 | 2022-11-08 | 吉林大学 | Based on YSZ and Fe 2 TiO 5 -TiO 2 Acetone sensor of sensitive electrode, preparation method and application thereof |
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