CN114137039B - Gas storage bag integrated with wireless passive ammonia sensor tag and preparation method thereof - Google Patents
Gas storage bag integrated with wireless passive ammonia sensor tag and preparation method thereof Download PDFInfo
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- CN114137039B CN114137039B CN202111417609.5A CN202111417609A CN114137039B CN 114137039 B CN114137039 B CN 114137039B CN 202111417609 A CN202111417609 A CN 202111417609A CN 114137039 B CN114137039 B CN 114137039B
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- ammonia gas
- hydrochloric acid
- interdigital electrode
- sensor
- acid solution
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000003860 storage Methods 0.000 title claims abstract description 19
- 229910021529 ammonia Inorganic materials 0.000 title claims description 26
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 53
- 229920000767 polyaniline Polymers 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 124
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 100
- 239000000243 solution Substances 0.000 claims description 87
- 239000010408 film Substances 0.000 claims description 66
- 239000000758 substrate Substances 0.000 claims description 53
- 239000000178 monomer Substances 0.000 claims description 50
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 48
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 24
- 241000590002 Helicobacter pylori Species 0.000 claims description 20
- 229940037467 helicobacter pylori Drugs 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 18
- 239000010409 thin film Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000002121 nanofiber Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 230000008859 change Effects 0.000 description 17
- 230000000694 effects Effects 0.000 description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
- 239000004202 carbamide Substances 0.000 description 6
- OKTJSMMVPCPJKN-NJFSPNSNSA-N Carbon-14 Chemical compound [14C] OKTJSMMVPCPJKN-NJFSPNSNSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-OUBTZVSYSA-N Carbon-13 Chemical compound [13C] OKTJSMMVPCPJKN-OUBTZVSYSA-N 0.000 description 4
- 239000002775 capsule Substances 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 241000167880 Hirundinidae Species 0.000 description 3
- 108010046334 Urease Proteins 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000008506 pathogenesis Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000007882 Gastritis Diseases 0.000 description 1
- 206010019375 Helicobacter infections Diseases 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 231100000676 disease causative agent Toxicity 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 210000004051 gastric juice Anatomy 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 208000017169 kidney disease Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 208000018556 stomach disease Diseases 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B10/00—Other methods or instruments for diagnosis, e.g. instruments for taking a cell sample, for biopsy, for vaccination diagnosis; Sex determination; Ovulation-period determination; Throat striking implements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a gas storage bag integrated with a wireless passive ammonia gas sensor tag and a preparation method thereof, and the gas storage bag is characterized by comprising a bag body, wherein the top of the bag body is provided with an opening, a sealing cover is arranged on the opening, and an ammonia gas detection film sensor and a passive NFC tag are arranged in the inner wall of the bag body; the ammonia gas detection film sensor comprises an interdigital electrode fixed on the bag body and a polyaniline composite film covered on the interdigital electrode, and the interdigital electrode is electrically connected with a passive NFC tag. The integrated degree is high, the sensitivity of the ammonia gas detection sensor is high, the response time and the recovery time are both short, the time utilization rate is high, and the ammonia gas detection sensor can be repeatedly utilized. The detection is completed, the result can be directly transmitted in a wireless mode, and the operation is simple.
Description
Technical Field
The invention belongs to the technical field of detection sensors, and particularly relates to a thin film sensor detection device for detecting ammonia content in expired air and a preparation method thereof.
Background
Helicobacter Pylori (HP) is a monopolar, multi-flagellum, spiral bacterium which can exist in gastric juice and is also a causative agent of the pathogenesis of various stomach diseases, such as gastric ulcer, gastritis and the like, even stomach cancer, and plays an important role in the pathogenesis, and is extremely harmful to human bodies. At the same time, the rapid pace of life and unhealthy lifestyle make their infection rate extremely high. Therefore, the attention of modern medicine to helicobacter pylori is also increasing. Helicobacter pylori detection windows are specifically opened in some pilot hospitals.
Although many efforts have been made in the medical sector, little has been done. On the one hand, the incubation period of helicobacter pylori is longer, and most people do not pay attention to the helicobacter pylori; on the other hand, at present, the medical science is used for detecting helicobacter pylori infection condition by using a mass spectrometer, and the mass spectrometer has the advantages of high price, heavy volume and higher requirements on operators, so that the popularization and development of the mass spectrometer in primary hospitals are limited to a great extent, and the opportunity of more patients to accept detection and treatment is limited.
The current medical detection method for helicobacter pylori is mainly carbon 13/carbon 14 exhalation test. In the test, a patient swallows a urea capsule with a carbon 13/carbon 14 mark in advance, and after the patient swallows the capsule, helicobacter pylori in the stomach can secrete urease to decompose urea, so that carbon dioxide and ammonia with the carbon 13/carbon 14 mark are generated. Medical staff determine whether the patient needs treatment by detecting the carbon dioxide content of the expired air with the carbon 13/carbon 14 mark through a mass spectrometer. The medical high-precision isotope mass spectrometer has the advantages of higher price, high detection cost for patients, long detection time, radioactivity of carbon 14 and harm to human bodies.
Disclosure of Invention
The invention provides a gas storage bag integrated with a wireless passive ammonia sensor tag, which improves the detection speed of helicobacter pylori.
In order to achieve the purpose, the gas storage bag integrated with the wireless passive ammonia sensor tag comprises a bag body, wherein an opening is formed in the bag body, a sealing cover is arranged on the opening, and an ammonia detection film sensor and a passive NFC tag are arranged in the inner wall of the bag body; the ammonia gas detection film sensor comprises an interdigital electrode fixed on the bag body and a polyaniline composite film covered on the interdigital electrode, and the interdigital electrode is connected with a passive NFC label.
Further, the passive NFC tag includes an antenna and a microchip, wherein an end connector of the antenna is connected to a pin of the microchip, and a disconnected position of the antenna is connected to an electrode pin of the interdigital electrode.
Further, the interdigital electrode is a silver electrode.
Further, the polyaniline composite film is polyaniline/Ti 3 C 2 T X And (3) a composite film.
The preparation method of the air storage bag integrated with the wireless passive ammonia sensor tag comprises the following steps of:
s1, preparing an ammonia gas detection film flexible film sensor on a substrate;
s1.1: taking nanofiber paper as a flexible substrate, and directly writing interdigital electrodes on the flexible substrate;
s1.2: mixing aniline monomer and hydrochloric acid solution in the volume ratio of 1 (100-300) to obtain aniline monomer hydrochloric acid solution; adding ammonium persulfate powder into a hydrochloric acid solution, and performing ultrasonic dispersion to prepare an ammonium persulfate hydrochloric acid solution; ti is mixed with 3 C 2 T X Ultrasonic dispersing NMP solution to obtain Ti after ultrasonic treatment 3 C 2 T X NMP dispersion;
s1.3: taking Ti 3 C 2 T X Adding NMP dispersion into aniline monomer hydrochloric acid solution prepared by S1.2, and stirring uniformly to obtain aniline monomer/Ti 3 C 2 T X Mixing solution in which Ti 3 C 2 T X The volume ratio of NMP dispersion liquid to aniline monomer hydrochloric acid solution is 1 (1.5-2.5);
s1.4: mixing ammonium sulfate solution with aniline monomer/Ti 3 C 2 T X Mixing and stirring the mixed solution according to the volume ratio of 1 (2-4) until ammonium persulfate hydrochloric acid and aniline monomer/Ti 3 C 2 T X Completely reacting to obtain a solution A;
s1.5: inserting the flexible substrate with the interdigital electrodes into the solution A, and forming a layer of composite film on the surfaces of the interdigital electrodes;
s1.6: taking out the flexible substrate, dripping and washing, and then drying to obtain the ammonia gas detection flexible film sensor;
s2, preparing an NFC label on a substrate of the ammonia gas detection flexible film sensor to obtain an NFC label of the integrated ammonia gas detection flexible film sensor;
s3, manufacturing the substrate integrated with the ammonia gas detection film flexible film sensor and the NFC label into a bag body, and arranging a sealing cover at the opening of the bag body.
In step S1.2, the concentration of the ammonium persulfate hydrochloric acid solution is 0.08mol/L to 0.12mol/L.
Further, in step S1.2, ti 3 C 2 T X The concentration of NMP solution is 0.8 mg/mL-1.0 mg/mL.
Further, S2 includes the following steps:
s2.1, printing conductive ink on a substrate to obtain an antenna, connecting two ends of the prepared interdigital electrode of the film sensor into the antenna, and drying;
s2.2, printing the microchip on a substrate, and connecting the microchip with the silver interdigital electrode by using conductive resin as a wire;
s2.3, solidifying the structure obtained in the step S2.2 to obtain the NFC label integrated with the ammonia gas detection flexible film sensor.
Compared with the prior art, the invention has at least the following beneficial technical effects:
the invention provides a convenient and environment-friendly gas storage bag integrated with a wireless passive ammonia sensor tag, which adopts nanofiber paper with a smooth surface as a packaging material, has low production cost, is rich in raw material natural reserves and is natural and degradable. Meanwhile, the nanofiber paper is used as a substrate, the ammonia gas detection film sensor and the passive NFC label can be directly manufactured on the nanofiber paper, and the integration degree is high. The polyaniline in the ammonia detection film sensor has high sensitivity in detecting ammonia, short response time and recovery time, high time utilization rate and repeated use. The detection is completed, the result can be directly transmitted in a wireless mode, and the operation is simple.
Further, the polyaniline composite film is polyaniline/Ti 3 C 2 T X Composite film, ti 3 C 2 T X The gas sensor has high specific surface area, obvious surface effect and strong chemical activity, so that the gas sensor is extremely easy to adsorb a large amount of gas molecules in the environment, and the response of the gas sensor is obviously improved. According to the preparation method, the polyaniline composite film and the interdigital electrode are prepared on the substrate to obtain the ammonia gas detection film sensor, then the NFC label is manufactured on the same substrate, the substrate is manufactured into a bag body to obtain the air storage bag integrated with the wireless passive ammonia gas sensor label, polyaniline in the ammonia gas detection film sensor reacts with ammonia gas to detect, and the operation is convenient.
According to the preparation method of the air storage bag integrated with the wireless passive ammonia sensor tag, the ammonia detection flexible film sensor and the NFC tag are prepared on the same substrate, the preparation method is simple and convenient, the substrate is directly used as a bag body, the integration level is high, and the use is convenient.
Drawings
FIG. 1 is a schematic illustration of a gas storage bag;
FIG. 2 is a schematic diagram of ammonia gas detecting film structure;
fig. 3 is a schematic diagram of connection between an NFC tag and an ammonia gas detecting film.
In the accompanying drawings: 1-sealing cover, 2-bag body, 3-composite film, 4-interdigital electrode, 5-substrate, 6-wire, 7-antenna and 8-microchip.
Detailed Description
In order to make the purpose and technical scheme of the invention clearer and easier to understand. The present invention will now be described in further detail with reference to the drawings and examples, which are given for the purpose of illustration only and are not intended to limit the invention thereto.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more. In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Example 1
Referring to fig. 1, a gas storage bag integrated with a wireless passive ammonia gas sensor tag comprises a bag body 2, wherein an opening is formed in the top of the bag body 2, a sealing cover 1 with a sealing ring is arranged on the opening, and an ammonia gas detection film sensor and a passive NFC tag are arranged in an inner cavity of the bag body 2. The bag body 2 is made of nanofiber paper and is natural and degradable.
Referring to fig. 2 and 3, the ammonia gas detecting thin film sensor is composed of three thin films including an upper layer Polyaniline (PANI)/Ti 3 C 2 T X The composite film, the middle silver interdigital electrode and the lower substrate 5, wherein the substrate 5 is nanofiber paper (NCP). The passive NFC tag connected with it to form a complete structure is composed of a substrate 5, an antenna 7 and a microchip 8. The antenna 7 is directly written on the substrate 5 and the microchip 8 is fixed at the antenna end for signal conditioning. The ammonia gas detection film sensor is connected with the passive NFC tag through a lead 6, namely, two ends of the interdigital electrode 4 are respectively connected with two disconnected ends of the antenna 7.
The device can be used for detecting helicobacter pylori and also is suitable for detecting some kidney diseases. Before use, the sealing cover 1 is taken down, the sealing cover 1 is covered after blowing air into the inner cavity of the bag body 2, and the detection result can be waited.
When the gas in the bag body 2 contains ammonia, the ammonia is adsorbed on Polyaniline (PANI)/Ti 3 C 2 T X And protons combined with the conductive PANI amine groups are extracted from the composite film, so that the positive charge of the PANI with conductivity is reduced, and the resistance of the ammonia gas detection film sensor is increased. Further, since the thin film sensor is integrally connected to the antenna 7, the resistance of the antenna end increases with the increase of the sensor resistance. At this time, the network analyzer transmits a sinusoidal sweep frequency signal to the antenna, the NFC tag receives the signal, obtains its energy activation circuit, modulates the signal, and forms an echo to return to the network analyzer. The network analyzer obtains the return loss S by comparing the emitted sine sweep signal and the echo signal 11 Magnitude of amplitude. The magnitude of the return loss changes with the change of the antenna end resistance, the antenna end resistance change depends on the change of the thin film sensor resistance, and the thin film sensor resistance changes with the change of the ammonia volume fraction. Thus return loss S 11 The amplitude change can directly represent the resistance change of the film sensor, and the formula is as follows:
wherein Z is in Is a thin film sensor resistance; z is Z 0 The inherent resistance of the antenna is set to 50Ω by default. The antenna end resistance is equal to the sum of the film sensor resistance and the antenna inherent resistance. When the resistance of the film sensor changes along with the change of the ammonia gas volume fraction, the antenna end resistance changes along with the change of the resistance of the film sensor, and the return loss S is reduced 11 Also changes with the change of the antenna end resistance, thus the return loss S 11 The change in ammonia volume fraction can be indirectly characterized. The larger the volume fraction of the ammonia gas, the more amount of helicobacter pylori secreted urease reacts with urea, and the helicobacter pylori content in a human body is indirectly represented.
The network analyzer is any NFC enabled device, such as a cell phone.
Example 2
The preparation method of the ammonia gas detection flexible film sensor comprises the following steps:
s1: taking nanofiber paper (NCP) with a smooth surface as a flexible substrate, and directly writing the interdigital electrode 4 on the flexible substrate by utilizing the Wessenberg effect to obtain the flexible substrate with the interdigital electrode 4; the interdigital electrode 4 is a metal material, preferably silver.
S2: preparing 1.5-2.5 mol/L hydrochloric acid solution;
s3: dripping aniline monomer (ANI) into the hydrochloric acid solution prepared in the S2 by using a pipette gun, mixing the aniline monomer and the hydrochloric acid solution according to the volume ratio of 1:100-1:300, and slowly stirring until the aniline monomer and the hydrochloric acid solution are uniformly dispersed to obtain aniline monomer hydrochloric acid solution;
s4: ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Slowly adding the powder into the hydrochloric acid solution prepared by the S2, carrying out ultrasonic treatment to uniformly mix the powder and the hydrochloric acid solution, and preparing ammonium persulfate hydrochloric acid solution with the concentration of 0.08-0.12 mol/L;
s5: taking 0.8-1.0 mg/mL Ti 3 C 2 T X Placing NMP into cell wall breaking machine, ultrasonic probe 1.5cm away from cup bottom, ultrasonic power 150W, ultrasonic pulse interval 3s to obtain Ti 3 C 2 T X NMP dispersion;
s6: taking Ti 3 C 2 T X NMP dispersion liquid is dropwise added into aniline monomer hydrochloric acid solution prepared in S3, ti 3 C 2 T X NMP dispersion liquid and aniline monomer hydrochloric acid solution are mixed according to the volume ratio of 1:1.5-1:2.5, and aniline monomer/Ti is obtained 3 C 2 T X Mixing the solutions;
s7: dropwise dripping the ammonium persulfate hydrochloric acid solution prepared in the step S4 into the aniline monomer/Ti obtained in the step S6 3 C 2 T X In the mixed solution, ammonium persulfate solution and aniline monomer/Ti 3 C 2 T X Mixing the mixed solution in a volume ratio of 1:2-1:4, continuously stirring until the solution is completely reacted, and inserting the flexible substrate with the interdigital electrode 4;
s8: and waiting for 15-20 minutes, forming a layer of composite film on the surface of the interdigital electrode 4 by the mixed solution, taking out the flexible substrate, washing with hydrochloric acid solution drops, and drying at room temperature after the completion of the dripping, thereby obtaining the ammonia gas detection flexible film sensor.
Example 3
The preparation method of the ammonia gas detection flexible film sensor comprises the following steps:
s1: taking nanofiber paper (NCP) with a smooth surface as a flexible substrate, and directly writing the interdigital electrode 4 on the flexible substrate by utilizing the Wessenberg effect to obtain the flexible substrate with the interdigital electrode 4; the interdigital electrode 4 is a metal material, preferably silver.
S2: preparing 1.5mol/L hydrochloric acid solution;
s3: dripping aniline monomer (ANI) into the hydrochloric acid solution prepared in the S2 by using a pipette gun, mixing the aniline monomer and the hydrochloric acid solution according to the volume ratio of 1:100, and slowly stirring until the aniline monomer and the hydrochloric acid solution are uniformly dispersed to obtain aniline monomer hydrochloric acid solution;
s4: ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Slowly adding the powder into the hydrochloric acid solution prepared by the S2, and carrying out ultrasonic treatment to uniformly mix the powder and the hydrochloric acid solution with 0.10mol/L ammonium persulfate so as to prepare the hydrochloric acid solution;
s5: taking 0.8mg/mL Ti 3 C 2 T X NMP solution settingPutting into cell wall breaking machine, and performing ultrasonic treatment to obtain Ti 3 C 2 T X NMP dispersion;
s6: taking Ti 3 C 2 T X NMP dispersion liquid is dropwise added into aniline monomer hydrochloric acid solution prepared in S3, ti 3 C 2 T X NMP dispersion liquid and aniline monomer hydrochloric acid solution are mixed according to the volume ratio of 1:1.5 to obtain aniline monomer/Ti 3 C 2 T X Mixing the solutions;
s7: dropwise dripping the ammonium persulfate hydrochloric acid solution prepared in the step S4 into the aniline monomer/Ti obtained in the step S6 3 C 2 T X In the mixed solution, ammonium persulfate solution and aniline monomer/Ti 3 C 2 T X Mixing the mixed solution in a volume ratio of 1:2, continuously stirring until the solution is completely reacted, and inserting the flexible substrate with the interdigital electrode 4;
s8: and waiting for 15 minutes, forming a layer of composite film on the surface of the interdigital electrode 4 by the mixed solution, taking out the flexible substrate, washing with hydrochloric acid solution drops, and drying at room temperature after the completion of the dripping, thereby obtaining the ammonia gas detection flexible film sensor.
Example 4
The preparation method of the ammonia gas detection flexible film sensor comprises the following steps:
s1: taking nanofiber paper (NCP) with a smooth surface as a flexible substrate, and directly writing the interdigital electrode 4 on the flexible substrate by utilizing the Wessenberg effect to obtain the flexible substrate with the interdigital electrode 4; the interdigital electrode 4 is a metal material, preferably silver.
S2: preparing a hydrochloric acid solution with the concentration of 2.0 mol/L;
s3: dripping aniline monomer (ANI) into the hydrochloric acid solution prepared in the S2 by using a pipette gun, mixing the aniline monomer and the hydrochloric acid solution according to the volume ratio of 1:200, and slowly stirring until the aniline monomer and the hydrochloric acid solution are uniformly dispersed to obtain aniline monomer hydrochloric acid solution;
s4: ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Slowly adding the powder into the hydrochloric acid solution prepared by the S2, performing ultrasonic treatment to uniformly mix the powder and the hydrochloric acid solution with 0.08mol/L ammonium persulfate;
s5: taking 0.9mg/mLTi 3 C 2 T X Placing NMP solution into cell wall breaking machine, and making ultrasonic treatment to obtain Ti 3 C 2 T X NMP dispersion;
s6: taking Ti 3 C 2 T X NMP dispersion liquid is dropwise added into aniline monomer hydrochloric acid solution prepared in S3, ti 3 C 2 T X NMP dispersion liquid and aniline monomer hydrochloric acid solution are mixed in a volume ratio of 1:2 to obtain aniline monomer/Ti 3 C 2 T X Mixing the solutions;
s7: dropwise dripping the ammonium persulfate hydrochloric acid solution prepared in the step S4 into the aniline monomer/Ti obtained in the step S6 3 C 2 T X In the mixed solution, ammonium persulfate solution and aniline monomer/Ti 3 C 2 T X Mixing the mixed solution in a volume ratio of 1:3, continuously stirring until the solution is completely reacted, and inserting the flexible substrate with the interdigital electrode 4;
s8: and waiting for 20 minutes, forming a layer of composite film on the surface of the interdigital electrode 4 by the mixed solution, taking out the flexible substrate, washing with hydrochloric acid solution drops, and drying at room temperature after the completion of the dripping, thereby obtaining the ammonia gas detection flexible film sensor.
Example 5
The preparation method of the ammonia gas detection flexible film sensor comprises the following steps:
s1: taking nanofiber paper (NCP) with a smooth surface as a flexible substrate, and directly writing the interdigital electrode 4 on the flexible substrate by utilizing the Wessenberg effect to obtain the flexible substrate with the interdigital electrode 4; the interdigital electrode 4 is a metal material, preferably silver.
S2: preparing a hydrochloric acid solution with the concentration of 2.5 mol/L;
s3: dripping aniline monomer (ANI) into the hydrochloric acid solution prepared in the S2 by using a pipette gun, mixing the aniline monomer and the hydrochloric acid solution according to the volume ratio of 1:300, and slowly stirring until the aniline monomer and the hydrochloric acid solution are uniformly dispersed to obtain aniline monomer hydrochloric acid solution;
s4: ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Slowly adding the powder into the hydrochloric acid solution prepared by the S2, performing ultrasonic treatment to uniformly mix the powder and the hydrochloric acid solution with 0.12mol/L ammonium persulfate;
s5: 1.0mg/mL of Ti was taken 3 C 2 T X Placing NMP solution into cell wall breaking machine, and making ultrasonic treatment to obtain Ti 3 C 2 T X NMP dispersion;
s6: taking Ti 3 C 2 T X NMP dispersion liquid is dropwise added into aniline monomer hydrochloric acid solution prepared in S3, ti 3 C 2 T X NMP dispersion liquid and aniline monomer hydrochloric acid solution are mixed according to the volume ratio of 1:2.5 to obtain aniline monomer/Ti 3 C 2 T X Mixing the solutions;
s7: dropwise dripping the ammonium persulfate hydrochloric acid solution prepared in the step S4 into the aniline monomer/Ti obtained in the step S6 3 C 2 T X In the mixed solution, ammonium persulfate solution and aniline monomer/Ti 3 C 2 T X Mixing the mixed solution in a volume ratio of 1:4, continuously stirring until the solution is completely reacted, and inserting the flexible substrate with the interdigital electrode 4;
s8: after the mixed solution forms a layer of composite film on the surface of the interdigital electrode 4, the flexible substrate is taken out and is washed by hydrochloric acid solution drops, and the flexible film sensor for detecting ammonia gas is obtained after the completion of the drop washing and drying at room temperature.
Example 6
A method of preparing an NFC tag comprising the steps of:
s1, taking out the thin film sensor prepared in the embodiment 3, and preparing an NFC label on a substrate of the thin film sensor;
s2, printing an antenna on nanofiber paper by utilizing a screen printing technology, wherein the used material is silver conductive ink, partial antenna disconnection is reserved, and two ends of the prepared thin film sensor interdigital electrode 4 are in butt joint with two ends of the disconnection position of the antenna 7 to form a complete structure;
s3, drying the structure obtained in the step S2;
s4, printing the microchip 8 on nanofiber paper, and connecting the microchip 8 with the silver interdigital electrode 4 by using conductive resin as a wire 6;
s5, the structure obtained in the step 4 is placed in a hot blast stove to be solidified, and the NFC label integrated with the ammonia gas detection flexible film sensor is obtained.
Example 7
The preparation method of the air storage bag integrated with the wireless passive ammonia sensor tag comprises the following steps of:
s1, preparing an ammonia gas detection thin film flexible thin film sensor on a substrate 5 by using the method described in the embodiment 3-5;
s2, preparing an NFC label on a substrate 5 of the ammonia gas detection flexible film sensor by using the method described in the embodiment 6;
s3, manufacturing the substrate 5 integrated with the NFC label and the ammonia gas detection film flexible film sensor into a bag body 2, and arranging a sealing cover 1 at an opening of the bag body 2.
The working principle of the invention is as follows:
the inspector swallows the carbon-free 13/14-labeled urea capsule and then blows the urea capsule into the bag, and if the exhaled air contains ammonia gas, the ammonia gas is used as alkaline gas, and alkali de-doping is generated after the ammonia gas contacts Polyaniline (PANI). The ammonia gas molecules have a stronger proton acid affinity than the amine groups on PANI, which causes the ammonia to abstract protons that would otherwise bind to the conductive PANI amine groups, resulting in a decrease in the positive charge that causes PANI to have conductivity and an increase in electrical resistance. And Ti is 3 C 2 T X Has high specific surface area, obvious surface effect and strong chemical activity. These characteristics make it extremely easy to adsorb a large amount of gas molecules in the environment, thereby significantly improving the response of the gas sensor. The wireless transmission of signals is completed between the network analyzer and the NFC tag through an electromagnetic coupling method, when the network analyzer transmits a sine sweep frequency signal to the antenna, the NFC tag receives the signal to obtain an energy activation circuit of the signal, and if the resistance of the ammonia gas detection film sensor changes at the moment, the input resistance measured from the antenna end correspondingly changes. The NFC tag modulates the signal and returns the signal to the network analyzer. The network analyzer obtains the return loss S by comparing the two signals 11 Magnitude of amplitude. The magnitude of the return loss changes with the change of the antenna end resistance, the antenna end resistance change depends on the change of the thin film sensor resistance, and the thin film sensor resistance changes with the change of the ammonia volume fraction. Because ofThis return loss S 11 The amplitude change can directly represent the resistance change of the antenna end, so that the change of the ammonia volume fraction is indirectly represented. The larger the volume fraction of the ammonia gas, the more amount of helicobacter pylori secreted urease reacts with urea, and the helicobacter pylori content in a human body is indirectly represented.
The above detailed description is merely illustrative of the preferred embodiments of the present invention and is not intended to limit the scope of the present invention. Various modifications, substitutions and improvements of the technical scheme of the present invention will be apparent to those skilled in the art from the description and drawings provided herein without departing from the spirit and scope of the invention. The scope of the invention is defined by the claims.
Claims (6)
1. The air storage bag for the integrated wireless passive ammonia gas sensor tag for detecting helicobacter pylori is characterized by comprising a bag body (2), wherein an opening is formed in the bag body (2), a sealing cover (1) is arranged on the opening, and an ammonia gas detection film sensor and a passive NFC tag are arranged in the inner wall of the bag body (2); the ammonia gas detection film sensor is characterized in that the bag body (2) is made of nanofiber paper, and comprises an interdigital electrode (4) fixed on the bag body (2) and a polyaniline composite film covered on the interdigital electrode (4), wherein the interdigital electrode (4) is electrically connected with a passive NFC tag;
the passive NFC tag comprises an antenna (7) and a microchip (8), wherein the tail end joint of the antenna (7) is connected with a pin of the microchip (8), and the disconnection position of the antenna (7) is connected with an electrode pin of the interdigital electrode (4);
the NFC tag receives the signal when the network analyzer transmits a sine sweep frequency signal to the antenna, an energy activation circuit of the signal is obtained, if the resistance of the ammonia gas detection film sensor is changed at the moment, the input resistance measured from the antenna end is also changed, and the NFC tag modulates the signal and returns the signal to the network analyzer;
the polyaniline composite film is polyaniline/Ti 3 C 2 T X A composite film;
before use, the sealing cover (1) is taken down, the sealing cover (1) is covered after blowing air into the inner cavity of the bag body (2), and then the detection result can be waited.
2. A gas storage bag for an integrated wireless passive ammonia sensor tag for detecting helicobacter pylori according to claim 1, characterized in that the interdigital electrode (4) is a silver electrode.
3. A method of manufacturing a gas storage bag for an integrated wireless passive ammonia sensor tag for detecting helicobacter pylori as defined in claim 1, comprising the steps of:
s1, preparing an ammonia gas detection thin film flexible thin film sensor on a substrate (5);
s1.1: taking nanofiber paper as a flexible substrate, and directly writing the interdigital electrode (4) on the flexible substrate;
s1.2: mixing aniline monomer and hydrochloric acid solution uniformly in a volume ratio of 1 (100-300) to obtain aniline monomer hydrochloric acid solution; adding ammonium persulfate powder into a hydrochloric acid solution, and performing ultrasonic dispersion to prepare an ammonium persulfate hydrochloric acid solution; ti is mixed with 3 C 2 T X Ultrasonic dispersing NMP solution to obtain Ti after ultrasonic treatment 3 C 2 T X NMP dispersion;
s1.3: taking Ti 3 C 2 T X Adding NMP dispersion into aniline monomer hydrochloric acid solution prepared by S1.2, and stirring uniformly to obtain aniline monomer/Ti 3 C 2 T X Mixing solution in which Ti 3 C 2 T X The volume ratio of the NMP dispersion liquid to the aniline monomer hydrochloric acid solution is 1 (1.5-2.5);
s1.4: mixing ammonium sulfate solution with aniline monomer/Ti 3 C 2 T X Mixing and stirring the mixed solution according to the volume ratio of 1 (2-4) until ammonium persulfate hydrochloric acid and aniline monomer/Ti 3 C 2 T X Completely reacting to obtain a solution A;
s1.5: inserting a flexible substrate with an interdigital electrode (4) into the solution A, and forming a layer of composite film on the surface of the interdigital electrode (4);
s1.6: taking out the flexible substrate, dripping and washing, and then drying to obtain the ammonia gas detection flexible film sensor;
s2, preparing an NFC label on a substrate (5) of the ammonia gas detection flexible film sensor to obtain an NFC label of the integrated ammonia gas detection flexible film sensor;
s3, manufacturing the substrate (5) integrated with the ammonia gas detection film flexible film sensor and the NFC label into a bag body (2), and arranging a sealing cover (1) at the opening of the bag body (2).
4. The method for preparing the air storage bag for the integrated wireless passive ammonia sensor tag for detecting helicobacter pylori according to claim 3, wherein the concentration of the ammonium persulfate hydrochloric acid solution prepared in the step S1.2 is 0.08 mol/L-0.12 mol/L.
5. A method for manufacturing a gas storage bag for an integrated wireless passive ammonia sensor tag for detecting helicobacter pylori according to claim 3, characterized in that in step S1.2, ti 3 C 2 T X The concentration of the NMP solution is 0.8 mg/mL-1.0 mg/mL.
6. A method for preparing a gas storage bag for an integrated wireless passive ammonia sensor tag for detecting helicobacter pylori according to claim 3, characterized in that S2 comprises the steps of:
s2.1, printing conductive ink on a substrate (5) to obtain an antenna (7), connecting two ends of the prepared interdigital electrode of the film sensor into the antenna (7), and drying;
s2.2, printing a microchip (8) on the substrate (5), and connecting the microchip (8) with the silver interdigital electrode (4) by using conductive resin as a wire (6);
s2.3, solidifying the structure obtained in the step S2.2 to obtain the NFC label integrated with the ammonia gas detection flexible film sensor.
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