CN108387612A - With Al2O3/α-Fe2O3Composite nano fiber is sensitive material triethylamine sensor and preparation method thereof - Google Patents
With Al2O3/α-Fe2O3Composite nano fiber is sensitive material triethylamine sensor and preparation method thereof Download PDFInfo
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- CN108387612A CN108387612A CN201810162994.5A CN201810162994A CN108387612A CN 108387612 A CN108387612 A CN 108387612A CN 201810162994 A CN201810162994 A CN 201810162994A CN 108387612 A CN108387612 A CN 108387612A
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- G01—MEASURING; TESTING
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
Abstract
One kind is with Al2O3/α‑Fe2O3Composite nano fiber is the triethylamine sensor and preparation method thereof of sensitive electrode material, belongs to gas sensor technical field.Sensor carries the Al of 2 discrete rectangle gold electrodes by upper surface with 2 discrete L-shaped gold electrodes, lower surface with ruthenium-oxide heating layer and in ruthenium-oxide heating layer surface2O3Insulated ceramic plates are coated in L-shaped gold electrode and Al2O3The Al of insulated ceramic plates upper surface2O3/α‑Fe2O3Composite nano fiber sensitive material film forms.Al2O3Addition, change α Fe2O3The shape characteristic of semiconductor nano fiber, it is suppressed that α Fe2O3The growth of crystal grain increases the specific surface area of sensitive material, to improve the sensitivity of sensor.Meanwhile Al2O3/α‑Fe2O3The loose porous structure of composite nano fiber makes the triethylamine sensor that we make have response time quickly, good repeatability and response recovery characteristics.The Monitoring lower-cut of the sensor is 1ppm, can be used for the detection of triethylamine steam content in indoor environment.
Description
Technical field
The invention belongs to gas sensor technical fields, and in particular to one kind is with Al2O3/α-Fe2O3Composite nano fiber is
Triethylamine (triethylamine) sensor of sensitive electrode material and preparation method thereof, is mainly used for the inspection of atmospheric environment
It surveys.
Background technology
Triethylamine (TEA), is mainly used as organic solvent, catalyst, curing agent and polymerization inhibitor, is a kind of extremely important
Chemical industry Organic Ingredients.And at the same time, it is also a kind of inflammable, explosive and toxic one of volatile organic compound.
If our skin contact can cause chemical burn to triethylamine.Importantly, it have to our respiratory tract it is very strong
Irritation can cause serious pulmonary edema.Currently, detection triethylamine relies primarily on large-scale analytical instrument, such as makings connection spectrum
Instrument and infrared spectrometer etc., however its volume is big, price is high, the shortcomings of can not detecting in real time, limit them in real life
Application.Metal oxide semiconductor gas sensor is low with price, manufacture craft is simple, high sensitivity, can be used in real time
The advantages that detection, can be applied and build portable detector.Therefore, it has become everybody research hotspots.
In fact, deepening constantly always around the research for improving triethylamine transducer sensitivity.Especially nanometer
The improvement sensor performance that develops into of science and technology provides good opportunity.α-Fe2O3Because it is with preferable stability, valence
Lattice are cheap, prepare the advantages such as simple, are applied to the numerous areas such as photocatalysis, lithium battery, pigment, in addition to this, α-
Fe2O3It is considered as after SnO2With gas sensitive most widely used after ZnO.Studies have shown that can answering with two kinds of different oxides
It closes to promote the further modification of gas-sensitive property, to obtain better gas-sensitive property.Al will be used in this patent2O3With α-
Fe2O3Compound method promotes α-Fe2O3The further modification of gas-sensitive property.
Invention content
The object of the present invention is to provide a kind of Al prepared based on electrostatic spinning technique2O3/α-Fe2O3Composite nano fiber
Answering in terms of triethylamine steam is detected in environment for the triethylamine sensor of sensitive electrode material, preparation method and its indoors
With.The present invention is compound by being carried out to semi-conducting material, increases the sensitivity of sensor, improves the response speed of sensor, promotees
Into such sensor field of gas detection functionization.
The obtained sensor of the present invention has the rapid response time other than with higher sensitivity, well
Repeatability and response recovery characteristics.The Monitoring lower-cut of the sensor is 1ppm, can be used for triethylamine steam in indoor environment and contains
The detection of amount.
As shown in Figure 1, Al of the present invention2O3/α-Fe2O3Composite nano fiber is that the triethylamine of sensitive electrode material passes
Sensor is plate armature, and by upper surface band, there are two discrete L-shaped gold electrode 1, lower surfaces to carry ruthenium-oxide heating layer 5
Al2O3Insulated ceramic plates 4 and semiconductor sensitive material film 3 form, and wherein there are two discrete for 5 lower surface band of ruthenium-oxide heating layer
Rectangle gold electrode 6；Semiconductor sensitive material film 3 is prepared in two discrete L-shaped gold electrodes 1 and Al2O3Insulated ceramic plates 4
Upper surface；Each L-shaped gold electrode 1 and rectangle gold electrode 6 are respectively welded with a platinum line 2 and 2 ', by measuring and 2 L
Resistance between two platinum lines 2 that shape gold electrode 1 is respectively welded can obtain the resistance between two L-shaped gold electrodes, by with two
Two platinum lines 2 ' that rectangle gold electrode 6 is respectively welded can apply electric current to ruthenium-oxide heating layer 5, give Al2O3Insulated ceramic plates 4
It is heated so as to control the operating temperature of gas sensor.
According to the definition S=R of sensitivity Sa/Rg, wherein RaThe aerial resistance value of representative sensor, RgRepresent sensing
The size of resistance value of the device under test gas, resistance value is by Fluke instrument measurements, by measuring RaAnd Rg, being computed can
Obtain the sensitivity of sensor；It is characterized in that：Semiconductor sensitive material is Al2O3/α-Fe2O3Compound oxide semiconductor
Nanofiber, the mass ratio 0.125~0.375 of silicon source (aluminium isopropoxide) and source of iron (ferric acetyl acetonade)：1；The sensitive material
It is to be prepared using electrostatic spinning technique, hot pressing is in L-shaped gold electrode 1 and Al after calcining2O3The upper surface of insulated ceramic plates 4；
Al2O3Addition, change α-Fe2O3The shape characteristic of semiconductor nano fiber so that α-Fe2O3Nanofiber is received by hollow
Mitron eventually becomes the more smooth solid nanofiber in surface, it is suppressed that α-Fe2O3The growth of crystal grain, increases sensitive material
Specific surface area, to improve the sensitivity of sensor.Meanwhile Al2O3/α-Fe2O3The loose porous structure of composite nano fiber makes
Obtaining the triethylamine sensor that we make has the response time quickly.In addition, the system of tablet type sensor and oxide semiconductor
Make simple for process, is conducive to industrial batch production.α-Fe2O3Nanofiber and Al2O3/α-Fe2O3Composite nano fiber it is straight
Diameter is about 100nm.
One kind of the present invention is with Al2O3/α-Fe2O3Composite nano fiber is that the triethylamine of sensitive electrode material senses
The preparation method of device, its step are as follows：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5~10mL N-N dimethylformamides,
Stirring obtains solution A in 2~5 hours；The aluminium isopropoxide of 0.05~0.15g, 0.5g polyacrylonitrile are dissolved in 5~10mL N-N bis-
In methylformamide, heating stirring obtains solution B in 2~5 hours under 60~80 DEG C of water-baths, and later, solution A is poured into solution B,
Continue stirring 0.5~3 hour after obtaining mixed liquor；
2) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 10~20cm, spinning nozzle
The voltage applied between collecting board is 5~15kV, collects plate earthing, and spinning obtains a nanometer electrospinning after 2~5 hours on collecting board
Silk product；
3) above-mentioned nanometer Electrospun product is calcined 1~3 hour at 450~550 DEG C and obtains Al2O3/α-Fe2O3It is compound
Nanofiber sensitive material, by the sensitive material be placed on commercially available upper surface carry 2 discrete L-shaped gold electrodes 1, following tables
Face carries the insulation Al of 2 discrete rectangle gold electrodes 6 with ruthenium-oxide heating layer 5 and on 5 surface of ruthenium-oxide heating layer2O3Pottery
The upper surface of porcelain plate 4, and make sensitive material that L-shaped gold electrode 1 be completely covered, then hot pressing 2~6 minutes, shape at 80~120 DEG C
At 10~30 μm thick of conductor oxidate sensitive material film 3；A length of 1.3~1.7mm of ceramic wafer, width be 0.8~
1.3mm, thickness are 0.08~0.12mm；
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 is calcined 1~3 hour at 350~450 DEG C, finally by above-mentioned device
Part is welded and is encapsulated, to obtain sensor of the present invention.
Advantages of the present invention：
(1) sensor utilizes common N-type semiconductor material α-Fe2O3, it has good chemical stability；
(2) Al is utilized2O3/α-Fe2O3Composite nano fiber can be such that the sensitivity of sensor improves as sensitive material,
Promote its functionization；
(3)Al2O3/α-Fe2O3Composite nano fiber is in 175~300 DEG C of test temperature, the response to 100ppm triethylamines
Time is 1~2s, is not reported both at home and abroad.
(4)Al2O3/α-Fe2O3Composite nano fiber is made using electrostatic spinning technique, and production method is simple, low cost
The honest and clean industrial production conducive to mass.
Description of the drawings
Fig. 1：Al2O3/α-Fe2O3The structural schematic diagram of composite nano fiber semiconductor triethylamine sensor；
Fig. 1 (a) is sensor surface structure schematic diagram；Fig. 1 (b) sensor lower surface configuration schematic diagrames；
Fig. 2：The XRD diagram of comparative example, embodiment 1, embodiment 2 and embodiment 3；
Fig. 3：The SEM figures of comparative example, embodiment 1, embodiment 2 and embodiment 3；
Fig. 4：In comparative example, embodiment 1, embodiment 2 and embodiment 3 sensor in different operating temperature to 100ppm tri-
The Sensitivity comparison curve of ethamine；
Fig. 5：In the temperature range (175~300 DEG C) of test, response recovery time of the embodiment 2 to 100ppm triethylamines
Line chart.
As shown in Figure 1, the names of the parts are：L-shaped gold electrode 1；Platinum line 2 and 2 '；Semiconductor sensitive material 3；Al2O3Insulation
Ceramic wafer 4；Ruthenium-oxide heating layer 5；Rectangle gold electrode 6.
Fig. 2 is comparative example and embodiment 1, the XRD diagram of 2,3 four samples.It can be seen from the figure that the XRD of four samples
It peak can be with pure α-Fe2O3Characteristic peak match, be not found the presence of the relevant peaks of aluminium oxide, it was demonstrated that aluminium oxide exists
In composite sensitive material in the form of unbodied there is.In addition to this, with Al2O3Increase, the diffraction maximum of XRD becomes to get over
Come it is wider, this also means that with Al2O3Increase, the crystal grain for forming nanofiber is smaller and smaller.
Fig. 3 (a)-(d) corresponds respectively to comparative example and the SEM of embodiment 1,2,3 four samples schemes.From Fig. 3, we can be with
Know, the diameter of the nanofiber of four groups of samples is all in 100 rans.The pattern of fiber becomes loose porous from nanotube
Nanofiber arrives smooth nanofiber again.Consistent with the result that the XRD diagram of Fig. 2 obtains, the particle of the fiber of composition becomes to get over
Come smaller.
Fig. 4 is for the device made by comparative example and embodiment 1,2,3 to the sensitivity of 100ppm triethylamines with operating temperature
Change curve.It can be seen from the figure that the optimum working temperature of all devices is all 250 DEG C.At a temperature of this, comparative example
Made device is 3.91 to the sensitivity of 100ppm triethylamines, and the device made by 2 sample of embodiment is right at 250 DEG C
The sensitivity highest of 100ppm triethylamines, value 15.19, its sensitivity are probably the 3.88 of comparative example making devices
Times.
Fig. 5 is response recovery time broken line of the embodiment 2 to 100ppm triethylamines within the temperature range of entire test
Figure.It will be seen that under all test temperatures to the response time of 100ppm triethylamines be no more than two seconds, and recovery time with
The increase for test temperature is accordingly being shortened.
Specific implementation mode
Comparative example：
With α-Fe2O3Nanotube makes flat triethylamine sensor, specific manufacturing process as sensitive material：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5mL N-N dimethylformamides, are stirred
Obtain solution A within 3 hours；0.5g polyacrylonitrile is dissolved in 5mL N-N dimethylformamides, 70 DEG C of heating stirrings 3 of water-bath are small
When obtain solution B, later, solution A is poured into solution B, obtains continuing stirring after mixed liquor obtaining the forerunner of spinning in 1 hour
Liquid.
2) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Integrate and apply voltage between plate as 9.5kV, collection plate earthing obtains a nanometer Electrospun product after spinning about 3 hours on collecting board；
3) above-mentioned nanometer Electrospun product is calcined at 500 DEG C and obtains within 2 hours di-iron trioxide nanotube sensitive material,
The sensitive material is placed on commercially available upper surface and carries ruthenium-oxide heating layer 5 with 2 discrete L-shaped gold electrodes 1, lower surface
Insulation Al2O3The upper surface of ceramic wafer 4, and make sensitive material that L-shaped gold electrode 1 be completely covered, the then hot pressing 3 at 100 DEG C
Minute, form 10~30 μm of sensitive material film 3.
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 is calcined 2 hours at 400 DEG C, finally welds above-mentioned device
It connects and encapsulates, to obtain sensor of the present invention.
Embodiment 1
With the mass ratio of silicon source (aluminium isopropoxide) and source of iron (ferric acetyl acetonade) for 0.125：1 Al2O3/α-Fe2O3It is multiple
It closes nanofiber sensitive material and makes flat triethylamine sensor, specific manufacturing process：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5mL N-N dimethylformamides, are stirred
Obtain solution A within 3 hours；By 0.05g aluminium isopropoxides, 0.5g polyacrylonitrile is dissolved in 5 mL N-N dimethylformamides, water-bath
70 DEG C of heating stirrings obtain solution B in 3 hours, and later, solution A is poured into solution B, continue stirring 1 hour after obtaining mixed liquor
Obtain the precursor liquid of spinning.
2) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Collect that apply voltage between plate be 9.5 ± 1kV, collects plate earthing, after spinning about 3 hours, a nanometer Electrospun production is obtained on collecting board
Object；
3) above-mentioned nanometer Electrospun product is calcined at 500 DEG C and obtains within 2 hours di-iron trioxide nanotube sensitive material,
The sensitive material is placed on commercially available upper surface and carries ruthenium-oxide heating layer 5 with 2 discrete L-shaped gold electrodes 1, lower surface
Insulation Al2O3The upper surface of ceramic wafer 4, and make sensitive material that L-shaped gold electrode 1 be completely covered, the then hot pressing 3 at 100 DEG C
Minute, form 10~30 μm of sensitive material film 3.
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 is calcined 2 hours at 400 DEG C, finally welds above-mentioned device
It connects and encapsulates, to obtain Al2O3/α-Fe2O3Oxide semiconductor triethylamine sensor.
Embodiment 2
With the mass ratio of silicon source and source of iron for 0.25：1 Al2O3/α-Fe2O3Composite nano fiber sensitive material makes flat
Board-like triethylamine sensor, specific manufacturing process：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5mL N-N dimethylformamides, are stirred
Obtain solution A within 3 hours；By 0.10g aluminium isopropoxides, 0.5g polyacrylonitrile is dissolved in 5 mL N-N dimethylformamides, water-bath
70 DEG C of heating stirrings obtain solution B in 3 hours, and later, solution A is poured into solution B, continue stirring 1 hour after obtaining mixed liquor
Obtain the precursor liquid of spinning.
2) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Collect that apply voltage between plate be 9.5 ± 1kV, collects plate earthing, after spinning about 3 hours, a nanometer Electrospun production is obtained on collecting board
Object；
3) above-mentioned nanometer Electrospun product is calcined at 500 DEG C and obtains within 2 hours di-iron trioxide nanotube sensitive material,
The sensitive material is placed on commercially available upper surface and carries ruthenium-oxide heating layer 5 with 2 discrete L-shaped gold electrodes 1, lower surface
Insulation Al2O3The upper surface of ceramic wafer 4, and make sensitive material that L-shaped gold electrode 1 be completely covered, the then hot pressing 3 at 100 DEG C
Minute, form 10~30 μm of sensitive material film 3.
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 is calcined 2 hours at 400 DEG C, finally welds above-mentioned device
It connects and encapsulates, to obtain Al2O3/α-Fe2O3Oxide semiconductor triethylamine sensor.
Embodiment 3
With the mass ratio of silicon source and source of iron for 0.375：1 Al2O3/α-Fe2O3Composite nano fiber sensitive material makes flat
Board-like triethylamine sensor, specific manufacturing process：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5mL N-N dimethylformamides, are stirred
Obtain solution A within 3 hours；By 0.15g aluminium isopropoxides, 0.5g polyacrylonitrile is dissolved in 5 mL N-N dimethylformamides, water-bath
70 DEG C of heating stirrings obtain solution B in 3 hours, and later, solution A is poured into solution B, continue stirring 1 hour after obtaining mixed liquor
Obtain the precursor liquid of spinning.
2) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Collect that apply voltage between plate be 9.5 ± 1kV, collects plate earthing, after spinning about 3 hours, a nanometer Electrospun production is obtained on collecting board
Object；
3) above-mentioned nanometer Electrospun product is calcined at 500 DEG C and obtains within 2 hours di-iron trioxide nanotube sensitive material,
The sensitive material is placed on commercially available upper surface and carries ruthenium-oxide heating layer 5 with 2 discrete L-shaped gold electrodes 1, lower surface
Insulation Al2O3The upper surface of ceramic wafer 4, and make sensitive material that L-shaped gold electrode 1 be completely covered, the then hot pressing 3 at 100 DEG C
Minute, form 10~30 μm of sensitive material film 3.
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 is calcined 2 hours at 400 DEG C, finally welds above-mentioned device
It connects and encapsulates, to obtain Al2O3/α-Fe2O3Oxide semiconductor triethylamine sensor.
Claims (3)
1. one kind is with Al2O3/α-Fe2O3Composite nano fiber is the triethylamine sensor of sensitive electrode material, is flat knot
Structure, by upper surface band, there are two the Al that discrete L-shaped gold electrode (1), lower surface carry ruthenium-oxide heating layer (5)2O3Insulating ceramics
Plate (4) and semiconductor sensitive material film (3) composition, wherein there are two discrete rectangles for ruthenium-oxide heating layer (5) lower surface band
Gold electrode (6)；Semiconductor sensitive material film (3) is prepared in two discrete L-shaped gold electrodes (1) and Al2O3Insulated ceramic plates
(4) upper surface；It is characterized in that：Semiconductor sensitive material is Al2O3/α-Fe2O3Composite nano fiber, silicon source and source of iron
Mass ratio 0.125~0.375：1.
2. one kind described in claim 1 is with Al2O3/α-Fe2O3Composite nano fiber is that the triethylamine of sensitive electrode material senses
The preparation method of device, its step are as follows：
1) 0.4g ferric acetyl acetonades, 0.5g polyvinylpyrrolidones are dissolved in 5~10mL N-N dimethylformamides, are stirred
Obtain solution A within 2~5 hours；The aluminium isopropoxide of 0.05~0.15g, 0.5g polyacrylonitrile are dissolved in 5~10mL N-N dimethyl
In formamide, heating stirring obtains solution B in 2~5 hours under 60~80 DEG C of water-baths, later pours into solution B solution A, obtains
Continue stirring after mixed liquor 0.5~3 hour；
2) above-mentioned solution is fitted into electrostatic spinning apparatus, carries out Electrospun, a nanometer Electrospun product is obtained on collecting board；
3) above-mentioned nanometer Electrospun product is calcined 1~3 hour at 450~550 DEG C and obtains Al2O3/α-Fe2O3Composite Nano is fine
Sensitive material is tieed up, it is aerobic with 2 discrete L-shaped gold electrodes 1, lower surface bands which is placed on commercially available upper surface
Change ruthenium heating layer 5 and carries the insulation Al of 2 discrete rectangle gold electrodes 6 in 5 lower surface of ruthenium-oxide heating layer2O3Ceramic wafer 4
Upper surface, and make sensitive material that L-shaped gold electrode 1 be completely covered, then hot pressing 2~6 minutes at 80~120 DEG C, form 10~
The conductor oxidate sensitive material film 3 of 30 μ m-thicks；
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 calcines 1~3 hour at 350~450 DEG C, finally by above-mentioned device into
Row welding and encapsulation, to obtain with Al2O3/α-Fe2O3Composite nano fiber is the triethylamine sensor of sensitive electrode material.
3. one kind as claimed in claim 2 is with Al2O3/α-Fe2O3Composite nano fiber is that the triethylamine of sensitive electrode material passes
The preparation method of sensor, it is characterised in that：In electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 10~20cm, spinneret
The voltage applied between mouth and collecting board is 5~15kV, collects plate earthing, and spinning obtains nanometer electricity on collecting board after 2~5 hours
Spinning product.
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Cited By (1)
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| CN113125519A (en) * | 2021-04-19 | 2021-07-16 | 江南大学 | In2O3/α-Fe2O3Nanowire, triethylamine sensor and preparation method thereof |
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Application publication date: 20180810 |