CN103115947A - 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 PDF

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CN103115947A
CN103115947A CN2013100693299A CN201310069329A CN103115947A CN 103115947 A CN103115947 A CN 103115947A CN 2013100693299 A CN2013100693299 A CN 2013100693299A CN 201310069329 A CN201310069329 A CN 201310069329A CN 103115947 A CN103115947 A CN 103115947A
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acetone
preparation
metal oxide
sensor
mwnt
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CN103115947B (en
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魏琴
杜斌
冯锐
王志玲
王玉兰
吴丹
张勇
马洪敏
高亮
王晓东
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University of Jinan
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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

A kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor
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 gases are inflammable and explosive, for example: methane, acetylene, hydrogen and liquefied petroleum gas (LPG) etc.; A lot of gases contain severe toxicity, for example: carbon monoxide, sulfuretted hydrogen and nitrogen-containing oxide etc.
In order to ensure production safety, just must strengthen to gas monitoring and qualitative analysis at aspects such as production, use, transportation, storages, the application of gas sensor is shown one's talent in many sensors, 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 mainly used in solvent, the solvent in commercial production and extraction agent etc. in organic synthesis raw material, cosmetics as a kind of volatile, easy system poison commonly used, easily cause quick-fried chemical substance, and is significant to its detection.
Gas sensor commonly used is oxide by building after the modification such as adulterate.In all kinds of gas sensors, instrument detects has the advantages such as highly sensitive, that 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, the response advantage such as fast is occupied the larger market share.
Start with to improve sensitivity, selectivity and stability from exploitation nanoscale gas sensitive 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, the people such as Mitesh Parmar with CuO with obtain gas sensitive after multi-walled carbon nano-tubes mixes mutually, and studied its sensitivity response to ethanol, reach a conclusion: sensing range is 100-700 ppm, adds multi-walled carbon nano-tubes to promote 50% than the sensitivity of simple CuO.
Can find out by list of references: 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, a kind of preparation method of carbon-doped mesoporous metal oxide acetone sensor to be 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 used 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) the monodisperse mesoporous tri-iron tetroxide of multi-walled carbon nano-tubes doping (MWNT@Fe 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 simultaneously multi-walled carbon nano-tubes, 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 dry 4.0 ~ 6.0 h of vacuum drying chamber of 50 ~ 60 ℃, namely 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) the carbon-doped mesoporous metal oxide acetone of preparation heater-type sensor
1) the MWNT@Fe that (1) is synthetic 3O 4, grind 10 ~ 15 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, drying at room temperature;
3) with the lead-in wire platinum filament on alumina ceramic tube and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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 that contains 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, is used 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 4Directly be coated in the aluminium oxide ceramics tube-surface after synthetic and get final product, 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 under 280 ℃, during to 1000ppm acetone, sensitivity is 20.07;
MWNT@Fe 3O 4The carbon-doped mesoporous metal oxide acetone sensor of preparation is wide and to detect lower limit low to the sensing range of acetone, and sensing range is 1 ~ 5400 ppm.
MWNT@Fe 3O 4The carbon-doped mesoporous metal oxide acetone sensor of preparation is to detection response time and release time of acetone, and 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, with MWNT@Fe of the present invention 3O 4Gas sensor and the Fe of preparation 3O 4The gas sensor of preparation compares experiment, and the detection sensitivity of finding the former is 3.7 times of the latter.
This shows, MWNT is doped into mesopore metal oxide Fe 3O 4After, significantly improved the sensitivity of sensor.
The carbon-doped mesoporous metal oxide acetone sensor of the present invention's preparation is a kind of heater-type gas sensor, it has overcome the shortcoming of directly-heated type structure, make and measure the utmost point and add thermoae the 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 the device heats temperature, and its stability, reliability are all good than directly-heated type device.
Description of drawings
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 that the carbon-doped mesoporous metal oxide acetone sensor that makes is to the response recovery curve of 400 ppm acetone.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
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 simultaneously multi-walled carbon nano-tubes, 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 the dry 6.0h of vacuum drying chamber of 50 ℃, namely makes MWNT@Fe 3O 4The 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 that contains 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 simultaneously multi-walled carbon nano-tubes, 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 dry 5.0 h of vacuum drying chamber of 55 ℃, namely makes MWNT@Fe 3O 4The 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 that contains 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 simultaneously multi-walled carbon nano-tubes, 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 dry 5.0 h of vacuum drying chamber of 60 ℃, namely makes MWNT@Fe 3O 4The 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 that contains 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 simultaneously multi-walled carbon nano-tubes, 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 dry 4.0 h of vacuum drying chamber of 60 ℃, namely makes MWNT@Fe 3O 4The 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 that contains 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 use one
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) with embodiment 1 or 2 or the 3 or 4 synthetic MWNT@Fe that obtain 3O 4After the nano particle drying, grind 10 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, and namely consists of gas sensing layer, sees accompanying drawing 1, drying at room temperature;
3) with the lead-in wire platinum filament on ceramic pipe and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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) with carbon-doped mesoporous metal oxide acetone sensor under 280 ℃ of conditions of working temperature, be used for the detection of acetone.
Detection obtains correlation parameter as shown in Figure 2: element work optimum temperature is 280 ℃; Gas sensor is 20.07 in 280 ℃ of detection sensitivities to 1000 ppm acetone (Ra/Rg), is response time and release time 10 ~ 20 s, and sensing range is wide and the detection lower limit is low, is 1 ~ 5400 ppm; Element serviceable life was greater than 25 days.
Embodiment 6:Acetone transducer production method and use two
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) with embodiment 1 or 2 or the 3 or 4 synthetic MWNT@Fe that obtain 3O 4After the nano particle drying, grind 13 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, drying at room temperature;
3) with the lead-in wire platinum filament on ceramic pipe and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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) with carbon-doped mesoporous metal oxide acetone sensor under 270 ℃ of conditions of working temperature, be used 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 the detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element serviceable life was greater than 25 days.
Embodiment 7:Acetone transducer production method and use three
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) with embodiment 1 or 2 or the 3 or 4 synthetic MWNT@Fe that obtain 3O 4After the nano particle drying, grind 15 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, drying at room temperature;
3) with the lead-in wire platinum filament on ceramic pipe and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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) with carbon-doped mesoporous metal oxide acetone sensor under 280 ℃ of conditions of working temperature, be used 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 the detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element serviceable life was greater than 25 days.
Embodiment 8:Acetone transducer production method and use four
The invention provides a kind of preparation method and application of carbon-doped mesoporous metal oxide acetone sensor, step is as follows:
1) with embodiment 1 or 2 or the 3 or 4 synthetic MWNT@Fe that obtain 3O 4After the nano particle drying, grind 15 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, drying at room temperature;
3) with the lead-in wire platinum filament on ceramic pipe and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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) with carbon-doped mesoporous metal oxide acetone sensor under 290 ℃ of conditions of working temperature, be used 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 the detection lower limit is low, and sensing range is 1 ~ 5400 ppm; Element serviceable life was greater than 25 days.
Embodiment 9:The detection Contrast on effect of two kinds of gas sensors
Step is as follows:
1) with the synthetic MWNT@Fe that obtains of embodiment 1 3O 4The Fe of nano particle and non-impurity-doped multi-walled carbon nano-tubes 3O 4After the nano material drying, grind respectively 15 min in mortar, 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 evenly are coated in respectively the formation of aluminium oxide ceramics tube-surface and film, drying at room temperature;
3) with the lead-in wire platinum filament on ceramic pipe and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 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 under 280 ℃ of conditions of working temperature, are used for the detection of escaping gas acetone.
Compare the acetone sensors of two kinds of gas sensing materials preparations, their detection effect can be found out by accompanying drawing 2 as shown in Figure 2, MWNT@Fe 3O 4With Fe 3O 4The gas sensor of gas sensing materials preparation is compared, and the former detection sensitivity is 3.7 times of the latter.

Claims (4)

1. the preparation method of a carbon-doped mesoporous metal oxide acetone sensor is characterized in that preparation process is as follows:
(1) the monodisperse mesoporous tri-iron tetroxide of multi-walled carbon nano-tubes doping (MWNT@Fe 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 simultaneously multi-walled carbon nano-tubes, 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 dry 4.0 ~ 6.0 h of vacuum drying chamber of 50 ~ 60 ℃, namely 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) the carbon-doped mesoporous metal oxide acetone of preparation heater-type sensor
1) the MWNT@Fe that (1) is synthetic 3O 4, grind 10 ~ 15 min in mortar, and add a small amount of absolute ethyl alcohol furnishing MWNT@Fe 3O 4Pasty slurry;
2) with MWNT@Fe 3O 4Pasty slurry evenly is coated in the formation of aluminium oxide ceramics tube-surface and films, drying at room temperature;
3) with the lead-in wire platinum filament on alumina ceramic tube and pass the heater strip of tube chamber and the base welding, make the gas sensor semi-manufacture;
4) with the gas sensor semi-manufacture under 160 ~ 170 ℃, aging 4 ~ 7 days, the 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 that contains 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. a kind of carbon-doped mesoporous metal oxide acetone sensor of preparation according to claim 1, is characterized in that under 270 ~ 290 ℃ of conditions of working temperature, is used for the detection of escaping gas acetone.
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