CN110669237A - Polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline film ammonia gas sensor and preparation method thereof - Google Patents
Polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline film ammonia gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline film ammonia gas sensor which comprises a polyvinylidene fluoride layer, a poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline layer and an interdigital electrode layer. The sensor prepared by the invention has high sensitivity, high selectivity and high stability for detecting ammonia gas; the invention can adjust the conductivity and gas-sensitive property of the polyaniline film layer by regulating and controlling the concentrations of poly (2-acrylamide-2-methylpropanesulfonic acid), aniline and ammonium persulfate, has the advantages of miniaturization and room-temperature work, thereby reducing power consumption, and simultaneously has the advantages of large-scale production and low cost, and is beneficial to industrial production. In addition, the polyaniline can be obtained after the residual solution is filtered and dried, so that the waste is reduced, and the cost is saved.
Description
Technical Field
The invention relates to a gas sensor, in particular to a detection sensor for ammonia gas, and also relates to a preparation method thereof.
Background
Today, the problem of atmospheric pollution is undoubtedly affecting the normal production and living activities of human beings. It is known that ammonia gas has serious harm to human health due to its high toxicity and strong corrosiveness, and in addition, ammonia gas is also a potential biomarker for diagnosing diseases such as uremia and duodenal ulcer in the detection of respiratory gas components of human bodies. Therefore, the development of the high-performance flexible room-temperature gas sensor has important significance in the fields of environmental detection, human health early warning, military, national defense and the like.
Since the relevant gas in the human respiratory gas, which reflects the human health condition, generally has low concentration and complex composition factors, there are high sensitivity and high selectivity requirements for the gas sensor for human health condition early warning. In order to achieve the purpose of industrial production, the sensor also needs to have the advantages of high stability, low cost, simple manufacture, large-scale manufacture and the like. Further, in practical applications of products, flexibility, low-temperature operation, low power consumption, miniaturization, integration, wireless, and the like are generally required. Currently, the sensitive materials for ammonia detection are generally classified into four types: metal oxides, carbon tubes, graphene, and organic polymers. The metal oxide material is a conventional gas-sensitive material for gas detection at present, but the metal oxide generally needs a very high working temperature, so that the power consumption is large, and the detected concentration of the metal oxide is mostly above ppm level, so that the metal oxide material is not suitable for wearable equipment applied to the aspect of human body breathing gas detection. And carbon tubes and graphene materials generally have the defects of low sensitivity, poor selectivity and the like. The organic polymer has the advantages of room-temperature working, high sensitivity, simple manufacturing method, good stability and the like, and is an important research material in the aspect of ammonia gas detection at present. However, generally, the sensor is made of an organic polymer such as polyaniline by dissolving the powder in an organic solvent (e.g., hexafluoroisopropanol, and azomethylpyrrolidone), and then coating the powder on the electrode by means of dropping or spin coating. The sensor manufactured by the method has the defects of low sensitivity, poor stability, complex manufacturing and the like. In addition, the invention patent CN 109613069 discloses a preparation method of an ammonia gas sensor of a polyvinylidene fluoride and polyaniline composite flexible membrane, but in the preparation method, the polyaniline is polymerized by using hydrochloric acid as protonic acid, and finally the detection of ammonia gas reaches 100 ppb. But the detection of ammonia in human respiratory gas with lower concentration has higher requirement for the detection limit of ammonia.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the high-efficiency ammonia gas sensor based on the polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline composite flexible membrane, and the performance of the obtained gas sensor is greatly improved compared with other ammonia gas sensors.
The technical scheme of the invention is to provide a high-efficiency ammonia gas sensor based on a polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline composite flexible membrane, which comprises a polyvinylidene fluoride layer, a poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline layer and an interdigital electrode layer.
Further, a poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline layer is grown on the polyvinylidene fluoride porous membrane layer by adopting an in-situ growth method.
Further, the interdigital electrode layer is formed by depositing a conductive material on the polyaniline layer by a screen printing method, an ink-jet printing method or the like; wherein the conductive material is one of silver conductive ink or copper conductive ink.
The invention also provides a preparation method of the high-efficiency ammonia gas sensor based on the polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline composite flexible membrane, which comprises the following steps:
(1) sequentially and respectively soaking a polyvinylidene fluoride porous membrane in ethanol and acetone, and ultrasonically cleaning for 15-20 minutes generally; then heat-treating at 50-150 deg.C for 10-100 min;
(2) adding 1-13g of 2-acrylamide-2-methylpropanesulfonic acid into a container filled with 75ml of deionized water, then carrying out magnetic stirring for 10-300 minutes, adding 1-5g of potassium persulfate into the solution, and then carrying out magnetic stirring for 10-100 minutes;
(3) putting the solution into an oil bath kettle preheated to 50-100 ℃, introducing nitrogen into the solution in the reaction process, and reacting for 1-6 h;
(4) cooling the solution to room temperature, then pouring the solution into a beaker, adding 500ml of acetone with the volume of 200-;
(5) adding 1-10g of the powder obtained in the step (4) into 100-300ml of deionized water, magnetically stirring for 10-300 minutes, adding 0.01-3g of aniline, ultrasonically oscillating for 10-100 minutes, putting the polyvinylidene fluoride porous membrane treated in the step (1) into the solution to obtain a solution A, and putting the solution A into ice water;
(6) adding 1-10g of ammonium persulfate into 20ml of deionized water, carrying out ultrasonic oscillation for 5-100 minutes, adding the obtained solution into the solution A, and keeping the solution in ice water for reaction for 5-30 hours;
(7) taking out the polyvinylidene fluoride porous membrane, washing with deionized water, and then carrying out heat treatment at 30-150 ℃ for 1-10 h;
(8) depositing one of silver conductive ink and copper conductive ink on the polyvinylidene fluoride porous membrane by screen printing, ink-jet printing or sputtering, and then carrying out heat treatment at 40-200 ℃ for 30-200 minutes.
The invention has the advantages and beneficial effects that:
the sensor prepared by the invention has high sensitivity and better response to low-concentration ammonia gas (30 ppb); high selectivity, and has larger response to ammonia gas only; high stability, and basically unchanged initial resistance after multiple measurements.
The invention can adjust the conductivity and gas-sensitive property of the polyaniline film layer by regulating and controlling the concentrations of poly (2-acrylamide-2-methylpropanesulfonic acid), aniline and ammonium persulfate, has the advantages of miniaturization and room-temperature work, thereby reducing power consumption, and simultaneously has the advantages of large-scale production and low cost, and is beneficial to industrial production. In addition, the polyaniline can be obtained after the residual solution is filtered and dried, so that the waste is reduced, and the cost is saved.
The invention has the advantages of simple manufacture, low cost, mild reaction conditions and good controllability, and is beneficial to industrial production.
Drawings
Fig. 1 shows response tests of the ammonia gas sensor prepared in example 1 of the present invention to ammonia gas of different concentrations.
FIG. 2 is a graph showing the selectivity test of the ammonia gas sensor prepared in example 1 of the present invention for various gases.
Fig. 3 is a graph showing the resistance change of the ammonia gas sensor prepared in example 1 of the present invention after repeated several times.
Fig. 4 is a test of the stability of the long-term response performance of the ammonia gas sensor prepared in example 1 of the present invention.
FIG. 5 is a schematic diagram of a performance test flow of the ammonia gas sensor prepared by the invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
(1) Respectively soaking a polyvinylidene fluoride porous membrane in ethanol and acetone, and ultrasonically cleaning for 15 minutes generally; then heat-treating at 100 deg.C for 10 min;
(2) adding 12g of 2-acrylamide-2-methylpropanesulfonic acid into a three-hole flask filled with 75ml of deionized water, then carrying out magnetic stirring for 200 minutes, adding 3g of potassium persulfate into the solution, and then carrying out magnetic stirring for 60 minutes;
(3) putting the solution into an oil bath kettle preheated to 75 ℃, introducing nitrogen into the solution in the reaction process, and reacting for 5 hours;
(4) cooling the solution to room temperature, then pouring the solution into a beaker, adding 300ml of acetone into the beaker, standing for 20min, carrying out centrifugal treatment, repeatedly adding acetone and centrifuging, finally collecting precipitate and carrying out heat treatment at 60 ℃ for 1000 min, and grinding the obtained solid substance into powder for later use;
(5) adding 3g of the powder obtained in the step (4) into 300ml of deionized water, magnetically stirring for 120 minutes, adding 0.9g of aniline, ultrasonically oscillating for 60 minutes, putting a polyvinylidene fluoride porous membrane into the solution to obtain a solution A, and then putting the solution into ice water;
(6) adding 2g of ammonium persulfate into 20ml of deionized water, carrying out ultrasonic oscillation for 10 minutes, adding the obtained solution into the solution A, and keeping the solution in ice water for reaction for 10 hours;
(7) the polyvinylidene fluoride porous membrane is taken out, washed by deionized water and then put into a drying oven to be dried for 20 minutes at the temperature of 80 ℃.
(8) Depositing silver paste on a polyvinylidene fluoride porous membrane by a screen printing mode, and then carrying out heat treatment at 100 ℃ for 30 minutes;
(9) the finally obtained flexible PVDF/PANI-PAMPS composite membrane can be used as an ammonia gas sensor for performance test, and the test flow comprises the steps of firstly putting the manufactured sensor into a test tube, and extracting NH with certain concentration3The resistance change of the sensor is transmitted to a computer end through Bluetooth equipment, data are stored and processed at the PC end, and a test flow schematic diagram is shown in figure 5; the test results are shown in fig. 1 to 4.
Example 2
(1) The polyvinylidene fluoride porous membrane is respectively cleaned by ultrasonic in acetone and ethanol for 20 minutes, and then is thermally treated in an electric forced air drying oven at 80 ℃ for 20 minutes.
(2) Adding 6g of 2-acrylamide-2-methylpropanesulfonic acid into a three-hole flask filled with 75ml of deionized water, then carrying out magnetic stirring for 100 minutes, adding 1g of potassium persulfate into the solution, and then carrying out magnetic stirring for 60 minutes;
(3) putting the solution into an oil bath kettle preheated to 80 ℃, introducing nitrogen into the solution in the reaction process, and reacting for 3 hours;
(4) cooling the solution to room temperature, then pouring the solution into a beaker, adding 500ml of acetone into the beaker, standing for 20min, carrying out centrifugal treatment, repeatedly adding the acetone and centrifuging, finally collecting the precipitate and carrying out heat treatment at 80 ℃ for 1200 min, and grinding the obtained solid substance into powder for later use;
(5) adding 1g of the powder obtained in the step (4) into 300ml of deionized water, magnetically stirring for 200 minutes, adding 0.5g of aniline, ultrasonically oscillating for 100 minutes, putting a polyvinylidene fluoride porous membrane into the solution to obtain a solution A, and then putting the solution into ice water;
(6) adding 1g of ammonium persulfate into 20ml of deionized water, carrying out ultrasonic oscillation for 10 minutes, adding the obtained solution into the solution A, and keeping the solution in ice water for reaction for 20 hours;
(7) the polyvinylidene fluoride porous membrane was taken out, rinsed with deionized water, and then heat-treated at 40 ℃ for 50 minutes.
(8) Depositing silver conductive ink on a polyvinylidene fluoride porous membrane by an ink-jet printing mode, and then carrying out heat treatment at 100 ℃ for 30 minutes;
(9) and finally, the obtained flexible PVDF/PANI-PAMPS composite membrane can be used as an ammonia gas sensor for performance test, and the test result is very close to that of the embodiment 1.
FIG. 1 shows the result of the response test of the flexible PVDF/PANI-PAMPS composite membrane obtained by the invention as an ammonia gas sensor to ammonia gas with different concentrations, and it can be known from FIG. 1 that the ammonia gas sensor has a detection limit of 30ppb to ammonia gas, thereby greatly improving the detection sensitivity of the ammonia gas sensor; FIG. 2 shows the selectivity test of the flexible PVDF/PANI-PAMPS composite membrane obtained by the invention as an ammonia gas sensor on different gases, and as can be seen from FIG. 2, the ammonia gas sensor has high selectivity on ammonia gas, accurate detection process and high precision; FIG. 3 is a diagram showing resistance change of the flexible PVDF/PANI-PAMPS composite membrane obtained by the invention as an ammonia gas sensor after repeated tests, and FIG. 4 is a diagram showing a long-term Response performance test of the flexible PVDF/PANI-PAMPS composite membrane obtained by the invention as an ammonia gas sensor, wherein the Response (%) is (R-R)0)/R0100%, R is the maximum resistance value reached after ammonia gas is introduced, R0As can be seen from FIGS. 3 and 4, the stability of the invention in ammonia gas testing is very high, and the initial resistance can be kept basically unchanged under multiple and long-term testing conditions. Comprehensively, the ammonia gas sensor of the invention can provide stable, accurate,Sensitive ammonia gas test results, and the existing ammonia gas test method is optimized.
Materials, reagents and experimental equipment related to the embodiment of the invention are all commercial products meeting the field of gas measurement and test if no special description is provided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, modifications and decorations can be made without departing from the core technology of the present invention, and these modifications and decorations shall also fall within the protection scope of the present invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (5)
1. The polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline film ammonia gas sensor is characterized by sequentially comprising a polyvinylidene fluoride layer, a poly (2-acrylamide-2-methylpropanesulfonic acid) doped polyaniline layer and an interdigital electrode layer.
2. The polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline film ammonia gas sensor of claim 1, wherein the poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline layer is grown on the polyvinylidene fluoride porous film layer by an in-situ growth method.
3. The polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline film ammonia gas sensor according to claim 1, wherein the interdigital electrode layer is formed by depositing a conductive material on the polyaniline layer through screen printing, ink-jet printing and sputtering deposition.
4. The polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline film ammonia gas sensor of claim 3, wherein the conductive material is one of a silver conductive ink or a copper conductive ink.
5. A method for preparing the polyvinylidene fluoride/poly (2-acrylamide-2-methylpropanesulfonic acid) -doped polyaniline film ammonia gas sensor as described in any one of claims 1 to 4, which comprises the following steps:
(1) sequentially and respectively soaking a polyvinylidene fluoride porous membrane in ethanol and acetone, and ultrasonically cleaning for 15-20 minutes generally; then heat-treating at 50-150 deg.C for 10-100 min;
(2) adding 1-13g of 2-acrylamide-2-methylpropanesulfonic acid into a container filled with 75ml of deionized water, then carrying out magnetic stirring for 10-300 minutes, adding 1-5g of potassium persulfate into the solution, and then carrying out magnetic stirring for 10-100 minutes;
(3) putting the solution into an oil bath kettle preheated to 50-100 ℃, introducing nitrogen into the solution in the reaction process, and reacting for 1-6 h;
(4) cooling the solution to room temperature, then pouring the solution into a beaker, adding 500ml of acetone into the beaker, standing for 10-60min, carrying out centrifugal treatment, repeating the acetone addition and the centrifugal treatment for one to three times, finally collecting the precipitate, carrying out heat treatment at 40-80 ℃ for 200-1200 min, and grinding the obtained solid substance into powder for later use;
(5) adding 1-10g of the powder obtained in the step (4) into 100-300ml of deionized water, magnetically stirring for 10-300 minutes, adding 0.01-3g of aniline, ultrasonically oscillating for 10-100 minutes, putting the polyvinylidene fluoride porous membrane treated in the step (1) into the solution to obtain a solution A, and putting the solution A into ice water;
(6) adding 1-10g of ammonium persulfate into 20ml of deionized water, carrying out ultrasonic oscillation for 5-100 minutes, adding the obtained solution into the solution A, and keeping the solution in ice water for reaction for 5-30 hours;
(7) taking out the polyvinylidene fluoride porous membrane, washing with deionized water, and then carrying out heat treatment at 30-150 ℃ for 1-10 h;
(8) depositing one of silver conductive ink and copper conductive ink on the polyvinylidene fluoride porous membrane by screen printing, ink-jet printing or sputtering, and then carrying out heat treatment at 40-200 ℃ for 30-200 minutes.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170082565A1 (en) * | 2011-09-16 | 2017-03-23 | The Research Foundation For The State University Of New York | Low concentration ammonia nanosensor |
| CN109613069A (en) * | 2018-11-12 | 2019-04-12 | 中国科学院宁波材料技术与工程研究所 | A kind of PVDF/PANI composite and flexible ammonia gas sensor and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170082565A1 (en) * | 2011-09-16 | 2017-03-23 | The Research Foundation For The State University Of New York | Low concentration ammonia nanosensor |
| CN109613069A (en) * | 2018-11-12 | 2019-04-12 | 中国科学院宁波材料技术与工程研究所 | A kind of PVDF/PANI composite and flexible ammonia gas sensor and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 王超: ""高电导率改性聚苯胺的合成新工艺"", 《技术与教育》 * |
| 谢英男等: ""磺酸掺杂聚苯胺的氨敏性能"", 《化工新型材料》 * |
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