CN115259156B - Can detect low concentration NO at room temperature2Gas-sensitive component and preparation method thereof - Google Patents
Can detect low concentration NO at room temperature2Gas-sensitive component and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 84
- 239000002131 composite material Substances 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 55
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 46
- 230000004044 response Effects 0.000 claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 37
- 239000000843 powder Substances 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001514 detection method Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 229910020808 NaBF Inorganic materials 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000010335 hydrothermal treatment Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 113
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 abstract description 13
- 239000001301 oxygen Substances 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 9
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 3
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- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 206010006451 bronchitis Diseases 0.000 description 1
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- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
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- 229910021389 graphene Inorganic materials 0.000 description 1
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- 238000010952 in-situ formation Methods 0.000 description 1
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- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- C01G23/043—Titanium sub-oxides
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- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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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
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Abstract
The invention relates to a gas-sensitive element capable of detecting low-concentration NO 2 at room temperature and a preparation method thereof. The preparation method comprises the following steps: (1) Synthesizing a plurality of layers of Ti 3C2 MXene; (2) Synthesizing TiO 2/Ti3C2; (3) Synthesizing TiO 2‑x/Ti3C2; and (4) manufacturing the gas-sensitive component. The invention aims to solve the problem of poor gas sensitivity of the existing MXene-based material, the preparation method is simple and convenient in process and low in cost, tiO 2 in the TiO 2‑x/Ti3C2 composite material prepared by the method has a special high-energy high-activity {001} crystal face and rich oxygen vacancies, the composite material has a Schottky heterostructure, and the response (delta R/R a) of the composite material to 10ppmNO 2 at room temperature is respectively as high as 4.6, which is far higher than that of the existing MXene-based gas-sensitive material. In addition, tiO 2‑x/Ti3C2 also has good cyclic response. The invention provides an effective method for constructing the MOS/MXene gas sensitive material with special crystal face and rich oxygen vacancy, and further promotes the development of gas sensitive technology.
Description
Technical Field
The invention relates to a preparation method of a gas-sensitive material in the field of gas concentration detection, in particular to a preparation method of a gas-sensitive material for detecting low concentration NO 2 at room temperature, a preparation method for preparing corresponding gas-sensitive components by using the gas-sensitive material, a gas-sensitive component prepared by using the preparation method of the gas-sensitive component, a room temperature NO 2 gas sensor formed by packaging the gas-sensitive component, and a detection method for detecting low concentration NO 2 at room temperature by using the gas-sensitive component or the room temperature NO 2 gas sensor.
Background
The development of chemical and automotive industries has resulted in the increasingly serious environmental pollution of fossil fuels used in large quantities, which has been a major problem worldwide. The large amount of greenhouse gas emissions can cause global warming of the atmosphere, which constitutes a great threat to the environment. Harmful gases mainly emitted by the combustion of coal and petroleum products also bring serious smog to the earth. Air pollution factors therefore require extensive human attention, rapid analysis, effective control and proper handling. Among various air-polluted gases, nitrogen dioxide (NO 2) is one of typical byproducts of fossil fuel combustion and automobile exhaust emissions. NO 2 is a volatile and irritating noxious smell that causes not only many environmental problems such as photochemical smog and acid rain, but also respiratory diseases such as bronchitis and pulmonary edema, and in severe cases, death. Therefore, it is important and urgent to develop a low-cost, high-sensitivity NO 2 gas sensor material.
Disclosure of Invention
The invention aims at solving the technical problems that the working temperature of the existing TiO 2 gas-sensitive material is high and the response of the Ti 3C2 gas-sensitive material is low, and discloses a preparation method of the gas-sensitive material for detecting low-concentration NO 2 at room temperature, a preparation method of corresponding gas-sensitive components by using the gas-sensitive material, the gas-sensitive components prepared by using the preparation method of the gas-sensitive components, a room-temperature NO 2 gas sensor formed by packaging the gas-sensitive components, and a detection method of detecting low-concentration NO 2 at room temperature by using the gas-sensitive components or the room-temperature NO 2 gas sensor.
The invention is realized by adopting the following technical scheme: a method for producing a gas-sensitive material capable of detecting NO 2 at low concentration at room temperature, the gas-sensitive material comprising a plurality of layers of Ti 3C2 MXene, the method comprising the steps of:
(1) Multilayer Ti 3C2 MXene was synthesized: uniformly dispersing Ti 3AlC2 powder in HF at a ratio of 1g Ti 3AlC2 powder to 15mLHF, stirring at 35deg.C, cleaning, and drying to obtain multilayer Ti 3C2 MXene.
As a further improvement of the above scheme, mechanical stirring was carried out at 35℃for 4h.
As a further improvement of the above scheme, the gas-sensitive material further comprises a TiO 2/Ti3C2 composite, and the preparation method of the gas-sensitive material further comprises the following steps:
(2) Synthesizing a TiO 2/Ti3C2 composite material: slowly adding the multilayer Ti 3C2 MXene powder into deionized water to form a suspension at a ratio of 0.3g of multilayer Ti 3C2 MXene powder to 0.5g of NaBF 4 to 3.87mL of HCl, adding NaBF 4 and HCl into the suspension, stirring, and transferring into a polytetrafluoroethylene autoclave for hydrothermal treatment at 160 ℃ to obtain the TiO 2/Ti3C2 composite material.
Preferably, after stirring for 1h, the mixture is transferred into a polytetrafluoroethylene autoclave and treated for 12h at 160 ℃.
Preferably, the gas-sensitive material further comprises a TiO 2-x/Ti3C2 composite material, and the preparation method of the gas-sensitive material further comprises the following steps:
(3) Synthesizing a TiO 2-x/Ti3C2 composite material: and (3) annealing the TiO 2/Ti3C2 powder in a flowing dry Ar+10%H 2 atmosphere, wherein the heating rate is 10 ℃ and min -1, and the annealing temperature is 400 ℃, so as to obtain the TiO 2-x/Ti3C2 composite material.
Still more preferably, the TiO 2/Ti3C2 powder is placed in a tube furnace and annealed for 2 hours under a flow-dried ar+10% h 2 atmosphere.
The invention also provides a preparation method of the gas-sensitive element capable of detecting the low-concentration NO 2 at room temperature, which comprises the following steps:
Selecting one composite material from the multi-layer Ti 3C2MXene、TiO2/Ti3C2 composite material and the TiO 2-x/Ti3C2 composite material; wherein, the multi-layer Ti 3C2 MXene prepared by the preparation method of any gas-sensitive material capable of detecting low concentration NO 2 at room temperature is a TiO 2/Ti3C2 composite material prepared by the preparation method of any gas-sensitive material capable of detecting low concentration NO 2 at room temperature, and the TiO 2-x/Ti3C2 composite material prepared by the preparation method of any gas-sensitive material capable of detecting low concentration NO 2 at room temperature is a TiO 2-x/Ti3C2 composite material prepared by the preparation method of any gas-sensitive material capable of detecting low concentration NO 2 at room temperature;
Dispersing the selected composite material in ethanol at a ratio of 0.05g of the selected composite material to 0.1mL of ethanol, dripping the selected composite material on Pt interdigital electrodes on an alumina substrate, and drying to obtain the gas-sensitive component of the corresponding composite material.
The invention also provides a gas sensor capable of detecting low-concentration NO 2 at room temperature, which is a multilayer Ti 3C2 MXene gas sensor, a TiO 2/Ti3C2 gas sensor or a TiO 2-x/Ti3C2 gas sensor prepared by adopting the preparation method of the gas sensor capable of detecting low-concentration NO 2 at room temperature.
The invention also provides a room temperature NO 2 gas sensor which is formed by packaging the gas-sensitive component capable of detecting low-concentration NO 2 at room temperature.
The invention also provides a detection method for detecting the low-concentration NO 2 at room temperature, which comprises the following steps:
The gas-sensitive component capable of detecting low-concentration NO 2 at room temperature or the room temperature NO 2 gas sensor is adopted, the room temperature is controlled to be 25+/-2 ℃, the substrate coated with the gas-sensitive material is exposed to NO 2 and then air is introduced, and the resistance R g of the coated substrate exposed to the gas and the resistance R a of the coated substrate in the air are recorded;
The gas response resistance is calculated from the resistance R g and the resistance R a: r= (R g-Ra)/Ra.
Compared with the existing gas sensitive material, the invention has the advantages that (1) the TiO 2 {001} crystal face has high surface energy and reaction activity and can provide more active oxygen adsorption sites; (2) Unpaired electrons and unsaturated coordination atoms generated by oxygen vacancies become electron aggregation centers, and provide effective channels for transferring electrons from the composite material to adsorbed gas molecules, thereby improving the sensitivity to NO 2; (3) The schottky heterojunction between TiO 2-x/Ti3C2 helps to accelerate charge transfer and separation.
The method comprises the following steps:
(1) For example, literature ,"J.Choi,et al.,In situ formation of multiple Schottky barriers in a Ti3C2MXene film and its application in highly sensitive gas sensors,Adv.Funct.Mater.30(2020)2003998." prepared a TiO 2 modified Ti 3C2 monolith by solution oxidation, and achieved about 0.05 and 0.16 response to 0.5 and 5ppm NO 2, respectively, at room temperature. Compared with the invention, besides the different materials of the matrix (single-layer Ti 3C2 MXene), the in-situ grown TiO 2 has different morphologies, does not have a special crystal face, and does not form rich oxygen vacancies.
(2) For example, in document ,"H.L.Tai,et al.,Enhanced ammonia response of Ti3C2Txnanosheets supported by TiO2 nanoparticles at room temperature,Sens.Actuators B Chem.298(2019)12687.", a TiO 2 is sprayed on an interdigital electrode, and then a single layer of Ti 3C2 is sprayed on a TiO 2 film to prepare a TiO 2/Ti3C2 double-layer film, and the result shows that the double-layer film has a response value of 0.03 to 10ppm of ammonia gas at room temperature. Compared with the invention, besides the difference of the materials of the matrix (single-layer Ti 3C2 MXene), the preparation method is different, the obtained materials are also different (not TiO 2/Ti3C2 composite material but double-layer film), and the sprayed TiO 2 has no special crystal face and oxygen vacancies.
(3) For example, literature ,"T.T.He,et al.,MXene/SnO2 heterojunction based chemical gas sensors,Sens.Actuators B Chem.329(2021)129275." prepares a MXene/SnO 2 composite by hydrothermally growing SnO 2 particles on a multilayer Ti 3C2 MXene, having a response of 0.02 to 0.5ppm ammonia at room temperature. Compared with the invention, snO 2 has no abundant oxygen vacancies except for loading different metal oxides.
In summary, the present invention, in comparison with the above-mentioned document, forms in situ a flaky TiO 2 having a {001} crystal plane on a multi-layered Ti 3C2 MXene by a hydrothermal method in addition to a base material, and then anneals to make TiO 2 have abundant oxygen vacancies. The {001} crystal face of anatase TiO 2 has higher surface energy and reactivity than other surfaces, so that the anatase TiO 2 has more active oxygen adsorption sites, unpaired electrons and unsaturated coordination atoms generated by oxygen vacancies can also provide more active sites for absorbing target gas, tiO 2 can form a Schottky heterojunction with metallic matrix material Ti 3C2, and the synergistic effect can accelerate electron transmission, so that the sensitivity to NO 2 is improved, and therefore, the ppb-level NO 2 can be detected at room temperature. This is not the case in the above-mentioned documents.
Drawings
Fig. 1 is a flow chart of a detection method for detecting low concentration NO 2 at room temperature according to example 1 of the present invention.
Fig. 2 is a surface scanning electron micrograph of the Ti 3C2,TiO2/Ti3C2 and TiO 2-x/Ti3C2 composite used in fig. 1 with high sensitivity room temperature detection NO 2.
FIG. 3 is an X-ray diffraction pattern of the Ti 3C2,TiO2/Ti3C2 and TiO 2-x/Ti3C2 composite material of high sensitivity room temperature detection NO 2 employed in FIG. 1.
FIG. 4 is a plot of the response of the Ti 3C2,TiO2/Ti3C2 and TiO 2-x/Ti3C2 composite of high sensitivity room temperature detection NO 2 employed in FIG. 1 versus 10ppmNO 2.
FIG. 5 is an EPR curve of the TiO 2-x/Ti3C2 composite material of FIG. 1 for high sensitivity room temperature detection NO 2.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It is noted that when an element is referred to as being "mounted to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "secured to" another element, it can be directly secured to the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "or/and" as used herein includes any and all combinations of one or more of the associated listed items.
Example 1:
Fig. 1 is a flow chart of a detection method for detecting low concentration NO 2 at room temperature according to an embodiment of the invention. The detection method for detecting the low-concentration NO 2 at room temperature comprises the following steps:
Adopting a gas-sensitive component capable of detecting low-concentration NO 2 at room temperature or a gas sensor capable of detecting NO 2 at room temperature, controlling the room temperature to 25+/-2 ℃, exposing a substrate coated with a gas-sensitive material to NO 2, then introducing air, and recording the resistance R g of the substrate coated with the gas and the resistance R a of the substrate coated with the gas;
The gas response resistance is calculated from the resistance R g and the resistance R a: r= (R g-Ra)/Ra.
The room temperature detection NO 2 gas sensor in the step can be formed by packaging the gas sensitive component. The gas sensor can be a multilayer Ti 3C2 MXene gas sensor or a TiO 2/Ti3C2 gas sensor or a TiO 2-x/Ti3C2 gas sensor prepared by a preparation method of the gas sensor capable of detecting low-concentration NO 2 at room temperature.
The preparation method of the gas sensor capable of detecting the low concentration NO 2 at room temperature can comprise the following steps:
Selecting one composite material from the multi-layer Ti 3C2MXene、TiO2/Ti3C2 composite material and the TiO 2-x/Ti3C2 composite material; wherein, the multi-layer Ti 3C2 MXene prepared by the preparation method of the gas sensitive material capable of detecting low concentration NO 2 at room temperature, the TiO 2/Ti3C2 composite material prepared by the preparation method of the gas sensitive material capable of detecting low concentration NO 2 at room temperature and the TiO 2-x/Ti3C2 composite material prepared by the preparation method of the gas sensitive material capable of detecting low concentration NO 2 at room temperature;
Dispersing the selected composite material in ethanol at a ratio of 0.05g of the selected composite material to 0.1mL of ethanol, dripping the selected composite material on Pt interdigital electrodes on an alumina substrate, and drying to obtain the gas-sensitive component of the corresponding composite material.
The preparation method of the gas-sensitive material capable of detecting low-concentration NO 2 at room temperature can comprise a multi-layer Ti 3C2 MXene、TiO2/Ti3C2 composite material and a TiO 2-x/Ti3C2 composite material.
The preparation method of the gas-sensitive material comprises the following steps:
(1) Multilayer Ti 3C2 MXene was synthesized: uniformly dispersing Ti 3AlC2 powder in HF at a ratio of 1g Ti 3AlC2 powder to 15mLHF, stirring at 35deg.C, cleaning, and drying to obtain multilayer Ti 3C2 MXene. Wherein the mixture was mechanically stirred at 35℃for 4h.
Ti 3C2 MXene is commonly used to fabricate room temperature gas sensitive materials due to good electrical conductivity and the rich functionality created by HF etching. The signal-to-noise ratio of Ti 3C2 MXene is 2 orders of magnitude higher than that of other two-dimensional materials (e.g., reduced graphene oxide, black phosphorus, and MoS 2). In addition, the experimental and theoretical limits for detecting VOC gases at room temperature for Ti 3C2 MXene are also minimal compared to other two-dimensional materials. And Ti 3C2 MXene can also be used as a substrate material for anchoring MOS to enhance the sensing performance.
(2) Synthesizing a TiO 2/Ti3C2 composite material: slowly adding the multilayer Ti 3C2 MXene powder into deionized water to form a suspension at a ratio of 0.3g of multilayer Ti 3C2 MXene powder to 0.5g of NaBF 4 to 3.87mL of HCl, adding NaBF 4 and HCl into the suspension, stirring, and transferring into a polytetrafluoroethylene autoclave for hydrothermal treatment at 160 ℃ to obtain the TiO 2/Ti3C2 composite material. Wherein, stirring for 1h, transferring into a polytetrafluoroethylene autoclave, and carrying out hydrothermal treatment at 160 ℃ for 12h.
(3) Synthesizing a TiO 2-x/Ti3C2 composite material: and (3) annealing the TiO 2/Ti3C2 powder in a flowing dry Ar+10%H 2 atmosphere, wherein the heating rate is 10 ℃ and min -1, and the annealing temperature is 400 ℃, so as to obtain the TiO 2-x/Ti3C2 composite material. Wherein the TiO 2/Ti3C2 powder was placed in a tube furnace and annealed for 1h under a flow-dried ar+10% h 2 atmosphere.
Example 2:
(1) Synthesis of multilayer Ti 3C2 MXene: uniformly dispersing 1g of Ti 3AlC2 powder in 15mLHF, mechanically stirring for 4 hours at 35 ℃, and cleaning and drying to obtain a multilayer Ti 3C2 MXene;
(2) And (3) manufacturing a gas-sensitive component: to prepare Ti 3C2 gas sensitive components, 0.05g Ti 3C2 powder was dispersed in 0.1mL ethanol, dropped onto Pt interdigital electrodes on an alumina substrate, dried, and then the response and recovery characteristics of the gas sensitive material to target gas were recorded using a dynamic four-channel gas sensitive test system (SD 101). The test temperature was controlled at 25.+ -. 2 ℃ and after exposing the substrate coated with the gas sensitive material to NO 2, air was vented and the resistance of the coated substrate exposed to the gas (R g) and the resistance in air (R a) were recorded. The gas response is calculated by the formula r= (R g-Ra)/Ra.
To analyze the morphology and performance of Ti 3C2, the Ti 3C2 powder had a unique accordion multilayer structure as shown in region a in fig. 2, and the XRD characteristic of Ti 3C2 is also shown in fig. 3. As shown in region a of FIG. 4, the response of Ti 3C2 to 10ppm NO 2 is 0.16.
Example 3:
(1) Synthesis of multilayer Ti 3C2 MXene: uniformly dispersing 1g of Ti 3AlC2 powder in 15mL of HF, mechanically stirring for 4 hours at 35 ℃, and cleaning and drying to obtain a multilayer Ti 3C2 MXene;
(2) Synthesis of TiO 2/Ti3C2: slowly adding 0.3g of multilayer Ti 3C2 powder into deionized water, adding 0.5g of NaBF 4 and 3.87mL of HCl into the suspension, stirring for 1h, transferring into a 100mL polytetrafluoroethylene autoclave, and carrying out hydrothermal treatment at 160 ℃ for 12h to obtain TiO 2/Ti3C2;
(3) And (3) manufacturing a gas-sensitive component: in order to prepare the TiO 2/Ti3C2 gas-sensitive component, 0.05g of TiO 2/Ti3C2 composite material is dispersed in 0.1mL of ethanol and is dripped on a Pt interdigital electrode on an alumina substrate, and after drying, the response and recovery characteristics of the gas-sensitive material to target gas are recorded by a dynamic four-channel gas-sensitive test system (SD 101). The test temperature was controlled at 25.+ -. 2 ℃ and after exposing the substrate coated with the gas sensitive material to NO 2, air was vented and the resistance of the coated substrate exposed to the gas (R g) and the resistance in air (R a) were recorded. The gas response is calculated by the formula r= (R g-Ra)/Ra.
To analyze the morphology and performance of TiO 2/Ti3C2, flaky TiO 2 particles were uniformly grown on the multi-layered Ti 3C2 as shown in region b in fig. 2, and XRD also showed the formation of TiO 2 as shown in fig. 3. As shown in region b of fig. 4, the TiO 2/Ti3C2 has a response to 10ppm NO 2 of 2.6 and good cyclicity.
Example 4:
(1) Synthesis of multilayer Ti 3C2 MXene: uniformly dispersing 1g of Ti 3AlC2 powder in 15mL of HF, mechanically stirring for 4 hours at 35 ℃, and cleaning and drying to obtain a multilayer Ti 3C2 MXene;
(2) Synthesis of TiO 2/Ti3C2: slowly adding 0.3g of multilayer Ti 3C2 powder into deionized water, adding 0.5g of NaBF 4 and 3.87mL of HCl into the suspension, stirring for 1h, transferring into a 100mL polytetrafluoroethylene autoclave, and carrying out hydrothermal treatment at 160 ℃ for 12h to obtain TiO 2/Ti3C2;
(3) TiO 2-x/Ti3C2 synthesis: placing TiO 2/Ti3C2 powder in a tube furnace, and annealing for 1h in a flowing dry Ar+10% H 2 atmosphere at a heating rate of 10 ℃ and min -1 and an annealing temperature of 400 ℃ to obtain a TiO 2-x/Ti3C2 composite material;
(4) And (3) manufacturing a gas-sensitive component: in order to prepare the TiO 2-x/Ti3C2 gas-sensitive component, 0.05g of TiO 2-x/Ti3C2 composite material is dispersed in 0.1mL of ethanol and is dripped on a Pt interdigital electrode on an alumina substrate, and after drying, the response and recovery characteristics of the gas-sensitive material to target gas are recorded by a dynamic four-channel gas-sensitive test system (SD 101). The test temperature was controlled at 25.+ -. 2 ℃ and after exposing the substrate coated with the gas sensitive material to NO 2, air was vented and the resistance of the coated substrate exposed to the gas (R g) and the resistance in air (R a) were recorded. The gas response is calculated by the formula r= (R g-Ra)/Ra.
To analyze the morphology and performance of TiO 2-x/Ti3C2, the morphology of TiO 2-x/Ti3C2 is similar to TiO 2/Ti3C2 as shown in region c in fig. 2. As shown in fig. 5, analysis of the EPR spectrum of TiO 2-x/Ti3C2 revealed that TiO 2-x/Ti3C2 developed a distinct paramagnetic signal at g= 1.9878, indicating that TiO 2-x/Ti3C2 had a rich oxygen vacancy. As shown in region c of fig. 4, the response of TiO 2-x/Ti3C2 to 10ppm NO 2 is 4.6, indicating that TiO 2-x/Ti3C2 has a highly sensitive response to NO 2 at room temperature.
As can be seen from a combination of the above examples 2, 3, 4: the invention relates to the technical field of a gas sensor for detecting NO 2 at room temperature, and particularly can be applied to high-efficiency detection of NO 2 at room temperature. The preparation method comprises the following steps: (1) Synthesizing a plurality of layers of Ti 3C2 MXene; (2) Synthesizing TiO 2/Ti3C2; (3) Synthesizing TiO 2-x/Ti3C2; and (4) manufacturing the gas-sensitive component. The invention aims to solve the problem of poor gas sensitivity of the existing MXene-based material, the preparation method is simple and convenient in process and low in cost, tiO 2 in the TiO 2-x/Ti3C2 composite material prepared by the method has a special high-energy high-activity {001} crystal face and rich oxygen vacancies, the composite material has a Schottky heterostructure, and the response (delta R/R a) of the composite material to 10ppmNO 2 at room temperature is respectively as high as 4.6, which is far higher than that of the existing MXene-based gas-sensitive material. In addition, tiO 2-x/Ti3C2 also has good cyclic response. The invention provides an effective method for constructing the MOS/MXene gas sensitive material with special crystal face and rich oxygen vacancy, and further promotes the development of gas sensitive technology.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of the invention should be assessed as that of the appended claims.
Claims (7)
1. A preparation method of a gas-sensitive material capable of detecting low-concentration NO 2 at room temperature is characterized by comprising the following steps: the gas-sensitive material comprises a multi-layer Ti 3C2MXene、TiO2/Ti3C2 composite material and a TiO 2-x/Ti3C2 composite material, and the preparation method of the gas-sensitive material comprises the following steps:
(1) Multilayer Ti 3C2 MXene was synthesized: uniformly dispersing Ti 3AlC2 powder in HF at a ratio of 1gTi 3AlC2 powder to 15mLHF, stirring at 35 ℃, and cleaning and drying to obtain multilayer Ti 3C2 Mxene;
(2) Synthesizing a TiO 2/Ti3C2 composite material: slowly adding the multilayer Ti 3C2 MXene powder into deionized water to form a suspension according to the ratio of 0.3 g multilayer Ti 3C2 MXene powder to 0.5g NaBF 4 to 3.87 mL HCl, adding NaBF 4 and HCl into the suspension, stirring, and transferring into a polytetrafluoroethylene autoclave for hydrothermal treatment at 160 ℃ to obtain a TiO 2/Ti3C2 composite material; wherein, stirring for 1h, transferring into a polytetrafluoroethylene autoclave, and carrying out hydrothermal treatment at 160 ℃ for 12 h;
(3) Synthesizing a TiO 2-x/Ti3C2 composite material: and (3) annealing the TiO 2/Ti3C2 powder in a flowing dry Ar+10%H 2 atmosphere, wherein the heating rate is 10 ℃ and min -1, and the annealing temperature is 400 ℃, so as to obtain the TiO 2-x/Ti3C2 composite material.
2. The method for producing a gas-sensitive material capable of detecting NO 2 at low concentration at room temperature according to claim 1, characterized by mechanically stirring for 4 hours at 35 ℃.
3. The method for producing a gas-sensitive material capable of detecting NO 2 at low concentration at room temperature according to claim 1, wherein TiO 2/Ti3C2 powder is placed in a tube furnace and annealed 2h under a flow-dried ar+10% h 2 atmosphere.
4. The preparation method of the gas-sensitive component capable of detecting low-concentration NO 2 at room temperature is characterized by comprising the following steps of:
Selecting one composite material from the multi-layer Ti 3C2MXene、TiO2/Ti3C2 composite material and the TiO 2-x/Ti3C2 composite material; wherein, the multi-layer Ti 3C2 MXene prepared by the preparation method of the gas-sensitive material capable of detecting low concentration NO 2 at room temperature according to claim 1 or 2, the TiO 2/Ti3C2 composite prepared by the preparation method of the gas-sensitive material capable of detecting low concentration NO 2 at room temperature according to claim 1 and the TiO 2-x/Ti3C2 composite prepared by the preparation method of the gas-sensitive material capable of detecting low concentration NO 2 at room temperature according to claim 1;
Dispersing the selected composite material in ethanol at a ratio of 0.05g of ethanol of 0.1: 0.1 mL, dripping the mixture on Pt interdigital electrodes on an alumina substrate, and drying to obtain the gas-sensitive component of the corresponding composite material.
5. A gas sensor capable of detecting low concentration NO 2 at room temperature, which is characterized in that the gas sensor is a multilayer Ti 3C2 MXene gas sensor, a TiO 2/Ti3C2 gas sensor or a TiO 2-x/Ti3C2 gas sensor prepared by the method for preparing the gas sensor capable of detecting low concentration NO 2 at room temperature according to claim 4.
6. A room temperature NO 2 gas sensor, which is characterized in that it is packaged by a gas sensitive component capable of detecting low concentration NO 2 at room temperature according to claim 5.
7. A detection method for detecting low concentration NO 2 at room temperature, characterized by comprising the steps of:
A gas-sensitive element capable of detecting low-concentration NO 2 at room temperature or a room temperature NO 2 gas sensor as claimed in claim 6 is adopted, the room temperature is controlled to be 25+/-2 ℃, the substrate coated with the gas-sensitive material is exposed to NO 2 and then air is introduced, and the resistance R g of the substrate coated with the gas and the resistance R a of the substrate coated with the gas are recorded;
The gas response resistance is calculated from the resistance R g and the resistance R a: r= (R g-Ra)/Ra.
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