CN112268937B - Based on perovskite Cs2PdBr6Carbon monoxide sensor of nano hollow sphere and preparation method and application thereof - Google Patents
Based on perovskite Cs2PdBr6Carbon monoxide sensor of nano hollow sphere and preparation method and application thereof Download PDFInfo
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- CN112268937B CN112268937B CN202011105376.0A CN202011105376A CN112268937B CN 112268937 B CN112268937 B CN 112268937B CN 202011105376 A CN202011105376 A CN 202011105376A CN 112268937 B CN112268937 B CN 112268937B
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 13
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 3
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 3
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 3
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 claims description 3
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 230000001680 brushing effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 6
- 230000004044 response Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000007603 infrared drying Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses a perovskite-based Cs2PdBr6A carbon monoxide sensor of a nano hollow sphere, a preparation method and application thereof. Specifically, the carbon monoxide sensor comprises a membrane material and an interdigital electrode, wherein the membrane material is perovskite Cs2PdBr6The nano hollow ball is coated on the interdigital electrode in a brushing way, and the thickness of the nano hollow ball is 10-100 mu m. The carbon monoxide sensor has the following advantages: the preparation is convenient and fast, and the operation is simple; very low concentrations of carbon monoxide (50 ppb) can be detected; the device performance is more stable.
Description
Technical Field
The invention belongs to the technical field of organic semiconductor materials, and particularly relates to a perovskite-based Cs2PdBr6A carbon monoxide sensor of a nano hollow sphere, a preparation method thereof and application thereof in environmental carbon monoxide detection.
Background
In the everyday life environment, the exhaust gases of automobiles and portable generators, as well as the incomplete combustion of some fuels (including wood, coal, oil, natural gas and waste), all produce carbon monoxide. Carbon monoxide is a colorless and odorless gas, and even causes human death when the concentration in the air reaches a certain limit, so the detection of carbon monoxide is particularly important. At present, a carbon monoxide sensor is a hotspot in many research directions in the field of sensing devices, and common carbon monoxide sensing devices are basically based on metal oxide materials, and although the carbon monoxide sensing devices have good stability, the carbon monoxide sensing devices have poor responsiveness, high detection limit and complex preparation process, and cannot be applied to large-scale application. In order to meet the requirements of the current market on the aspects of low price, practicability, easy preparation and the like of the sensor, a novel carbon monoxide sensor needs to be developed urgently.
Disclosure of Invention
In view of the above, the present invention employs perovskite Cs2PdBr6The carbon monoxide sensor is prepared by nano hollow spheres, and carbon monoxide with different concentrations is detected by observing the current change of the sensor under different carbon monoxide concentrations. The invention tests the current change of the carbon monoxide sensor under carbon monoxide with different concentrations and the recovery of the device, firstly the device is placed in a pure nitrogen environment to test the current of the device, and then the content of the carbon monoxide in the environment is continuously increased to test the current of the device.
Specifically, the invention adopts the following technical scheme:
perovskite Cs2PdBr6The application of the nano hollow sphere in preparing a carbon monoxide sensor; or perovskite Cs2PdBr6The application of the nano hollow sphere in preparing a carbon monoxide sensor membrane material.
Based on perovskite Cs2PdBr6The carbon monoxide sensor of the nano hollow sphere comprises a membrane material and an interdigital electrode; the membrane material is perovskite Cs2PdBr6A nano hollow sphere layer.
Above perovskite-based Cs2PdBr6The preparation method of the carbon monoxide sensor of the nano hollow sphere comprises the following steps: perovskite Cs2PdBr6Coating the nano hollow ball solution on the interdigital electrode, heating, and preparing the perovskite-based Cs2PdBr6Carbon monoxide sensor of nanometer hollow sphere.
The carbon monoxide sensor comprises a membrane material and an interdigital electrode; the thickness of the membrane material is 10-100 mu m; the interdigital electrode is made of aluminum oxide (Al)2O3) Providing a substrate on which a silver-palladium alloy (Ag-Pd) is disposed; the width of an interdigital of the interdigital electrode is 200-300 mu m, and the distance between the interdigital electrodes is 100-200 mu m; the thickness of the substrate is 1-2 mm; the thickness of the silver-palladium alloy is 100-200 nm.
In the present invention, perovskite Cs2PdBr6Stirring the solvent and tertiary butanol to obtain the perovskite Cs2PdBr6The preferable stirring speed of the nano hollow ball is 800-3000 rpm; perovskite Cs2PdBr6The dosage ratio of the solvent to the tertiary butanol is 150-200 mg: 1 mL: 10mL, preferably 160 mg: 1 mL: 10 mL; the solvent is a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide, and preferably the N, N-dimethylformamide and the dimethyl sulfoxide are mixed according to the volume ratio of 1: 1. In the present invention, perovskite Cs2PdBr6Heating the mixture with a solvent, and then stirring the mixture with tert-butyl alcohol, wherein the heating temperature is 40-70 ℃, the heating time is 1-3 min, and the preferred temperature is 50 ℃, and the heating time is 2 min.
In the invention, the temperature of the heating and drying device is 70-100 ℃ for 4-6 min, and the preferred temperature is 90 ℃ for 5 min.
In the invention, cesium bromide and palladium bromide are heated and reacted in hydrogen bromide solution to prepare perovskite Cs2PdBr6And a non-hollow structure.
Above perovskite-based Cs2PdBr6The carbon monoxide sensor of the nano hollow sphere is applied to detecting carbon monoxide.
In particular, based on perovskite Cs2PdBr6The preparation method of the carbon monoxide sensor comprises the following steps:
(1) ultrasonically cleaning the finger-inserted electrode with deionized water and ethanol for 10min respectively, and drying;
(2) perovskite Cs2PdBr6Dissolving in 1mL of solvent, and heating at 40-60 ℃ for 2min to obtain a solution I;
(3) adding 200 mL of the first solution into 10mL of tert-butyl alcohol, stirring for 30 min, and standing for 12 h to obtain a second solution;
(4) adding the solution IICoating the layer precipitation solution on the surface of the interdigital electrode, and heating to obtain the perovskite-based Cs2PdBr6Carbon monoxide sensor of hollow sphere of nanometer.
Compared with the prior art, the invention using the technical scheme has the following advantages:
(1) the device is convenient to prepare and simple to operate;
(2) the detection limit is low, and the lowest detection concentration of carbon monoxide is lower than that of common metal oxides;
(3) the device performance is stable.
Drawings
FIG. 1 shows perovskite Cs2PdBr6SEM spectrum of (d).
FIG. 2 shows perovskite Cs2PdBr6XRD spectrum of (1).
FIG. 3 shows perovskite Cs2PdBr6SEM spectrogram of the nanometer hollow sphere.
FIG. 4 shows perovskite Cs2PdBr6TEM spectrum of nano hollow sphere.
FIG. 5 shows perovskite Cs2PdBr6XRD spectrogram of the nano hollow sphere.
FIG. 6 shows perovskite-based Cs2PdBr6The structure of the carbon monoxide sensor of the nano hollow sphere is shown schematically.
FIG. 7 shows Cs2PdBr6The response of the carbon monoxide sensor is plotted as a function of carbon monoxide concentration.
FIG. 8 shows perovskite Cs2PdBr6The structure is schematic.
Detailed Description
The technical solution of the present invention will be further explained with reference to the accompanying drawings and specific embodiments. Unless otherwise indicated, reagents, materials, instruments and the like used in the following examples are commercially available; unless otherwise specified, the parameters, environments of the examples are conventional; the substrate and the finger electrode are all existing products.
Example 1: perovskite Cs2PdBr6Synthesis of (2) and preparation of the sensor
(1) Perovskite Cs2PdBr6The synthesis of (2):
cesium bromide (4.2562 g, 20 mmol) and palladium bromide (2.6623 g, 10 mmol) were weighed and placed in hydrogen bromide solution (10 mL), heated at 85 ℃ and reacted with stirring for 10 min; then adding 1mL of dimethyl sulfoxide at 120 ℃, and stirring for 10 min; closing the heating table, cooling to room temperature, performing suction filtration on the product, washing with water and toluene, and drying in a vacuum oven at 100 ℃ for 10h to obtain the perovskite Cs product2PdBr6The SEM microstructure of the non-hollow structure is shown in figure 1, and the X-ray diffraction pattern of the non-hollow structure is shown in figure 2. As can be seen from FIG. 1, Cs2PdBr6Is relatively uniform octahedral small particles; the structure is schematically shown in figure 8.
As can be seen from FIG. 2, the above-synthesized Cs2PdBr6And standard Cs2PdBr6 The PDF cards completely correspond to each other, and the success of the synthesis can be determined.
(2) Perovskite Cs2PdBr6Synthesis of a nano hollow ball and preparation of a sensor:
(a) ultrasonically cleaning the finger-inserted electrode with deionized water and ethanol for 10min respectively, and drying; the length of the inserting fingers is 7 mm, the width of the inserting fingers is 0.2 mm, and the distance between the inserting fingers is 0.2 mm;
(b) mixing the above perovskite Cs2PdBr6Dissolving in 1 mLN, N-dimethylformamide and dimethyl sulfoxide in a volume ratio of 1: 1, heating the mixed solvent at 50 ℃ for 2min to obtain a solution I;
(c) adding 200 mL of the first solution into 10mL of tert-butyl alcohol, and stirring at 1500rpm for 30 min to obtain perovskite Cs2PdBr6And (4) nano hollow spheres. The SEM microstructure is shown in FIG. 3, the TEM microstructure is shown in FIG. 4, and the X-ray diffraction pattern is shown in FIG. 5.
As can be seen from FIG. 3, Cs2PdBr6Converted into small balls with rough surfaces and relatively uniform sizes;
as can be seen from FIG. 4, the above-synthesized Cs2PdBr6The pellet has a hollow structure.
As can be seen from FIG. 5, the above combinationFormed Cs2PdBr6Hollow pellets with standard Cs2PdBr6 The PDF cards completely correspond to each other, and the fact that phase change does not occur while the appearance is changed can be determined.
(d) Standing the solution for 12 hours to obtain a solution II;
(e) brushing the solution II lower layer precipitation solution on the surface of the interdigital electrode, and heating by an infrared drying lamp to obtain the perovskite Cs-based electrode2PdBr6A carbon monoxide sensor of a nano hollow sphere; the sensor is schematically shown in FIG. 6, wherein Cs is2PdBr6The film thickness was 30 μm.
Example 2: response determination experiment of carbon monoxide sensor in different carbon monoxide concentration environments
Perovskite-based Cs prepared in example 12PdBr6The carbon monoxide sensor with the nano hollow sphere is placed in a testing machine, under the condition of applying 1V constant voltage, the response of a testing device is changed within the range of 50 ppb-50 ppm, and the result is shown in figure 7.
As can be seen from FIG. 7, Cs-based atmosphere (diluted with nitrogen) was used for different concentrations of carbon monoxide2PdBr6The sensor response of the nano hollow sphere is obvious; the lowest detection limit can reach 50 ppb, and the method can be used for detecting carbon monoxide gas.
Example with "CN 2019111446042" perovskite-based Cs2PdBr6The same carbon monoxide test as above was carried out on the sensor (0.2% oleic acid), starting from 50 ppb, up to 5ppm, with poor response and no possibility of carbon monoxide gas detection.
In summary, the invention provides a perovskite Cs2PdBr6The resistance-type film sensor with simple structure is manufactured by the nano hollow ball, the detection of carbon monoxide with different concentrations is realized, the minimum detection limit can reach 50 ppb, the application of perovskite in the field of carbon monoxide sensing is realized, and the invention is based on the perovskite Cs2PdBr6The carbon monoxide sensor has high application value for detecting the carbon monoxide in the future environment.
Claims (11)
1. Perovskite Cs2PdBr6The application of the nano hollow sphere in preparing a carbon monoxide sensor.
2. The use of claim 1, wherein the carbon monoxide sensor comprises a membrane material and interdigitated electrodes; the thickness of the membrane material is 10-100 mu m.
3. Perovskite Cs2PdBr6The application of the nano hollow sphere in preparing a carbon monoxide sensor membrane material; the thickness of the membrane material is 10-100 mu m.
4. Use according to claim 2 or 3, wherein the perovskite Cs2PdBr6Stirring the solvent and tertiary butanol to obtain the perovskite Cs2PdBr6A nano hollow sphere; the solvent is a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide; when the membrane material is prepared, the heating temperature is 40-70 ℃, and the time is 1-3 min.
5. Based on perovskite Cs2PdBr6The carbon monoxide sensor of the nano hollow sphere comprises a membrane material and an interdigital electrode; the membrane material is perovskite Cs2PdBr6A nano hollow sphere layer.
6. The perovskite-based Cs of claim 52PdBr6Carbon monoxide sensor of nanometer hollow sphere, its characterized in that: the interdigital electrode takes alumina as a substrate, and silver-palladium alloy is arranged on the substrate; the thickness of the membrane material is 10-100 mu m.
7. The perovskite-based Cs of claim 52PdBr6The preparation method of the carbon monoxide sensor of the nano hollow sphere is characterized by comprising the following steps: perovskite Cs2PdBr6Coating the nano hollow ball solution on the interdigital electrode, heating, and preparing the baseIn perovskite Cs2PdBr6The carbon monoxide sensor of (1).
8. The perovskite-based Cs of claim 72PdBr6The preparation method of the carbon monoxide sensor of the nano hollow sphere is characterized in that perovskite Cs is added2PdBr6Stirring the solvent and tertiary butanol to obtain the perovskite Cs2PdBr6A nano hollow sphere; the heating temperature is 40-70 ℃, and the time is 1-3 min.
9. The perovskite-based Cs of claim 82PdBr6The preparation method of the carbon monoxide sensor of the nano hollow sphere is characterized in that the solvent is a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide.
10. The perovskite-based Cs of claim 72PdBr6The preparation method of the carbon monoxide sensor of the nano hollow sphere is characterized by comprising the following steps: dissolving cesium bromide and palladium bromide in a hydrogen bromide solution for heating reaction to prepare perovskite Cs2PdBr6。
11. The perovskite-based Cs of claim 52PdBr6The use of a carbon monoxide sensor according to (3) in the detection of carbon monoxide.
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