CN108802114A - With Pt-ZnO-In2O3Composite nano fiber is acetone sensor, the preparation method and applications of sensitive material - Google Patents
With Pt-ZnO-In2O3Composite nano fiber is acetone sensor, the preparation method and applications of sensitive material Download PDFInfo
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Abstract
One kind is with Pt-ZnO-In2O3Composite nano fiber is the acetone sensor, preparation method and its application in atmospheric environment in terms of detection acetone steam of sensitive material, belongs to gas sensor technical field.Sensor carries the Al of 2 discrete rectangle gold electrodes by front with 2 discrete L-shaped gold electrodes, the back side with ruthenium-oxide heating layer and in ruthenium-oxide heating layer surface2O3Insulated ceramic plates are coated in L-shaped gold electrode and Al2O3The positive Pt-ZnO-In of insulated ceramic plates2O3Composite nano fiber sensitive material film forms.The size for the platinum grain that the method obtains makes the sensitivity of the sensor based on such sensitive material significantly be promoted in 3nm or so, the superpower catalytic action of extra granular platinum.Meanwhile Pt-ZnO-In2O3The acetone sensor that composite nano fiber sensitive material makes has very low detection offline in acetone, can reach 0.5ppm.
Description
Technical field
The invention belongs to gas sensor technical fields, and in particular to one kind is with Pt-ZnO-In2O3Composite nano fiber is
Acetone sensor, preparation method and its application in atmospheric environment in terms of detection acetone steam of sensitive material.
Background technology
The today grown rapidly is industrialized, air quality problems receive the domestic and unprecedented concern of international community, part
Family and public place have begun to use air purification and monitoring device, regardless of be administered from source air pollution again or
Improve air quality, gas sensor all plays essential role wherein.Wherein semiconductor-type gas sensor because
It is at low cost, flexibility is high, has great development potentiality using simple.
In fact, deepening constantly always around the research for improving acetone sensor.Especially nanoscale science and technology
Develop into improve sensor performance provide good opportunity.Studies have shown that by using noble metal to metal oxide into
When row doping or modification, since noble metal has very strong catalytic action, sensitive material can be significantly increased
Gas-sensitive property.And in general, the nano-scale of noble metal granule is smaller, and the catalytic action played is stronger, to air-sensitive spy
The promotion amplitude of property is bigger.Based on this point, designing and preparing for the material of noble metal-oxide system of extra granular is studied,
There is highly important scientific meaning for the application of enlargement gas sensor.
Invention content
The object of the present invention is to provide a kind of Pt-ZnO-In prepared based on electrostatic spinning technique2O3Composite nano fiber is
Acetone sensor, preparation method and its application in atmospheric environment in terms of detection acetone steam of sensitive electrode material.This hair
The bright metal platinum particles by using super-small are to semi-conducting material In2O3It is modified, and then improves the air-sensitive of sensitive material
Characteristic increases the sensitivity of sensor, promotes such sensor in the functionization of field of gas detection.
The obtained sensor of the present invention also has the rapid response time other than with higher sensitivity.The biography
The Monitoring lower-cut of sensor is 0.5ppm, can be used for the detection of acetone steam content in atmospheric environment.
As shown in Figure 1, of the present invention with Pt-ZnO-In2O3Composite nano fiber is that the acetone sensor of sensitive material is
Plate armature, it is that there are two discrete L-shaped gold electrode 1 and 1 ', lower surfaces to carry ruthenium-oxide heating layer 5 by upper surface band
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 and 6 '；Semiconductor sensitive material film 3 is prepared in two discrete L-shaped gold electrodes and Al2O3Insulating ceramics
The upper surface of plate 4；Each L-shaped gold electrode 1 and 1 ' is respectively welded with a platinum line 21 and 21 ', each 6 He of rectangle gold electrode
6 ' are all respectively welded with a platinum line 22 and 22 ', can be measured between two L-shaped gold electrodes 1 and 1 ' by two platinum lines 21 and 21 '
Resistance, by two platinum lines 22 and 22 ' can to ruthenium-oxide heating layer 5 apply electric current, give Al2O3Insulated ceramic plates 4 are added
Heat is so as to controlling the operating temperature of gas sensor；It is characterized in that：Sensitive material is Pt-ZnO-In2O3Composite Nano
Fiber sensitive material, and it is prepared by following steps,
1) 1~3mmol zinc nitrate hexahydrates are dissolved in 20~30mL absolute methanols and obtain solution A；By 7~9mmol
2-methylimidazole be dissolved in 20~30mL absolute methanols and obtain solution B, later, solution A is poured into solution B, is mixed
Close liquid after continue 20~40min of stirring, solution is then aged 20~30h at room temperature, finally with absolute ethyl alcohol to solution into
Row centrifuge washing, by being dried to obtain product ZIF-8；
2) 60~90mg ZIF-8 are dispersed in 4~6mL deionized waters, then disperse the ammonium chloroplatinate of 6~10mg
In above-mentioned solution, 1~3h is stirred, then toward the sodium borohydride aqueous solution general of 6~10mL of addition, concentration 1.5mg/mL in solution
Platinum ion restores, and finally carries out centrifuge washing with absolute ethyl alcohol, product Pt@ZIF-8 are obtained after dry；
3) the Pt@ZIF-8 of 20~50mg is taken to be dispersed in 8~12mL N-N dimethylformamides, after stirring 3~6 min,
0.3~0.6g nitric hydrate indiums are added in toward above-mentioned solution, continue 3~6min of stirring, then toward being added 1.2~1.6g's in solution
Polyvinylpyrrolidone, mixed solution continue 4~6h of stirring；
4) 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 15~20kV, collects plate earthing, a nanometer Electrospun is obtained on collecting board after 2~5h of spinning
Product；Nanometer Electrospun product is calcined into 1~3h at 450~550 DEG C, to obtain Pt-ZnO-In2O3Composite nano fiber
Sensitive material.
One kind of the present invention is with Pt-ZnO-In2O3Composite nano fiber is the preparation of the acetone sensor of sensitive material
Method, its step are as follows：
1) by Pt-ZnO-In2O3Composite nano fiber sensitive material is placed on commercially available upper surface and carries 2 discrete L-shaped
Gold electrode 1 and 1 ', lower surface are with ruthenium-oxide heating layer 5 and on 5 surface of ruthenium-oxide heating layer with 2 discrete rectangle gold electricity
The Al of pole 6 and 6 '2O3The upper surface of insulated ceramic plates 4, and make sensitive material that L-shaped gold electrode 1 and 1 ' be completely covered, then 80
2~6min of hot pressing at~120 DEG C forms 10~30 μm thick of conductor oxidate sensitive material film 3；Al2O3Insulating ceramics
A length of 1.3~1.7mm, the width of plate are 0.8~1.3mm, thickness is 0.1~0.25mm；
2) the insulation Al for obtaining step 1)2O3Ceramic wafer 4 calcines 1~3h at 350~450 DEG C, finally by above-mentioned device into
Row welding and encapsulation, it is of the present invention with Pt-ZnO-In to obtain2O3Composite nano fiber is that the acetone of sensitive material passes
Sensor.
Advantages of the present invention：
(1) sensor utilizes common N-type semiconductor material In2O3, it has good chemical stability；
(2) metal platinum particles are fixed on ZIF-8, the platinum grain of super-small can be obtained, size is in~3nm；
The superpower catalytic action of extra granular platinum makes the sensitivity of the sensor based on such sensitive material significantly be promoted；
(3) with Pt-ZnO-In2O3Composite nano fiber is the sensor of sensitive material in 175~325 DEG C of test temperature,
Response to 100ppm acetone is 57.1, is not reported both at home and abroad.
Description of the drawings
Fig. 1:Based on Pt-ZnO-In2O3The acetone sensor structural schematic diagram of composite nano fiber sensitive material；
Fig. 1 (a) is sensor surface structure schematic diagram；
Fig. 1 (b) is sensor lower surface configuration schematic diagram；
Fig. 2：The phenogram for the ZIF-8 and Pt@ZIF-8 that the present invention synthesizes；
The XRD diagram of the ZIF-8 of Fig. 2 (a) ZIF-8, Pt@ZIF-8 and document report；
The SEM of Fig. 2 (b) ZIF-8 schemes；
The SEM of Fig. 2 (c) Pt@ZIF-8 schemes；
The TEM of Fig. 2 (d) Pt@ZIF-8 schemes；
Fig. 3：The XRD diagram of sensitive material prepared by comparative example 1, comparative example 2 and embodiment 1；
Fig. 4：The SEM figures of sensitive material prepared by comparative example 1, comparative example 2 and embodiment 1；
Fig. 5：Sensor prepared by comparative example 1, comparative example 2 and embodiment 1 is in different operating temperature to 100ppm acetone
Sensitivity comparison curve；
Fig. 6：When the temperature most preferably tested, sensitivity curve of the embodiment 1 to various concentration acetone.
As shown in Figure 1, the names of the parts are：L-shaped gold electrode 1 and 1 ', platinum line 21,21 ', 22 and 22 ', semiconductor sensitivity material
Material 3, Al2O3Insulated ceramic plates 4, ruthenium-oxide heating layer 5, rectangle gold electrode 6 and 6 '.
From the ZIF- for the XRD and document report that can be seen that ZIF-8 the and Pt@ZIF-8 synthesized in experiment in Fig. 2 (a)
Diffraction maximums all 8 XRD all match, and do not see the presence of the relevant peaks of platinum, this is seldom related with the amount of the platinum of addition
System.Fig. 2 (b) and (c) are respectively the SEM characterizations of ZIF-8 and Pt@ZIF-8, it can be seen that the consistent appearance of the two, by pair
Consistent appearance than and with ZIF-8 reported in the literature, it was demonstrated that the addition of platinum does not influence the structure of ZIF-8.Fig. 2 (d)
It is characterized for the TEM of Pt@ZIF-8, it will be seen that there is black particle of some sizes in 3nm or so to be evenly distributed in
On ZIF-8, by the numerical value of the interplanar distance of interior illustration it is found that the particle of these black is exactly metal platinum.
Fig. 3 (a) is the XRD diagram of sensitive material prepared by comparative example 1, comparative example 2 and embodiment 1, it can be seen that all
Peak all with In2O3Characteristic peak matches, and is not found the presence of the relevant peaks of ZnO and Pt, equally, this also with the Pt of addition
ZIF-8 (ZIF-8) measures rare relationship.
Fig. 4 (a)-(b) corresponds respectively to the SEM figures of 2 two samples of comparative example 1 and comparative example, and Fig. 4 (c)-(d) is to implement
The SEM of 1 sample of example schemes.It can be seen from the figure that the fibre diameter of three obtained sample is all in 90 rans, and shape
Looks do not change significantly.Illustrate that Pt@ZIF-8 (ZIF-8) particle is with the particle studded in fibre of Pt@ZnO (ZnO) after sintering
The inside of dimension and the size of particle and In2O3Granular size is almost the same.
Fig. 5 is the sensitivity of comparative example 1, comparative example 2 and 1 sensor of embodiment in different operating temperature to 100ppm acetone
Correlation curve.It can be seen from the figure that the optimum working temperature of all devices is all 300 DEG C.At a temperature of this, comparative example 1 and right
Device made by 2 sample of ratio is respectively 6.60 and 9.72 to the sensitivity of 100ppm acetone, made by 1 sample of embodiment
Device is in 300 DEG C of sensitivity highests to 100ppm acetone, value 57.1.
Fig. 6 is sensitivity curve of 1 sensor of embodiment to the acetone of various concentration in the temperature most preferably tested.I
It can be seen that this sensor have apparent response to the acetone of 0.5ppm for 300 DEG C in optimum temperature.
Specific implementation mode
Comparative example 1
With pure In2O3Fiber makes acetone sensor, specific manufacturing process as sensitive material：
1) 0.5g nitric hydrate indiums are dissolved in 10mL N-N dimethylformamides, stir 5min, then toward in solution plus
Enter the polyvinylpyrrolidone of 1.3677g, mixed solution continues to stir 5h；
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 the voltage applied between plate as 18kV, collects plate earthing, a nanometer Electrospun product is obtained on collecting board after spinning 3h；
3) above-mentioned nanometer Electrospun product is calcined into 2h at 500 DEG C and obtains pure In2O3Fiber sensitive material, by the sensitivity
Material be placed on commercially available upper surface with 2 discrete L-shaped gold electrodes 1 and 1 ', lower surface with ruthenium-oxide heating layer 5 and
5 surface of ruthenium-oxide heating layer carries the insulation Al of 2 discrete rectangle gold electrodes 6 and 6 '2O3The upper surface of ceramic wafer 4, and make quick
L-shaped gold electrode 1 is completely covered in sense material, then the hot pressing 3min at 100 DEG C, and the conductor oxidate for forming 20 μ m-thicks is sensitive
Material film 3；A length of 1.5mm, width 1.0mm, the thickness 0.1mm of ceramic wafer；
4) the insulation Al for obtaining step 3)2O3Ceramic wafer 4 calcines 2h at 400 DEG C, finally by above-mentioned device carry out welding and
Encapsulation, to obtain being based on pure In2O3Fiber is the acetone sensor of sensitive material.
Comparative example 2
With ZnO-In2O3Composite fibre makes acetone sensor, specific manufacturing process as sensitive material：
1) 2mmol zinc nitrate hexahydrates are dissolved in 25mL absolute methanols and obtain solution A；By the 2- methyl miaows of 8 mmol
Azoles, which is dissolved in 25mL absolute methanols, obtains solution B, and later, solution A is poured into solution B, continues to stir after obtaining mixed liquor
Solution is then aged for 24 hours, finally centrifuge washing is carried out to solution with absolute ethyl alcohol, by being dried to obtain by 30min at room temperature
Product ZIF-8；
2) ZIF-8 of 40mg is taken to be dispersed in 10mL N-N dimethylformamides, stir 5min after, toward above-mentioned solution in add
Enter 0.5g nitric hydrate indiums, continue to stir 5min, then toward the polyvinylpyrrolidone that 1.3677g is added in solution, mixed solution
Continue to stir 5h；
3) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Integrate the voltage applied between plate as 18kV, collects plate earthing, a nanometer Electrospun product is obtained on collecting board after spinning 3h；
4) above-mentioned nanometer Electrospun product is calcined into 2h at 400 DEG C and obtains ZnO-In2O3Composite nano fiber sensitivity material
The sensitive material is placed on commercially available upper surface and carries ruthenium-oxide with 2 discrete L-shaped gold electrodes 1 and 1 ', lower surface by material
Heating layer 5 and 5 surface of ruthenium-oxide heating layer carry 2 discrete rectangle gold electrodes 6 and 6 ' insulation Al2O3Ceramic wafer 4
Upper surface, and make sensitive material that L-shaped gold electrode 1 be completely covered, then the hot pressing 3min at 100 DEG C, forms partly leading for 20 μ m-thicks
Oxide body sensitive material film 3；A length of 1.5mm, width 1.0mm, the thickness 0.1mm of ceramic wafer；
5) the insulation Al for obtaining step 4)2O3Ceramic wafer 4 calcines 2h at 400 DEG C, finally by above-mentioned device carry out welding and
Encapsulation, to obtain with ZnO-In2O3Composite fibre is the acetone sensor of sensitive material.
Embodiment 1
With Pt-ZnO-In2O3Composite fibre makes acetone sensor, specific manufacturing process as sensitive material：
1) 2mmol zinc nitrate hexahydrates are dissolved in 25mL absolute methanols and obtain solution A；By the 2- methyl miaows of 8 mmol
Azoles, which is dissolved in 25mL absolute methanols, obtains solution B, and later, solution A is poured into solution B, continues to stir after obtaining mixed liquor
Solution is then aged for 24 hours, finally centrifuge washing is carried out to solution with absolute ethyl alcohol, by being dried to obtain by 30min at room temperature
Product ZIF-8；
2) 80mg ZIF-8 are dispersed in 5mL deionized waters, the ammonium chloroplatinate of 8mg are then dispersed in above-mentioned solution,
2h is stirred, is then restored platinum ion toward sodium borohydride (1.5mg/mL) aqueous solution of addition 8mL in solution, finally, use is anhydrous
Ethyl alcohol carries out centrifuge washing, and dries in an oven, and product Pt@ZIF-8 are obtained after production is dry；
3) the Pt ZIF-8 of 40mg are taken to be dispersed in 10mL N-N dimethylformamides, after stirring 5min, toward above-mentioned solution
In 0.5g nitric hydrate indiums are added, continue to stir 5min, then toward the polyvinylpyrrolidone that 1.3677g is added in solution, mixing
Solution continues to stir 5h；
4) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 15cm, spinning nozzle and receipts
Integrate the voltage applied between plate as 18kV, collects plate earthing, a nanometer Electrospun product is obtained on collecting board after spinning 3h；
5) above-mentioned nanometer Electrospun product is calcined into 2h at 400 DEG C and obtains Pt-ZnO-In2O3Composite nano fiber is sensitive
It is aerobic with 2 discrete L-shaped gold electrodes 1 and 1 ', lower surface bands to be placed on commercially available upper surface by material for the sensitive material
Change ruthenium heating layer 5 and carries the insulation Al of 2 discrete rectangle gold electrodes 6 and 6 ' on 5 surface of ruthenium-oxide heating layer2O3Ceramic wafer 4
Upper surface, and make sensitive material that L-shaped gold electrode 1 and 1 ' be completely covered, then the hot pressing 3min at 100 DEG C, form 20 μ m-thicks
Conductor oxidate sensitive material film 3；A length of 1.5mm, width 1.0mm, the thickness 0.10mm of ceramic wafer；
6) the insulation Al for obtaining step 5)2O3Ceramic wafer 4 calcines 2h at 400 DEG C, finally by above-mentioned device carry out welding and
Encapsulation, it is of the present invention with Pt-ZnO-In to obtain2O3Composite nano fiber is the acetone sensor of sensitive material.
Claims (3)
1. one kind is with Pt-ZnO-In2O3Composite nano fiber is the acetone sensor of sensitive material, is plate armature, by upper table
There are two the Al that discrete L-shaped gold electrode (1 and 1 '), lower surface carry ruthenium-oxide heating layer (5) for face band2O3Insulated ceramic plates (4)
It is formed with semiconductor sensitive material film (3)；Wherein there are two discrete rectangle gold electrodes for ruthenium-oxide heating layer (5) lower surface band
(6 and 6 '), semiconductor sensitive material film (3) are prepared in two discrete L-shaped gold electrodes (1 and 1 ') and Al2O3Insulated ceramic plates
(4) upper surface；It is characterized in that：Sensitive material is Pt-ZnO-In2O3Composite nano fiber sensitive material, and it is by walking as follows
Suddenly it is prepared,
1) 1~3mmol zinc nitrate hexahydrates are dissolved in 20~30mL absolute methanols and obtain solution A；By the 2- of 7~9mmol
Methylimidazole, which is dissolved in 20~30mL absolute methanols, obtains solution B, and later, solution A is poured into solution B, obtains mixed liquor
After continue 20~40min of stirring, solution is then aged 20~30h at room temperature, finally with absolute ethyl alcohol to solution carry out from
The heart washs, by being dried to obtain product ZIF-8；
2) 60~90mg ZIF-8 are dispersed in 4~6mL deionized waters, are then dispersed in the ammonium chloroplatinate of 6~10mg
It states solution, stirs 1~3h, then toward the sodium borohydride aqueous solution of 6~10mL, concentration 1.5mg/mL is added in solution by platinum ion
Reduction finally carries out centrifuge washing with absolute ethyl alcohol, product Pt@ZIF-8 is obtained after dry；
3) the Pt@ZIF-8 of 20~50mg are taken to be dispersed in 8~12mL N-N dimethylformamides, after stirring 3~6min, up
Addition 0.3~0.6g nitric hydrate indiums in solution are stated, 3~6min of stirring, then the poly- second toward 1.2~1.6g of addition in solution are continued
Alkene pyrrolidone, mixed solution continue 4~6h of stirring；
4) above-mentioned solution is fitted into electrostatic spinning apparatus, the distance of collecting board and spinning nozzle is 10~20cm, spinning nozzle and receipts
The voltage applied between collection plate is 15~20kV, collects plate earthing, obtains a nanometer Electrospun production after 2~5h of spinning on collecting board
Object；Nanometer Electrospun product is calcined into 1~3h at 450~550 DEG C, to obtain Pt-ZnO-In2O3Composite nano fiber is quick
Feel material.
2. one kind described in claim 1 is with Pt-ZnO-In2O3Composite nano fiber is the system of the acetone sensor of sensitive material
Preparation Method, its step are as follows：
1) by Pt-ZnO-In2O3Composite nano fiber sensitive material is placed on Al2O3The upper surface of insulated ceramic plates 4, and make sensitivity
L-shaped gold electrode (1 and 1 ') is completely covered in material, then 2~6min of hot pressing at 80~120 DEG C, forms the half of 10~30 μ m-thicks
Conducting oxide sensitive material film (3)；
2) the insulation Al for obtaining step 1)2O3Ceramic wafer (4) calcines 1~3h at 350~450 DEG C, finally carries out above-mentioned device
Welding and encapsulation, to obtain with Pt-ZnO-In2O3Composite nano fiber is the acetone sensor of sensitive material.
3. one kind described in claim 1 is with Pt-ZnO-In2O3Composite nano fiber is the acetone sensor of sensitive material big
The application in terms of acetone steam is detected in compression ring border.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109459470A (en) * | 2018-11-27 | 2019-03-12 | 中国石油大学(华东) | Palladium/cobaltosic oxide-the graphene film sensitive to extremely low concentration acetone under a kind of lower temperature |
| CN114703659A (en) * | 2022-03-14 | 2022-07-05 | 陕西师范大学 | Pt/In2O3-xComposite nanofiber material and preparation method and application thereof |
-
2018
- 2018-05-31 CN CN201810544727.4A patent/CN108802114A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| LANLAN GUO ET AL.: "Ultra-sensitive sensing platform based on Pt-ZnO-In2O3 nanofibers for detection of acetone", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109459470A (en) * | 2018-11-27 | 2019-03-12 | 中国石油大学(华东) | Palladium/cobaltosic oxide-the graphene film sensitive to extremely low concentration acetone under a kind of lower temperature |
| CN114703659A (en) * | 2022-03-14 | 2022-07-05 | 陕西师范大学 | Pt/In2O3-xComposite nanofiber material and preparation method and application thereof |
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