CN115656055A - AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe and preparation method and application thereof - Google Patents
AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe and preparation method and application thereof Download PDFInfo
- Publication number
- CN115656055A CN115656055A CN202211372091.2A CN202211372091A CN115656055A CN 115656055 A CN115656055 A CN 115656055A CN 202211372091 A CN202211372091 A CN 202211372091A CN 115656055 A CN115656055 A CN 115656055A
- Authority
- CN
- China
- Prior art keywords
- mxene
- aunps
- pmma
- tfbg
- sensing probe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920003229 poly(methyl methacrylate) Polymers 0.000 title claims abstract description 52
- 239000000523 sample Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims description 16
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 34
- 230000008313 sensitization Effects 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 239000013307 optical fiber Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 230000001235 sensitizing effect Effects 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 238000006722 reduction reaction Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002135 nanosheet Substances 0.000 claims description 7
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000009849 vacuum degassing Methods 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 230000005641 tunneling Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 16
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229940110676 inzo Drugs 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 medical diagnosis Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
Images
Abstract
The invention discloses an AuNPs/Ta 2 The sensor probe comprises a TFBG optical fiber and a composite sensitization sheet attached to the surface of the TFBG optical fiber, wherein the composite sensitization sheet is used for providing a sensing signal for the sensor probe; the composite sensitization plate comprises a PMMA matrix skeleton and Ta doped with AuNPs and dispersed in PMMA 2 C Mxene sensitizing material. AuNPs provide excellent localized surface plasmon enhancement and multilayer Ta 2 The C MXene material is characterized by a metal phase and stable properties, and the photoelectric properties of the MXene material can be adjusted by changing the number of layers or surface functional groups to adjust the direct band gap of the material. Most importantly, the rich oxygen-containing groups on the surface can realize NH 3 High selectivity of (2). Due to the introduction of the PMMA framework, a conduction path can be formed in the detection process due to the quantum tunneling effect, so that adjacent AuNPs/Ta 2 The distance between C MXene increases to increase contact resistance; moreover, the PMMA composite sensitization structure is very good in a thermal dissolution modeThe replacement is easy to realize, so that the detection performance and the utilization rate of the sensor are greatly increased, and the detection cost is saved.
Description
Technical Field
The invention belongs to the technical field of gas sensing, and particularly relates to AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe and preparation method and application thereof, based on AuNPs/Ta 2 The structure of the C MXene @ PMMA composite sensitization sheet can realize the high-identification detection analysis of ammonia molecules.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Ammonia gas is widely used in various fields including fertilizers, food processing, biochemical products, medical diagnosis, gunpowder and the like. It is also one of the most harmful environmental pollutants of common industrial production and manufacturing processes.
Surface Plasmon Resonance (SPR) -based tilted grating fiber optic sensors (TFBG) have a denser surface energy density due to their unique in-core refractive index periodic modulation and synergistic coupling reactions that excite Surface Plasmon Waves (SPWs). In addition, the optical fiber sensor has the advantages of high signal-to-noise ratio, electromagnetic interference resistance, small size and remote monitoring, and has ultrahigh sensitivity and narrow linear resolution which are not possessed by a leaky film optical fiber sensor.
However, the inventor finds that the sensitization structure in the field of fiber gas sensing is mostly metal oxide (SnO) 2 ，CdSnO 2 ，TiO 2 ，ZnO，RuO 2 And InzO 3 Etc.), p-n junction composites and low dimensionalMaterial (MoS) 2 Go, carbon nanotubes, etc.). It has the following problems: (1) Ammonia is a strong reducing agent and can continuously interfere with charge compensation of the sensitization layer; (2) The single sensitization structure can not meet the high detection standard of gas; (3) short sensor life and poor utilization.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe and preparation method and application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect, the present invention provides an AuNPs/Ta 2 The sensor probe comprises a TFBG optical fiber and a composite sensitization sheet attached to the surface of the TFBG optical fiber;
the composite sensitization plate comprises a PMMA matrix skeleton and Ta doped with AuNPs and dispersed in PMMA 2 A C Mxene sensitizing material;
ta doped with AuNPs 2 The mass percentage of the C Mxene sensitizing material in the composite sensitizing tablet is 5-30%.
In a second aspect, the present invention provides the AuNPs/Ta 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe comprises the following steps:
mixing Ta 2 Dispersing C-Mxene in water, collecting supernatant, centrifuging, and collecting precipitate to obtain Ta 2 A C-Mxene nanosheet;
chemical reduction of Ta 2 Doping AuNPs with C-Mxene nanosheets to obtain AuNPs/Ta 2 C Mxene；
Mixing AuNPs/Ta 2 Dispersing C Mxene in PMMA, performing ultrasonic treatment for a set time, adding an initiator, and blowing nitrogen;
heating the reaction mixture in water bath for reaction for a set time;
after vacuum degassing, pouring the mixture into a mould, and continuing polymerization reaction to obtain a composite sensitization sheet;
and (3) pasting the composite sensitization sheet on the surface of the TFBG optical fiber, and heating to obtain the sensing probe.
In a third aspect, the present invention provides the AuNPs/Ta 2 Application of a C MXene @ PMMA/TFBG sensing probe in detection of ammonia gas.
The beneficial effects achieved by one or more of the embodiments of the invention described above are as follows:
AuNPs/Ta of the invention 2 In the C MXene @ PMMA/TFBG gas sensing probe, the sensitization structure takes PMMA as a framework, and Ta doped with AuNPs is uniformly distributed in the PMMA as the framework 2 C MXene material.
AuNPs provide excellent localized surface plasmon enhancement and multilayer Ta 2 The C MXene material is characterized by a metal phase and stable properties, and the photoelectric characteristics of the MXene material can be adjusted by changing the number of layers or surface functional groups to adjust the direct band gap of the material. Most importantly, the rich surface oxygen-containing groups can realize NH 3 High selectivity of (2).
On one hand, due to the introduction of the PMMA framework, a conduction path can be formed in the detection process due to the quantum tunneling effect, so that adjacent AuNPs/Ta 2 The distance between C MXene increases to increase contact resistance; on the other hand, the PMMA composite sensitization structure is easy to replace by a thermal dissolution mode, so that the detection performance and the utilization rate of the sensor are greatly increased, and the detection cost is saved. Opens up a new road for the field of gas sensing.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to illustrate an exemplary embodiment of the invention and not to limit the invention.
FIG. 1 is AuNPs/Ta of an embodiment of the present invention 2 A flow chart of preparation and analysis test of the C MXene @ PMMA/TFBG sensor;
FIG. 2 is a diagram of a local area structure and a detection optical path of a TFBG sensor of an embodiment of the invention;
FIG. 3 is AuNPs/Ta of an embodiment of the present invention 2 The detection of the C MXene @ PMMA/TFBG sensor for ammonia gas, methane and hydrogen sulfide gas is compared.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. 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.
In a first aspect, the present invention provides an AuNPs/Ta 2 The sensor probe comprises a TFBG optical fiber and a composite sensitization sheet attached to the surface of the TFBG optical fiber;
the composite sensitization plate comprises a PMMA matrix skeleton and Ta doped with AuNPs and dispersed in PMMA 2 A C Mxene sensitizing material;
ta doped with AuNPs 2 The mass percentage of the C Mxene sensitizing material in the composite sensitizing tablet is 5-30%.
In some embodiments, ta of AuNPs is doped 2 The mass percentage of the C Mxene sensitizing material in the composite sensitizing tablet is 7-20%. E.g. Ta doped with AuNPs 2 The mass percentage of the C Mxene sensitizer may be 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%.
In some embodiments, the thickness of the composite sensitization sheet is 2.5-3 μm.
In a second aspect, the present invention provides the AuNPs/Ta 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe comprises the following steps:
mixing Ta 2 Dispersing C-Mxene in water, collecting supernatant, centrifuging, and collecting precipitate to obtain Ta 2 A C-Mxene nanosheet;
chemical reduction of Ta 2 Doping AuNPs with C-Mxene nanosheets to obtain AuNPs/Ta 2 C Mxene；
Mixing AuNPs/Ta 2 Dispersing C Mxene in PMMA, performing ultrasonic treatment for a set time, adding an initiator, and blowing nitrogen;
heating the reaction mixture in water bath for reaction for a set time;
vacuum degassing the mixture, pouring the mixture into a mold, and continuing polymerization reaction to obtain a composite sensitization sheet;
and (3) pasting the composite sensitization sheet on the surface of the TFBG optical fiber, and heating to obtain the sensing probe.
Polymethyl methacrylate (PMMA) needs to keep a dispersible liquid environment in a constant-heat environment, namely, water bath heating is performed to meet the environment (a magnetic rotor is arranged in the environment to enable the mixture to be fully stirred and mixed), so that the aim of ensuring that the mixture is more fully dispersed in the liquid environment to have a better response effect when subsequent plasmon resonance is ensured is achieved.
In some embodiments, the chemical reduction process is HAuCl 4 -3H 2 O and Ta 2 Mixed solution of C-MXene, under alkaline condition, in NaBH 4 Under the reduction action of (A) to realize the reaction of AuNPs to Ta 2 And doping of C-Mxene.
In some embodiments, the sonication time is between 0.5 and 1.5 hours. The ultrasonic treatment is used for treating AuNPs/Ta 2 C Mxene is well dispersed in PMMA.
In some embodiments, the initiator is Azobisisobutyronitrile (AIBN).
In some embodiments, the reaction mixture is heated in a water bath to react at a temperature of 65-80 ℃ for a period of 3-5 hours.
In some embodiments, the mixture is poured into a mold, and the polymerization is continued in a first stage and a second stage, wherein the first stage is to keep the mold containing the mixture in a water bath for 5-7h, and the temperature of the water bath is 65-75 ℃;
the second stage is to place the mold with the mixture inside hot blast furnace at 95-105 deg.c for 10-14 hr.
In some embodiments, after the compound sensitization tablet is pasted on the surface of the TFBG optical fiber, the temperature of the heating treatment is 75-85 ℃ and the time is 15-25min.
In a third aspect, the present invention provides the AuNPs/Ta 2 Application of a C MXene @ PMMA/TFBG sensing probe in detection of ammonia gas.
The present invention will be further described with reference to the following examples.
As shown in FIG. 1, auNPs/Ta 2 The preparation method of the C MXene @ PMMA/TFBG gas sensing probe comprises the following implementation steps:
1. preparation of TFBG optical fibers
The common single-mode optical fiber is arranged in the fixing frame, and the single-mode optical fiber needs to be preprocessed: remove 1.5cm of coating and wipe clean with alcohol. The parameters of the fiber core and the cladding are respectively as follows: diameter: 8.2 μm, refractive index of 1.45000 + -0.0025; cladding: 125 μm, and a refractive index of 1.4765. + -. 0.0025. The grating structure is manufactured under a phase mask technique, and 248nm ultraviolet light is irradiated to the surface of a bare optical fiber having a desired grating pattern through a mask. The parameters of the phase mask are as follows: center-to-center spacing =1099.05nm, mask length =10mm, mask height =15mm, substrate length =17.17mm, substrate height =25.4mm. And the modulation tilt angle of the grating is 12 deg.. And the laser operation frequency, voltage, energy, power and gas pressure are respectively 50Hz, 25kV, 160MJ, 7.92W and 3366mbar. To complete the bragg grating inscription, the polished section was exposed to uv light for 25 minutes. The prepared TFBG was left at 100 ℃ for 48 hours to remove hydrogen.
2、AuNPs/Ta 2 Synthesis of C MXene Structure
Mixing Ta 2 C-MXene (200 mg) was dispersed in 10mL deionized water at 500r min -1 Stirred for 5 hours. The dark green supernatant was centrifuged at 16000rpm for 30 minutes to collect the precipitate. The final product was then dispersed in 25mL of deionized water.
Chemical reduction of Ta 2 Decorating the C-MXene nanosheet with AuNPs. 60 μ L of HAuCl 4 -3H 2 O solution (0.1 g mL) -1 ) Added to 12mL of Ta 2 C-MXene(0.5mg mL -1 ) In solution, 0.16M NaBH, which will then be used as reducing agent under rapid stirring 4 And 1.6M NaOH (50. Mu.L) was added to the above solution. The mixture is stirred at 1000r min -1 Stirring for 30 minutes. The solution is washed by deionized water for three times and precipitates are collected, and the AuNPs/Ta is synthesized 2 C MXene material, au NPs diameter about 18-21nm.
3、AuNPs/Ta 2 Preparation of C MXene @ PMMA/TFBG sensor
100mg of AuNPs/Ta 2 C MXene was dispersed in PMMA (10 mL), sonicated in a glass reactor for 1 hour, then initiator AIBN (0.5 wt%) was added and nitrogen gas was blown into the system. The reaction mixture was heated in a water bath at 70 ℃ for 4 hours (the purpose of the water bath heating was to maintain a stable or stable environment, and the water bath heating was to place the mixture in a vial containing a magnetic rotor and stir it in a stable liquid environment sufficiently to allow the sensitizer to disperse well in the PMMA.
The mixture was degassed by vacuum and then poured into a mold consisting of two tempered glass plates and a rubber pad with a diameter of 3 mm. The mixture was allowed to stand at room temperature for 7 hours to complete the polymerization. Shaping AuNPs/Ta 2 Cutting C MXene @ PMMA film into 393μm 10000μm composite sensitization sheet (AuNPs/Ta) 2 C MXene content 10 wt%).
The tailored composite structure is pasted on the surface of the TFBG optical fiber and is heated constantly for 20 minutes at 80 ℃ on a heating platform so as to be better pasted, and the redundant position of the lamination is removed to ensure the uniformity of the sensitization structure.
4、AuNPs/Ta 2 Detection and analysis process of C MXene @ PMMA/TFBG sensor
First, auNPs/Ta 2 The C MXene @ PMMA/TFBG sensor probe was fixed in the detection light path as in FIG. 2, where the fixed gas chamber contained inlet and outlet facilities for gas. Before starting the measurement, the chamber needs to be evacuated with a rotary pump, the pressure inside the chamber is measured by a vacuum gauge connected to the chamber (which needs to be calibrated in advance), and the gas concentration is in ppm. A steel cylinder filled with pure ammonia gas is connected with the gas chamber through a steel pipe. For the measurement of the ammonia gradient (3 to 9 ppm) at the desired concentration to be detected, the chamber needs to be evacuated and then filled with the desired concentration of ammonia each time the gas is changed. Then, in the detection link, the polarization state of the light source is changed through the polarizer, and the AuNPs/Ta is adjusted through the polarization controller 2 The working state of the C MXene @ PMMA/TFBG sensor. Using lightThe spectrometer analyzes the detection performance of the sensor. The reference spectrum of the exhaust chamber was first calibrated and then the detected spectrum of ammonia gas was recorded for each concentration. The performance of the sensor was analyzed by the difference of the SPR reflection spectra, and the detection performance of the sensor is shown in fig. 3.
AuNPs/Ta is shown in FIG. 3 (a) 2 Compared with the data of the working state and the non-working state of the C MXene @ PMMA/TFBG sensor, the sensor has obvious attenuation response to gas in the P polarization state. Ammonia, methane and hydrogen sulfide gases detected at 3 to 9ppm are presented in fig. 3 (b) - (d), respectively. By comparison, it can be seen that the prepared sensor has better selectivity for ammonia gas when detecting different gases, and is shown in terms of both offset and amplitude variation, which is more obvious in the parameter statistics of fig. 3 (e). As an advantage of the other sensor, auNPs/Ta 2 The replaceability of the C MXene @ PMMA mixed sensitization structure is counted in FIG. 3 (f), the performance of the sensor is slightly reduced along with the increase of the replacement times, but the total variation still maintains the high detection performance of 3pm/ppm, which also shows the maximum advantage of the sensor and can reduce the detection cost.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe, its characterized in that: the composite sensitization plate comprises a TFBG optical fiber and a composite sensitization plate pasted on the surface of the TFBG optical fiber;
the composite sensitization plate comprises a PMMA matrix skeleton and AuNPs-doped Ta dispersed in PMMA 2 A C Mxene sensitizing material;
ta doped with AuNPs 2 The mass percentage of the C Mxene sensitization material in the composite sensitization tablet is 5-30%.
2. According to claimAuNPs/Ta as claimed in claim 1 2 C MXene @ PMMA/TFBG sensing probe, its characterized in that: ta doped with AuNPs 2 The mass percentage of the C Mxene sensitization material in the composite sensitization tablet is 7% -20%.
3. The AuNPs/Ta of claim 1 2 C MXene @ PMMA/TFBG sensing probe, its characterized in that: the thickness of the composite sensitization sheet is 2.5-3 μm.
4. AuNPs/Ta as claimed in any of claims 1 to 3 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps: the method comprises the following steps:
mixing Ta 2 Dispersing C-Mxene in water, collecting supernatant, centrifuging, and collecting precipitate to obtain Ta 2 A C-Mxene nanosheet;
chemical reduction of Ta 2 Doping AuNPs with C-Mxene nanosheets to obtain AuNPs/Ta 2 C Mxene；
Mixing AuNPs/Ta 2 Dispersing C Mxene in PMMA, performing ultrasonic treatment for a set time, adding an initiator, and blowing nitrogen;
heating the reaction mixture in water bath for reaction for a set time;
after vacuum degassing, pouring the mixture into a mould, and continuing polymerization reaction to obtain a composite sensitization sheet;
and (3) applying the composite sensitization sheet on the surface of the TFBG optical fiber, and heating to obtain the sensing probe.
5. The AuNPs/Ta of claim 4 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps of: the chemical reduction method is HAuCl 4 -3H 2 O and Ta 2 Mixed solution of C-MXene, under alkaline condition, in NaBH 4 Under the reduction action of (A) to (B), the reaction of AuNPs to (Ta) 2 And doping of C-Mxene.
6. The AuNPs/Ta according to claim 4 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps of: the time of the ultrasonic treatment is 0.5-1.5h。
7. The AuNPs/Ta according to claim 4 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps of: heating the reaction mixture in water bath at 65-80 deg.C for 3-5h.
8. The AuNPs/Ta of claim 4 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps: pouring the mixture into a mold, and continuously polymerizing for a first stage and a second stage, wherein the first stage is to keep the mold containing the mixture in a water bath for 5-7h, and the temperature of the water bath is 65-75 ℃;
the second stage is to place the mold containing the mixture at room temperature and cool for 7h.
9. The AuNPs/Ta of claim 4 2 The preparation method of the C MXene @ PMMA/TFBG sensing probe is characterized by comprising the following steps of: the composite sensitization sheet is pasted on the surface of the TFBG optical fiber, and then the temperature of the heating treatment is 75-85 ℃, and the time is 15-25min.
10. AuNPs/Ta as claimed in any of claims 1 to 3 2 Application of a C MXene @ PMMA/TFBG sensing probe in detection of ammonia gas.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210907028 | 2022-07-29 | ||
| CN2022109070288 | 2022-07-29 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115656055A true CN115656055A (en) | 2023-01-31 |
Family
ID=84995088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211372091.2A Pending CN115656055A (en) | 2022-07-29 | 2022-11-03 | AuNPs/Ta 2 C MXene @ PMMA/TFBG sensing probe and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115656055A (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375564A (en) * | 2017-07-03 | 2018-08-07 | 天津大学 | The preparation method of self-supporting stratified material MXenes and its application as Raman substrate |
| CN109613070A (en) * | 2019-01-02 | 2019-04-12 | 大连理工大学 | One kind being based on two dimension MXene/SnO2Ammonia gas sensor, preparation process and the application of hetero-junctions |
| CN109827945A (en) * | 2019-02-28 | 2019-05-31 | 合肥工业大学 | A kind of preparation method of high SERS activity Ag/MXene-Ti3C2 composite material |
| CN110455771A (en) * | 2019-08-13 | 2019-11-15 | 深圳市人民医院 | A kind of composite nano materials and its preparation method and application |
| US20190391099A1 (en) * | 2017-12-22 | 2019-12-26 | Korea Advanced Institute Of Science And Technology | Chemiresistor gas sensor using mxene and the manufacturing method thereof |
| US20200325025A1 (en) * | 2017-11-15 | 2020-10-15 | 2D Fluidics Pty Ltd | Devices and Methods for Thin Film Chemical Processing |
| CN113030213A (en) * | 2021-02-25 | 2021-06-25 | 浙江大学 | Preparation method of 3D nano composite material immunosensor based on AuNPs/MXene @ PAMAM |
| CN113533449A (en) * | 2021-07-05 | 2021-10-22 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
| CN113526507A (en) * | 2021-06-11 | 2021-10-22 | 厦门大学 | Novel MXene metal nano composite material, preparation method and application |
| CN113567510A (en) * | 2021-06-11 | 2021-10-29 | 厦门大学 | Preparation method of MXene-based composite metal nano-dot structure gas sensor |
| CN114088681A (en) * | 2021-10-15 | 2022-02-25 | 华南理工大学 | MXenes gold-loaded dimer SERS composite material and preparation method and application thereof |
-
2022
- 2022-11-03 CN CN202211372091.2A patent/CN115656055A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375564A (en) * | 2017-07-03 | 2018-08-07 | 天津大学 | The preparation method of self-supporting stratified material MXenes and its application as Raman substrate |
| US20200325025A1 (en) * | 2017-11-15 | 2020-10-15 | 2D Fluidics Pty Ltd | Devices and Methods for Thin Film Chemical Processing |
| US20190391099A1 (en) * | 2017-12-22 | 2019-12-26 | Korea Advanced Institute Of Science And Technology | Chemiresistor gas sensor using mxene and the manufacturing method thereof |
| CN109613070A (en) * | 2019-01-02 | 2019-04-12 | 大连理工大学 | One kind being based on two dimension MXene/SnO2Ammonia gas sensor, preparation process and the application of hetero-junctions |
| CN109827945A (en) * | 2019-02-28 | 2019-05-31 | 合肥工业大学 | A kind of preparation method of high SERS activity Ag/MXene-Ti3C2 composite material |
| CN110455771A (en) * | 2019-08-13 | 2019-11-15 | 深圳市人民医院 | A kind of composite nano materials and its preparation method and application |
| CN113030213A (en) * | 2021-02-25 | 2021-06-25 | 浙江大学 | Preparation method of 3D nano composite material immunosensor based on AuNPs/MXene @ PAMAM |
| CN113526507A (en) * | 2021-06-11 | 2021-10-22 | 厦门大学 | Novel MXene metal nano composite material, preparation method and application |
| CN113567510A (en) * | 2021-06-11 | 2021-10-29 | 厦门大学 | Preparation method of MXene-based composite metal nano-dot structure gas sensor |
| CN113533449A (en) * | 2021-07-05 | 2021-10-22 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
| CN114088681A (en) * | 2021-10-15 | 2022-02-25 | 华南理工大学 | MXenes gold-loaded dimer SERS composite material and preparation method and application thereof |
Non-Patent Citations (6)
| Title |
|---|
| ÁLVARO GONZÁLEZ-VILA等: ""Molecularly imprinted electropolymerization on a metal-coated optical fiber for gas sensing applications "", 《SENSORS AND ACTUATORS B: CHEMICAL》, vol. 244, 17 January 2017 (2017-01-17), pages 1145 - 1151, XP029926752, DOI: 10.1016/j.snb.2017.01.084 * |
| LI KAIKAI等: ""Fabrication of tunable hierarchical MXene@AuNPs nanocomposites constructed by self-reduction reactions with enhanced catalytic performances "", 《SCIENCE CHINA MATERIALS》, vol. 61, no. 5, 17 January 2018 (2018-01-17), pages 728 - 736 * |
| LIU RONGYANG等: ""MXene (Ti3C2Tx)-Ag nanocomplex as efficient and quantitative SERS biosensor platform by in-situ PDDA electrostatic self-assembly synthesis strategy"", 《SENSORS AND ACTUATORS: B. CHEMICAL》, vol. 333, 3 February 2021 (2021-02-03), pages 1 - 9, XP086504576, DOI: 10.1016/j.snb.2021.129581 * |
| YANG WEN等: ""Design and fabrication of an ultra-sensitive Ta2C MXene/Au-coated tilted grating sensor"", 《SENSORS AND ACTUATORS: B. CHEMICAL》, vol. 369, 16 July 2022 (2022-07-16), pages 1 - 11, XP087138745, DOI: 10.1016/j.snb.2022.132391 * |
| 尹优优等: ""二维ＭＸｅｎｅ材料在气体传感器领域的应用进展"", 《功能材料》, vol. 53, no. 3, 31 March 2022 (2022-03-31), pages 03058 - 03065 * |
| 赵秋妮等: ""MXene复合气敏材料_进展与未来挑战"", 《科学通报》, vol. 67, no. 24, 30 June 2022 (2022-06-30), pages 2823 - 2834 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Feldstein et al. | Electronic relaxation dynamics in coupled metal nanoparticles | |
| Cheng et al. | Depositing a flexible substrate of triangular silver nanoplates onto cotton fabrics for sensitive SERS detection | |
| Kiran et al. | Mechanism of intracellular detection of glucose through nonenzymatic and boronic acid functionalized carbon dots | |
| Zhou et al. | Recent advances in biosensors for antibiotic detection: Selectivity and signal amplification with nanomaterials | |
| Semwal et al. | Highly sensitive surface plasmon resonance based fiber optic pH sensor utilizing rGO-Pani nanocomposite prepared by in situ method | |
| Sun et al. | Ag@ C core/shell structured nanoparticles: controlled synthesis, characterization, and assembly | |
| Bossi et al. | An assay for ascorbic acid based on polyaniline-coated microplates | |
| Zhou et al. | Molecule-specific terahertz biosensors based on an aptamer hydrogel-functionalized metamaterial for sensitive assays in aqueous environments | |
| Zhang et al. | Metal-enhanced fluoroimmunoassay on a silver film by vapor deposition | |
| CN101544348A (en) | Composite micro-nano structure array on high light-transmission substrate and method and application thereof | |
| Liu et al. | “Turn-on” fluorescence determination of β-glucosidase activity using fluorescent polymer nanoparticles formed from polyethylenimine cross-linked with hydroquinone | |
| Liu et al. | Bis (molecular tube) s: supramolecular assembly of complexes of organoselenium-bridged β-cyclodextrins with platinum (IV) | |
| Xue et al. | Surface plasmon-enhanced optical formaldehyde sensor based on CdSe@ ZnS quantum dots | |
| Chen et al. | A highly stable optical humidity sensor | |
| CN108226137B (en) | Preparation method and application of flexible and transparent molybdenum disulfide @ silver particle/three-dimensional pyramid structure PMMA SERS substrate | |
| Volkan et al. | A sol–gel derived AgCl photochromic coating on glass for SERS chemical sensor application | |
| Liu et al. | Ultrasensitive photoelectrochemical immunosensor based on a g-C3N4/SnS2 nanocomposite for prostate-specific antigen detection | |
| Zhang et al. | Refractive index dependent real-time plasmonic nanoprobes on a single silver nanocube for ultrasensitive detection of the lung cancer-associated miRNAs | |
| Liu et al. | Novel fluorescent sensor using molecularly imprinted silica microsphere‐coated CdSe@ CdS quantum dots and its application in the detection of 2, 4, 6‐trichlorophenol from environmental water samples | |
| Wang et al. | Barium titanate film based fiber optic surface plasmon sensor with high sensitivity | |
| Lee et al. | High‐performance biosensing systems based on various nanomaterials as signal transducers | |
| Zhang et al. | Substantial enhancement toward the photocatalytic activity of CdS quantum dots by photonic crystal-supporting films | |
| CN107860760A (en) | Graphene oxide/silver nano-grain/pyramid PMMA three-dimension flexibles Raman enhancing substrate and preparation method and application | |
| Ali et al. | Electrochemiluminescence behaviour of m-CNNS quenched by CeO2@ PDA composites for sensitive detection of BNP | |
| Wang et al. | A photoelectrochemical immunosensor for prostate specific antigen detection based on graphdiyne oxide conjugated with horseradish peroxidase |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |