CN103115947B - Preparation method and application of carbon-doped mesoporous metal oxide acetone sensor - Google Patents
Preparation method and application of carbon-doped mesoporous metal oxide acetone sensor Download PDFInfo
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Abstract
The invention relates to a preparation method and application of a carbon-doped mesoporous metal oxide acetone sensor. A gas sensor adopts a heater type device structure and takes an alumina ceramic tube as a carrier. A forked gold electrode is applied to the outer surface of the gas sensor. Platinum extraction electrodes are arranged at the two ends of the gas sensor. A heater strip is arranged in the ceramic tube. A gas sensitive material is coated on the outside of the ceramic tube and is multiwalled carbon nanotube doped monodisperse mesoporous ferroferric oxide. The gas sensor is prepared by preparing the alumina ceramic tube on which the material is coated into a tube core and then welding, packaging and aging the tube core. The preparation method is simple in process, mild in conditions and low in cost and is especially suitable for volume production. The prepared gas sensitive element is used for detecting the acetone concentration at 270-290 DEG C, has the characteristics of high sensitivity to 1-5400ppm acetone, good restorability, quick response and the like and can be used for determining acetone concentration in cosmetic and industrial production and environment detection.
Description
Technical field
The present invention relates to a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, belong to functional material and Metal Oxide Semiconductor Gas Sensing sensor preparation technology field.
Background technology
Because scientific technological advance makes rapid progress, modernization of industry degree improves constantly, and gaseous species, the quantity using in process of production and produce are on the increase.Wherein a lot of gas is inflammable and explosive, for example: methane, acetylene, hydrogen and liquefied petroleum gas (LPG) etc.; A lot of gas contains severe toxicity, for example: carbon monoxide, sulfuretted hydrogen and nitrogen-containing oxide etc.
In order to ensure production safety, just must at aspects such as production, use, transportation, storages, strengthen monitoring and qualitative analysis to gas, in many sensors, the application of gas sensor is shown one's talent, having a extensive future and having embodies huge commercial value, and the research and development of gas sensor cause the extensive concern of various countries.
Acetone is as a kind of conventional volatile, easy system poison, easily cause quick-fried chemical substance, is mainly used in solvent in solvent, the commercial production in organic synthesis raw material, cosmetics and extraction agent etc., significant to its detection.
Conventional gas sensor is to build after oxide waits modification by doping.In all kinds of gas sensors, instrument detects has the advantages such as highly sensitive, accuracy is strong, but because instrument is bulky, expensive, and test preliminary work is loaded down with trivial details, be unfavorable for real time monitoring, thereby its application is restricted; Semiconductor gas sensor with cheap, volume is little, simple in structure, respond the advantage such as fast and occupy the larger market share.
From exploitation nanoscale gas sensitive, start with to improve sensitivity, selectivity and stability and just become the focus that people pay close attention to, granularity and the specific surface area of this sensor gas-sensitive property and Semiconductor Powder are closely related.
In document [1]: Journal of Chemical Physics, in 2010,114,6237 – 6242, the people such as Zhihui Ai utilize surperficial microwave ancillary technique to prepare flower-shaped Fe
3o
4, its peak response to ethanol reaches 4.32; In document [2]: Sensors and Actuators B, 2011,158, in 229-234, after mixing CuO mutually with multi-walled carbon nano-tubes, the people such as Mitesh Parmar obtain gas sensitive, and studied its sensitive response to ethanol, and reach a conclusion: sensing range is 100-700 ppm, add multi-walled carbon nano-tubes to promote 50% than the sensitivity of simple CuO.
By reference to document, can find out: gas sensor sensitivity is lower, sensing range is narrower.
For this problem, the present invention proposes a kind of preparation of overdelicate carbon-doped mesoporous metal oxide acetone sensor, the specific surface area that the absorption property that carbon-based material is good and porous nanometer material are large, make it can be used as the gas sensitive that detects reductibility and oxidizing gas, utilize the present invention to play an important role at the field monitoring in the fields such as cosmetics, commercial production and environment measuring.
Summary of the invention
One of technical assignment of the present invention is in order to make up the deficiencies in the prior art, and a kind of preparation method of carbon-doped mesoporous metal oxide acetone sensor is provided, this technology of preparing mature and reliable.
Two of technical assignment of the present invention is to provide the application of this sensor, and this sensor is for the detection of escaping gas acetone.
The preparation method of a kind of carbon-doped mesoporous metal oxide acetone sensor provided by the invention, comprises the steps:
(1) multi-walled carbon nano-tubes monodisperse mesoporous tri-iron tetroxide (the MWNT@Fe that adulterates
3o
4) synthetic
Pipette ethylene glycol 20 mL, add 1.1 ~ 1.2 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.8 ~ 2.9 g anhydrous sodium acetates and 9.6 ~ 9.8 mL anhydrous ethylenediamines, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 20 ~ 25 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 7.0 ~ 8.0 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to dry 4.0 ~ 6.0 h of vacuum drying chamber of 50 ~ 60 ℃, makes MWNT@Fe
3o
4;
The diameter of described multi-walled carbon nano-tubes is at 8 ~ 15nm, length 50 μ m, and purity is greater than 95%.
(2) prepare the carbon-doped mesoporous metal oxide acetone of heater-type sensor
1) by MWNT@Fe synthetic to (1)
3o
4, in mortar, grind 10 ~ 15 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, drying at room temperature;
3) by the lead-in wire platinum filament on alumina ceramic tube and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 160 ~ 170 ℃, aging 4 ~ 7 days, make the sensitivity of sensor keep stable, encapsulation, makes the carbon-doped mesoporous metal oxide acetone of heater-type sensor.
The described ethylenediamine of step (1) is excessive, and excessive ethylenediamine makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.1 ~ 0.2 μ g/mg.
The described MWNT@of step (1) Fe
3o
4middle multi-walled carbon nano-tubes and Fe
3o
4mass ratio be 0.02 ~ 0.2: 1.
The application of a kind of carbon-doped mesoporous metal oxide acetone sensor of the present invention, is characterized in that under 270 ~ 290 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
The carbon-doped mesoporous metal oxide acetone of this heater-type sensor possesses following characteristics:
MWNT@Fe
3o
4after synthetic, be directly coated in aluminium oxide ceramics tube-surface, do not need high-temperature calcination.
MWNT@Fe
3o
4the carbon-doped mesoporous metal oxide acetone sensor of preparation has high sensitivity to acetone, and at 280 ℃, during to 1000ppm acetone, sensitivity is 20.07;
MWNT@Fe
3o
4preparation carbon-doped mesoporous metal oxide acetone sensor to the sensing range of acetone wide and detect lower limit low, sensing range is 1 ~ 5400 ppm.
MWNT@Fe
3o
4detection response time and the release time of carbon-doped mesoporous metal oxide acetone sensor to acetone of preparation, averaging time is at 7 ~ 20 s.
MWNT and mesoporous Fe
3o
4the synergy sensitivity that makes carbon-doped mesoporous metal oxide acetone sensor measure acetone significantly improve, by MWNT@Fe of the present invention
3o
4gas sensor and the Fe of preparation
3o
4the gas sensor of preparation carries out contrast experiment, and the detection sensitivity of finding the former is 3.7 times of the latter.
As can be seen here, MWNT is doped into mesopore metal oxide Fe
3o
4after, significantly improved the sensitivity of sensor.
Carbon-doped mesoporous metal oxide acetone sensor prepared by the present invention is a kind of heater-type gas sensor, it has overcome the shortcoming of directly-heated type structure, make to measure the utmost point with add thermoae separation, and heater strip does not contact with gas sensitive, avoided influencing each other of measuring circuit and heating circuit, device thermal capacity is large, has reduced the impact of environment temperature on device heats temperature, and its stability, reliability are all good than directly-heated type device.
Accompanying drawing explanation
Accompanying drawing 1 is the carbon-doped mesoporous metal oxide acetone sensor of the inventive method, 1.Al
2o
3ceramic pipe, 2. gas sensing layer, 3. Ni-Cr heater strip, 4. gold interdigital electrode, 5. platinum filament.
Accompanying drawing 2 is the carbon-doped mesoporous metal oxide acetone sensor that makes response recovery curves to 400 ppm acetone.
Embodiment
below in conjunction with drawings and Examples, the present invention is further described.
embodiment 1:mWNT@Fe
3o
4synthetic method
one
Pipette ethylene glycol 20 mL, add 1.1 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.8 g anhydrous sodium acetates and 9.6 mL anhydrous ethylenediamines, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 20 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 7.0 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to the dry 6.0h of vacuum drying chamber of 50 ℃, makes MWNT@Fe
3o
4; The diameter of described multi-walled carbon nano-tubes is at 8 nm, length 50 μ m, and purity is greater than 95%; Described ethylenediamine is excessive, makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.2 μ g/mg; Multi-walled carbon nano-tubes and Fe
3o
4mass ratio be 0.02: 1.
embodiment 2:mWNT@Fe
3o
4synthetic method
two
Pipette ethylene glycol 20 mL, add 1.2 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.9 g anhydrous sodium acetates and 9.7mL anhydrous ethylenediamine, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 22 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 7.5 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to dry 5.0 h of vacuum drying chamber of 55 ℃, makes MWNT@Fe
3o
4; The diameter of described multi-walled carbon nano-tubes is at 12 nm, length 50 μ m, and purity is greater than 95%; Described ethylenediamine is excessive, makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.10 μ g/mg; Multi-walled carbon nano-tubes and Fe
3o
4mass ratio be 0.04: 1.
embodiment 3:mWNT@Fe
3o
4synthetic method three
Pipette ethylene glycol 20 mL, add 1.1 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.9 g anhydrous sodium acetates and 9.8 mL anhydrous ethylenediamines, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 25 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 8.0 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to dry 5.0 h of vacuum drying chamber of 60 ℃, makes MWNT@Fe
3o
4; The diameter of described multi-walled carbon nano-tubes is at 10 nm, length 50 μ m, and purity is greater than 95%; Described ethylenediamine is excessive, makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.15 μ g/mg; Multi-walled carbon nano-tubes and Fe
3o
4mass ratio be 0.1: 1.
embodiment 4:mWNT@Fe
3o
4synthetic method four
Pipette ethylene glycol 20 mL, add 1.2 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.9 g anhydrous sodium acetates and 9.7 mL anhydrous ethylenediamines, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 25 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 7.8 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to dry 4.0 h of vacuum drying chamber of 60 ℃, makes MWNT@Fe
3o
4; The diameter of described multi-walled carbon nano-tubes is at 15nm, length 50 μ m, and purity is greater than 95%; Described ethylenediamine is excessive, makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.18 μ g/mg; Multi-walled carbon nano-tubes and Fe
3o
4mass ratio be 0.2: 1.
embodiment 5:acetone transducer production method and application one
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) by synthetic embodiment 1 or 2 or the 3 or 4 MWNT@Fe obtaining
3o
4after nano particle is dry, in mortar, grinds 10 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, forms gas sensing layer, sees accompanying drawing 1, drying at room temperature;
3) by the lead-in wire platinum filament on ceramic pipe and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 160 ℃, aging 7 days, make the sensitivity of sensor keep stable, encapsulation, makes the carbon-doped mesoporous metal oxide acetone sensor of heater-type;
5) by carbon-doped mesoporous metal oxide acetone sensor under 280 ℃ of conditions of working temperature, for the detection of acetone.
Detection obtains correlation parameter as shown in Figure 2: element work optimum temperature is 280 ℃; At 280 ℃, the detection sensitivity (Ra/Rg) to 1000 ppm acetone is 20.07 to gas sensor, is response time and release time 10 ~ 20 s, and sensing range is wide and detection lower limit is low, is 1 ~ 5400 ppm; Element is greater than 25 days serviceable life.
embodiment 6:acetone transducer production method and application two
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) by synthetic embodiment 1 or 2 or the 3 or 4 MWNT@Fe obtaining
3o
4after nano particle is dry, in mortar, grinds 13 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, drying at room temperature;
3) by the lead-in wire platinum filament on ceramic pipe and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 165 ℃, aging 4 days, make the sensitivity of sensor keep stable, encapsulation, makes the carbon-doped mesoporous metal oxide acetone sensor of heater-type;
5) by carbon-doped mesoporous metal oxide acetone sensor under 270 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
Detection sensitivity (Ra/Rg) to 1000 ppm acetone is 20.07, is response time and release time 1 ~ 20 s, and sensing range is wide and detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element is greater than 25 days serviceable life.
embodiment 7:acetone transducer production method and application three
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) by synthetic embodiment 1 or 2 or the 3 or 4 MWNT@Fe obtaining
3o
4after nano particle is dry, in mortar, grinds 15 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, drying at room temperature;
3) by the lead-in wire platinum filament on ceramic pipe and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 170 ℃, aging 5 days, make the sensitivity of sensor keep stable, encapsulation, makes the carbon-doped mesoporous metal oxide acetone sensor of heater-type;
5) by carbon-doped mesoporous metal oxide acetone sensor under 280 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
Detection sensitivity (Ra/Rg) to 1000 ppm acetone is 20.07, is response time and release time 10 ~ 20 s, and sensing range is wide and detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element is greater than 25 days serviceable life.
embodiment 8:acetone transducer production method and application four
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) by synthetic embodiment 1 or 2 or the 3 or 4 MWNT@Fe obtaining
3o
4after nano particle is dry, in mortar, grinds 15 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, drying at room temperature;
3) by the lead-in wire platinum filament on ceramic pipe and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 170 ℃, aging 6 days, make the sensitivity of sensor keep stable, encapsulation, makes the carbon-doped mesoporous metal oxide acetone sensor of heater-type;
5) by carbon-doped mesoporous metal oxide acetone sensor under 290 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
Detection sensitivity (Ra/Rg) to 1000 ppm acetone is 20.07, is response time and release time 10 ~ 20 s, and sensing range is wide and detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element is greater than 25 days serviceable life.
embodiment 9:the detection Contrast on effect of two kinds of gas sensors
Step is as follows:
1) by the synthetic embodiment 1 MWNT@Fe obtaining
3o
4the Fe of nano particle and non-impurity-doped multi-walled carbon nano-tubes
3o
4after nano material is dry, in mortar, grinds respectively 15 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry and Fe
3o
4pasty slurry;
2) above-mentioned two kinds of slurries are evenly coated in respectively to aluminium oxide ceramics tube-surface and form film, drying at room temperature;
3) by the lead-in wire platinum filament on ceramic pipe and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 160 ℃, aging 5 days, make the sensitivity of sensor keep stable, encapsulation, makes heater-type carbon-doped mesoporous metal oxide acetone sensor and without carbon-doped mesoporous metal oxide acetone sensor;
5) above-mentioned two kinds of acetone sensors are under 280 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
Relatively two kinds of acetone sensors prepared by gas sensing materials, their detection effect as shown in Figure 2, can be found out by accompanying drawing 2, MWNT@Fe
3o
4with Fe
3o
4gas sensor prepared by gas sensing materials is compared, and the former detection sensitivity is 3.7 times of the latter.
Claims (4)
1. a preparation method for carbon-doped mesoporous metal oxide acetone sensor, is characterized in that preparation process is as follows:
(1) multi-walled carbon nano-tubes monodisperse mesoporous tri-iron tetroxide (the MWNT@Fe that adulterates
3o
4) synthetic
Pipette ethylene glycol 20 mL, add 1.1 ~ 1.2 g FeCl
36H
2o, ultrasonic, make its dissolving, under magnetic agitation, add 2.8 ~ 2.9 g anhydrous sodium acetates and 9.6 ~ 9.8 mL anhydrous ethylenediamines, and add multi-walled carbon nano-tubes simultaneously, vigorous stirring 20 ~ 25 min, potpourri is placed in the reactor of teflon, at 200 ℃ of pyroreaction 7.0 ~ 8.0 h, naturally cool to afterwards room temperature, be washed with water to solution and present neutrality, solid is placed in to dry 4.0 ~ 6.0 h of vacuum drying chamber of 50 ~ 60 ℃, makes MWNT@Fe
3o
4;
The diameter of described multi-walled carbon nano-tubes is at 8 ~ 15nm, length 50 μ m, and purity is greater than 95%;
(2) prepare the carbon-doped mesoporous metal oxide acetone of heater-type sensor
1) by MWNT@Fe synthetic to (1)
3o
4, in mortar, grind 10 ~ 15 min, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe
3o
4pasty slurry;
2) by MWNT@Fe
3o
4pasty slurry is evenly coated in aluminium oxide ceramics tube-surface and forms film, drying at room temperature;
3) by the lead-in wire platinum filament on alumina ceramic tube and through heater strip and the base of tube chamber, weld, make gas sensor semi-manufacture;
4) by gas sensor semi-manufacture at 160 ~ 170 ℃, aging 4 ~ 7 days, encapsulation, make the carbon-doped mesoporous metal oxide acetone of heater-type sensor.
2. the preparation method of a kind of carbon-doped mesoporous metal oxide acetone sensor according to claim 1, it is characterized in that: the described ethylenediamine of step (1) is excessive, excessive ethylenediamine makes the mesoporous ferriferrous oxide surface of preparation have amino group, and the amino amount containing is 0.1 ~ 0.2 μ g/mg.
3. the preparation method of a kind of carbon-doped mesoporous metal oxide acetone sensor according to claim 1, is characterized in that: the described MWNT@of step (1) Fe
3o
4the mass ratio of middle multi-walled carbon nano-tubes and tri-iron tetroxide is 0.02 ~ 0.2: 1.
4. the carbon-doped mesoporous metal oxide acetone of the one of preparation according to claim 1 sensor, is characterized in that under 270 ~ 290 ℃ of conditions of working temperature, for the detection of escaping gas acetone.
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| CN105259216A (en) * | 2015-11-18 | 2016-01-20 | 济南大学 | Preparing method and application of alcohol gas sensitive sensor based on ferroferric oxide hybridization carbon materials |
| CN107976469A (en) * | 2017-11-16 | 2018-05-01 | 吉林大学 | A kind of soil nutrient device for fast detecting based on Artificial Olfactory |
| CN111650317B (en) * | 2020-07-15 | 2022-04-26 | 南通市疾病预防控制中心 | High-flux detection method for polycyclic aromatic hydrocarbons in traditional Chinese medicinal materials |
| CN113092539A (en) * | 2021-03-16 | 2021-07-09 | 宁波大学 | High-stable-state PUF (physical unclonable function) utilizing semiconductor gas sensor |
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