CN115856203A - Preparation method of ammonia gas sensor based on aniline and tin oxide gas-sensitive composite material - Google Patents
Preparation method of ammonia gas sensor based on aniline and tin oxide gas-sensitive composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material, which comprises the following steps: 1. adding deionized water into tin chloride to prepare a tin chloride solution, and adjusting the pH value of the tin chloride solution by using a hydrochloric acid solution; 2. mixing a tin chloride solution and a hydrogen peroxide solution to obtain a white suspension; 3. aniline and ammonium persulfate are mixed and then added into the white suspension to be mixed to generate polyaniline; 4. carrying out polymerization reaction on polyaniline in ice bath to obtain aniline and tin oxide composite suspension; 5. repeatedly washing the aniline and tin oxide composite suspension with hydrochloric acid solution, and drying to obtain an aniline and tin oxide gas-sensitive composite material; 6. coating the PCF with an aniline and tin oxide gas-sensitive composite material; 7. and splicing two ends of the PCF between the two optical fibers to form the ammonia gas sensor. According to the invention, the PCF is wrapped by the aniline and tin oxide gas-sensitive composite material, so that the response speed for detecting low-concentration ammonia gas at room temperature is high.
Description
Technical Field
The invention relates to a preparation method of a gas-sensitive material, in particular to a preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material.
Background
In recent years, the problem of air pollution is receiving more and more attention, and the detection of pollutants such as toxic and harmful gases in the air becomes an important link of environmental monitoring. The ammonia gas is a common toxic gas, has obvious influence on climate change, is colorless, has irritant malodor, and can damage human health through respiratory system, eyes, skin and the like.
Conventional gas sensors generally employ N-type semiconductor metal oxides as gas-sensitive materials, such as: tin oxide (SnO) 2 ) Zinc oxide (ZnO), tungsten oxide (WO) 3 ) Titanium oxide (TiO) 2 ) However, the use of the conventional gas sensor at room temperature is greatly limited due to the high working temperature (150-200 ℃), and the detection function and the detection precision cannot be guaranteed.
The chinese invention patent application CN201811608197.1 discloses a flexible conductive film with gas sensitivity and its application, and specifically discloses: a PET (Polyethylene terephthalate) film having a thickness of 0.1mm was cut out to have a surface area of 0.49cm 2 The square thin film is coated with 0.5-1.5mg of rod-shaped tungsten trioxide, the preferred size of the tungsten trioxide is 10-20nm in diameter and 1.5-2 mu m in length, aniline and tungsten trioxide are mixed according to the weight ratio of 1 to 2, and aniline is attached to acidic active sites on the surface of the tungsten trioxide to polymerize to form protonated polyaniline in an acidic solution under the catalysis of ammonium persulfate, so that the flexible conductive thin film is prepared. However, since tungsten (W) is sensitive to the environment and has a variable valence state, the flexible conductive thin film has poor stability and reaction recovery, and is limited in use.
Chinese patent application CN201811540011.3 discloses a flexible exhaled ammonia gas sensor based on a porous substrate and a preparation method thereof, and specifically discloses: the flexible exhaled ammonia gas sensor comprises a substrate, a sensitive film covering the substrate and electrodes arranged on two sides of the sensitive film, wherein the flexible ammonia gas sensitive film with strong moisture resistance is made of a conductive organic polymer material or a conductive organic polymer composite material doped with metal oxide. The conductive organic polymer material is polyaniline PANI or polypyrrole PPy or 3, 4-polyethylene dioxythiophene PEDOT, and the metal oxide is zinc oxide ZnO or stannic oxide SnO 2 Or tungsten trioxide WO 3 Or titanium oxide TiO 2 Or indium oxide In 2 O 3 . The coating type sensor has more complex design steps and higher cost.
Disclosure of Invention
The invention aims to provide a preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material, which is characterized in that the aniline and tin oxide gas-sensitive composite material is used for wrapping PCF (photonic Crystal Fibers), and the ammonia gas sensor has a fast response speed to the detection of low-concentration ammonia gas at room temperature.
The invention is realized in the following way:
a preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material comprises the following steps:
step 1: adding tin chloride into deionized water to prepare a tin chloride solution, and adjusting the pH value of the tin chloride solution by using a hydrochloric acid solution;
step 2: uniformly mixing the tin chloride solution with the adjusted pH value and a hydrogen peroxide solution to obtain a white suspension;
and step 3: aniline and ammonium persulfate are mixed and then added into the white suspension, and the mixture is mixed and stirred to generate polyaniline;
and 4, step 4: carrying out polymerization reaction on polyaniline in ice bath to obtain aniline and tin oxide composite suspension;
and 5: repeatedly washing the aniline and tin oxide composite suspension by using a hydrochloric acid solution, and drying to obtain an aniline and tin oxide gas-sensitive composite material;
step 6: coating the PCF with the aniline and tin oxide gas-sensitive composite material;
and 7: and splicing two ends of the PCF between the two optical fibers to form the ammonia gas sensor.
In the step 1, the concentration of the tin chloride solution is 0.003mol/L, and the molar concentration of the hydrochloric acid solution is 0.1M; the pH value of the tin chloride solution is adjusted to 3.8-4.2.
In the step 2, the mixing volume ratio of the tin chloride solution and the hydrogen peroxide solution after the pH value is adjusted is 5; the concentration of the hydrogen peroxide solution is 2-5%.
In the step 3, the mixing mass ratio of aniline to ammonium persulfate is 2-3, and the molar ratio of aniline to tin chloride in the white suspension is 30-50.
In the step 4, the temperature of the polymerization reaction in ice bath is 0-10 ℃, and the time of the polymerization reaction is 50-70min.
In the aniline and tin oxide gas-sensitive composite material, the mass ratio of aniline to tin oxide is 4-9.
The method for coating the PCF with the aniline and tin oxide gas-sensitive composite material comprises the following steps:
step 6.1: cleaning the surface of the PCF by adopting the mixed solution;
step 6.2: washing PCF with deionized water for several times and drying;
step 6.3: immersing PCF into a silane coupling agent solution for surface modification;
step 6.4: drying PCF in nitrogen atmosphere;
step 6.5: preparing the aniline and tin oxide gas-sensitive composite material into mixed slurry with the concentration of 20-30% by using ethanol and sodium lignosulphonate, dipping the PCF into the mixed slurry, and drying at room temperature.
In the step 6.1, the mixed solution is formed by mixing 1mg of potassium dichromate, 0.1ml of deionized water and 10ml of concentrated sulfuric acid, and the time for processing the PCF by the mixed solution is 10min;
in the step 6.3, the silane coupling agent solution is prepared by mixing 1-3ml of APTMS, 4ml of acetic acid and 10ml of ethanol.
In the step 6.2, the drying temperature is 115 ℃, and the drying time is 2h;
in the step 6.4, the nitrogen temperature in the nitrogen environment is 100 ℃, and the drying time is 1h;
in the step 6.5, the PCF is soaked for 1-5h, and the room temperature drying time is 6-18h; in the mixed slurry, the content of the sodium lignosulfonate accounts for 5-8% of the content of the ethanol.
The ammonia gas sensor has the response time of 7-8s to 0-8ppm ammonia gas at normal temperature, the recovery time of 2-3s and the lowest detection limit of ammonia gas concentration of 8ppt.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the aniline layer is compounded on the surface of the tin oxide to obtain the aniline and tin oxide gas-sensitive composite material, and the aniline and tin oxide gas-sensitive composite material is coated on the surface of the PCF, so that the specific surface area is large, the ammonia gas sensor has the advantages of high selectivity, high stability and the like, the response time is short, and the energy consumption can be reduced.
2. The preparation method disclosed by the invention is simple, low in cost, mild in reaction conditions, good in controllability of the reaction process and good in application and popularization prospects.
The PCF surface is coated with the aniline and tin oxide gas-sensitive composite material, so that the PCF surface has a large specific surface area, is high in response speed and recovery speed for detecting low-concentration ammonia at room temperature, is high in stability, has a minimum detection limit of 8ppt for ammonia concentration, can effectively and accurately detect the content of the low-concentration ammonia at room temperature, and has the advantages of strong repeatability, low cost and the like.
Drawings
FIG. 1 shows the results of the selectivity tests of the ammonia gas sensor on different gases, which are prepared by the ammonia gas sensor preparation method based on the aniline and tin oxide gas-sensitive composite material of the invention; in the figure, I is ammonia gas, II is nitrogen gas, III is oxygen gas, IV is methane, V is hydrogen gas, VI is hydrogen sulfide, and the ordinate is the detection concentration;
fig. 2 shows the response and recovery time performance of the ammonia gas sensor prepared by the method for preparing an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material, wherein the abscissa shows the reaction time under different concentrations, the time from the lowest end to the highest peak in each waveform section is the response time, the time from the highest peak to the lowest end is the recovery time, and the ordinate shows the wavelength.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
A preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material comprises the following steps:
step 1: adding stannic chloride (SnCl) 4 ·5H 2 O) is added into deionized water to prepare a tin chloride solution, the pH value of the tin chloride solution is adjusted by hydrochloric acid solution HCl, if the pH value is too high, sn is easy to form a coordination complex, and otherwise, if the pH value is too low, sn is easy to precipitate quickly.
The concentration of the tin chloride solution is 0.003mol/L, and the molar concentration of the hydrochloric acid solution is 0.1M.
The pH value of the tin chloride solution is adjusted to 3.8-4.2.
Step 2: mixing the pH-adjusted stannic chloride solution and hydrogen peroxide solution H 2 O 2 Mix well to obtain a white suspension. Addition of H 2 O 2 Oxidizing tin chloride to obtain Sn 2+ Oxidized to Sn 4+ 。
Preferably, the hydrogen peroxide solution H 2 O 2 The concentration of (2-5%), if the concentration of the hydrogen peroxide solution is too high, the oxidation is too fast, which easily causes tin chloride agglomeration, whereas if the concentration of the hydrogen peroxide solution is too low, the reaction is too slow and the reaction time is longer.
The tin chloride solution and the hydrogen peroxide solution H after the pH value is adjusted 2 O 2 The mixing volume ratio of (1) is 5. If H is 2 O 2 Too high a proportion of (A) leads to agglomeration of tin chloride easily due to too rapid oxidation, whereas if H is added 2 O 2 The mixture ratio of (A) is too low, the reaction is too slow, and the reaction time is longer.
And step 3: aniline and Ammonium Persulfate (APS) are mixed and then added into the white suspension, and the mixture is mixed and stirred to generate polyaniline. Aniline and APS are mixed firstly, so that aniline and peroxydisulfate can be fully adsorbed, and polyaniline polymerization reaction is facilitated. If aniline and ammonium persulfate are added directly to the white suspension, the Sn will be oxidized first by the ammonium persulfate 2+ Resulting in too rapid oxidation. Aniline has the advantages of high conductivity, easy synthesis, high stability, etc., and has moderate sensitivity and selectivity to ammonia gas.
The mixing mass ratio of the aniline to the Ammonium Persulfate (APS) is 2-3, so that adsorption balance, polymerization balance and coordination balance can be ensured, the molar ratio of the aniline to tin chloride in the white suspension is 30-50.
And 4, step 4: polyaniline is polymerized in ice bath to obtain aniline and tin oxide (PANI @ SnO) 2 ) And (4) compounding the suspension.
The temperature of the polymerization reaction in the ice bath is 0-10 ℃, and the time of the polymerization reaction is 50-70min, so that the molecular weight distribution of the polymerized polymer is ensured to be uniform.
And 5: para-aniline and tin oxide (PANI @ SnO) with hydrochloric acid solution HCl 2 ) Repeatedly washing the composite suspension, and drying to obtain aniline and tin oxide (PANI @ SnO) 2 ) A gas-sensitive composite material. By repeated washing, unreacted monomers, e.g. aniline, sn, can be removed 2+ And the like.
The molar concentration of the hydrochloric acid solution is 1M.
Step 6: mixing aniline and tin oxide (PANI @ SnO) 2 ) The air-sensitive composite material is coated on the PCF made of zinc oxide (ZnO).
The aniline and the tin oxide (PANI @ SnO) 2 ) In the air-sensitive composite material, aniline PANI and tin oxide SnO 2 The mass ratio of (A) to (B) is 4-9, and aniline and tin oxide (PANI @ SnO) 2 ) The coating thickness of the gas-sensitive composite material on the surface of PCF is 500-800nm, so that the surface is coated with aniline and tin oxide (PANI @ SnO) 2 ) PCF of the gas-sensitive composite material has good performance at room temperatureSelectivity and stability.
Aniline and tin oxide (PANI @ SnO) 2 ) The method for coating the PCF with the gas-sensitive composite material comprises the following steps:
step 6.1: and (3) carrying out surface cleaning treatment on the PCF by using the mixed solution.
The mixed solution is formed by mixing 1mg of potassium dichromate, 0.1ml of deionized water and 10ml of concentrated sulfuric acid, and the surface cleaning treatment time of the PCF by the mixed solution is 10min. Wherein, the concentrated sulfuric acid can adopt the commercial concentrated sulfuric acid with the concentration of about 98 percent.
Step 6.2: and washing the PCF with deionized water for several times, removing impurities, preferably 3 times, and drying at 115 ℃ for 2h to achieve the purposes of cleaning the surface and texturing the surface.
Step 6.3: and (3) immersing the PCF into a silane coupling agent solution for surface modification.
The silane coupling agent solution is formed by mixing 1-3ml of APTMS (3-aminopropyl trimethoxysilane), 4ml of acetic acid and 10ml of ethanol.
Step 6.4: the PCF was dried in a nitrogen atmosphere.
The temperature of the nitrogen in the nitrogen environment is 100 ℃, the drying time is 1h, and the compound and the matrix are firmly bonded by blowing and drying.
Step 6.5: preparing the aniline and tin oxide gas-sensitive composite material into mixed slurry with the concentration of 20-30% by using ethanol and sodium lignosulphonate, dipping the mixed slurry in PCF, and drying at room temperature.
In the mixed slurry, the content of the sodium lignosulphonate accounts for 5-8% of the content of the ethanol.
The PCF is soaked for 1-5h, and dried for 6-18h at room temperature.
And 7: and splicing two ends of the PCF between the two optical fibers to form the ammonia gas sensor.
The PCF has a length of 2cm, and preferably, the PCF can be spliced between two fibers by using a fiber fusion splicer, and the conducting structure of the PCF is an SPS (Sandwich Plate System, i.e. a Sandwich structure) spliced by SMF-PCF-SMF.
Please refer to fig. 1, in whichAt normal temperature, compared with other gases such as nitrogen, oxygen, methane, hydrogen sulfide and the like, the ammonia gas sensor prepared by the method has strong selectivity on ammonia gas. Referring to the attached FIG. 2, the ammonia gas sensor prepared by the invention has a concentration of 0-8ppm (1ppm = 10) at normal temperature 3 ppb,1ppm = parts per million) ammonia gas, the waveforms in the figure being, in order: a test waveform of ammonia gas at a concentration of 1ppb, a test waveform of ammonia gas at a concentration of 2ppb, a test waveform of ammonia gas at a concentration of 3ppb, a test waveform of ammonia gas at a concentration of 6ppb, and a test waveform of ammonia gas at a concentration of 8 ppb. As can be seen from figure 2, the ammonia gas sensor prepared by the invention has the response time of 7-8s to ammonia gas with the concentration of 0-8ppm at normal temperature, the recovery time of 2-3s, the response speed is high, and the lowest detection limit of the ammonia gas concentration is 8ppt (1ppm = 10) 6 ppt,1ppm = parts per million).
Example 1:
step 1: 0.1g of tin chloride (SnCl) 4 ·5H 2 O) was added to 100ml of deionized water to prepare a 0.003mol/L tin chloride solution, and the pH of the tin chloride solution was adjusted with 0.1M HCl hydrochloride solution to achieve a tin chloride solution pH =4.
Step 2: mixing the tin chloride solution after pH value adjustment with 20ml of hydrogen peroxide solution H according to a volume ratio of 5 2 O 2 Mix well to obtain white suspension.
The tin chloride solution and the hydrogen peroxide solution H after the pH value is adjusted 2 O 2 The mixing volume ratio of (1).
And step 3: 0.9g of aniline and 100ml of Ammonium Persulfate (APS) with the molar concentration of 0.1M are mixed according to the mass ratio of 2. The molar ratio of aniline to tin chloride was 30.
And 4, step 4: and (3) carrying out polymerization reaction on polyaniline in an ice bath at 5 ℃ for 60min to obtain aniline and tin oxide composite suspension.
And 5: and repeatedly washing the aniline and tin oxide composite suspension by hydrochloric acid solution HCl with the molar concentration of 1M, and drying to obtain the aniline and tin oxide gas-sensitive composite material.
Step 6: and coating the PCF with the aniline and tin oxide gas-sensitive composite material, wherein the coating thickness is 500nm.
Step 6.1: the surface of PCF was cleaned with a mixed solution of 1mg potassium dichromate, 0.1ml deionized water and 10ml concentrated sulfuric acid for 10min. The concentration of concentrated sulfuric acid is 98%.
Step 6.2: the PCF was washed 3 times with deionized water and dried at 115 ℃ for 2h.
Step 6.3: PCF is immersed in silane coupling agent solution formed by mixing 1ml of APTMS, 4ml of acetic acid and 10ml of ethanol for surface modification.
Step 6.4: the PCF was dried for 1h at 100 ℃ under nitrogen.
Step 6.5: preparing a 25% mixed slurry of aniline and tin oxide gas-sensitive composite material by using ethanol and sodium lignosulphonate (5% of the content of the ethanol), soaking the mixed slurry in PCF for 3 hours, and drying the mixed slurry at room temperature for 12 hours.
And 7: and splicing two ends of the PCF with the length of 2cm between the two SMF-28 optical fibers by adopting an optical fiber fusion splicer to form the ammonia gas sensor, wherein the conductive structure of the ammonia gas sensor is the SPS spliced by the SMF-PCF-SMF.
The ammonia gas sensor prepared by the embodiment has the response time of 7s to 0-8ppm ammonia gas at normal temperature, the recovery time of 2s and high response speed.
Example 2:
step 1: 0.1g of tin chloride (SnCl) 4 ·5H 2 O) was added to 100ml of deionized water to prepare a 0.003mol/L tin chloride solution, and the pH of the tin chloride solution was adjusted with 0.1M HCl hydrochloride solution to achieve a pH =4.
Step 2: mixing the tin chloride solution after pH value adjustment with 20ml of hydrogen peroxide solution H according to a volume ratio of 5 2 O 2 Mix well to obtain white suspension.
The tin chloride solution and the hydrogen peroxide solution H after the pH value is adjusted 2 O 2 The mixing volume ratio of (1).
And step 3: mixing 1.35g of aniline and 100ml of Ammonium Persulfate (APS) with the molar concentration of 0.1M according to the mass ratio of 2. The molar ratio of aniline to tin chloride was 30.
And 4, step 4: and (3) carrying out polymerization reaction on polyaniline in an ice bath at 5 ℃ for 60min to obtain aniline and tin oxide composite suspension.
And 5: and repeatedly washing the aniline and tin oxide composite suspension by hydrochloric acid solution HCl with the molar concentration of 1M, and drying to obtain the aniline and tin oxide gas-sensitive composite material.
Step 6: the PCF is coated with the aniline and tin oxide gas-sensitive composite material, and the coating thickness is 500nm.
Step 6.1: the surface of PCF was cleaned with a mixed solution of 1mg potassium dichromate, 0.1ml deionized water and 10ml concentrated sulfuric acid for 10min. The concentration of concentrated sulfuric acid is 98%.
Step 6.2: the PCF was washed 3 times with deionized water and dried at 115 ℃ for 2h.
Step 6.3: PCF is immersed in silane coupling agent solution formed by mixing 1ml of APTMS, 4ml of acetic acid and 10ml of ethanol for surface modification.
Step 6.4: the PCF was dried for 1h at 100 ℃ under nitrogen.
Step 6.5: preparing a 30% mixed slurry of aniline and tin oxide gas-sensitive composite material by using ethanol and sodium lignosulphonate (8% of the content of the ethanol), soaking the mixed slurry in PCF for 3 hours, and drying the mixed slurry at room temperature for 12 hours.
And 7: and splicing two ends of the PCF with the length of 2cm between the two SMF-28 optical fibers by adopting an optical fiber fusion splicer to form the ammonia gas sensor, wherein the conductive structure of the ammonia gas sensor is the SPS spliced by the SMF-PCF-SMF.
The ammonia gas sensor prepared by the embodiment has the response time of 8s to 0-8ppm ammonia gas at normal temperature, the recovery time of 3s and high response speed.
The present invention is not limited to the above embodiments, and therefore, any modifications, equivalents, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of an ammonia gas sensor based on an aniline and tin oxide gas-sensitive composite material is characterized by comprising the following steps: the method comprises the following steps:
step 1: adding tin chloride into deionized water to prepare a tin chloride solution, and adjusting the pH value of the tin chloride solution by using a hydrochloric acid solution;
and 2, step: uniformly mixing the tin chloride solution with the adjusted pH value with a hydrogen peroxide solution to obtain a white suspension;
and step 3: aniline and ammonium persulfate are mixed and then added into the white suspension, and the mixture is mixed and stirred to generate polyaniline;
and 4, step 4: carrying out polymerization reaction on polyaniline in ice bath to obtain aniline and tin oxide composite suspension;
and 5: repeatedly washing the aniline and tin oxide composite suspension by using a hydrochloric acid solution, and drying to obtain an aniline and tin oxide gas-sensitive composite material;
step 6: coating the PCF with an aniline and tin oxide gas-sensitive composite material;
and 7: and splicing two ends of the PCF between the two optical fibers to form the ammonia gas sensor.
2. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: in the step 1, the concentration of the tin chloride solution is 0.003mol/L, and the molar concentration of the hydrochloric acid solution is 0.1M; the pH value of the tin chloride solution is adjusted to 3.8-4.2.
3. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: in the step 2, the mixing volume ratio of the tin chloride solution and the hydrogen peroxide solution after the pH value is adjusted is 5; the concentration of the hydrogen peroxide solution is 2-5%.
4. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: in the step 3, the mixing mass ratio of aniline to ammonium persulfate is 2-3, and the molar ratio of aniline to tin chloride in the white suspension is 30-50.
5. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: in the step 4, the temperature of the polymerization reaction in the ice bath is 0-10 ℃, and the time of the polymerization reaction is 50-70min.
6. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: in the aniline and tin oxide gas-sensitive composite material, the mass ratio of aniline to tin oxide is 4-9.
7. The method for preparing the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material of claim 1 or 6, which is characterized in that: the method for coating the PCF with the aniline and tin oxide gas-sensitive composite material comprises the following steps:
step 6.1: cleaning the surface of the PCF by adopting the mixed solution;
step 6.2: washing PCF with deionized water for several times and drying;
step 6.3: immersing PCF into a silane coupling agent solution for surface modification;
step 6.4: drying PCF in nitrogen atmosphere;
step 6.5: preparing the aniline and tin oxide gas-sensitive composite material into mixed slurry with the concentration of 20-30% by using ethanol and sodium lignosulphonate, dipping the PCF into the mixed slurry, and drying at room temperature.
8. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material of claim 7, which is characterized in that: in the step 6.1, the mixed solution is formed by mixing 1mg of potassium dichromate, 0.1ml of deionized water and 10ml of concentrated sulfuric acid, and the time for processing the PCF by the mixed solution is 10min;
in the step 6.3, the silane coupling agent solution is prepared by mixing 1-3ml of APTMS, 4ml of acetic acid and 10ml of ethanol.
9. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material of claim 7, which is characterized in that: in the step 6.2, the drying temperature is 115 ℃, and the drying time is 2 hours;
in the step 6.4, the nitrogen temperature in the nitrogen environment is 100 ℃, and the drying time is 1h;
in the step 6.5, the PCF is soaked for 1-5h, and the room temperature drying time is 6-18h; in the mixed slurry, the content of the sodium lignosulfonate accounts for 5-8% of the content of the ethanol.
10. The preparation method of the ammonia gas sensor based on the aniline and tin oxide gas-sensitive composite material as claimed in claim 1, which is characterized in that: the ammonia gas sensor has the response time of 7-8s to 0-8ppm ammonia gas at normal temperature, the recovery time of 2-3s and the lowest detection limit of ammonia gas concentration of 8ppt.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651828A (en) * | 2016-01-19 | 2016-06-08 | 武汉工程大学 | Gas sensor based on polyaniline/stannic oxide composite nanofibers and preparation method thereof |
| CN108956717A (en) * | 2018-09-07 | 2018-12-07 | 吉林大学 | One kind being based on PANI@SnO2The flexible flat formula ammonia gas sensor of nano sensitive material and its application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651828A (en) * | 2016-01-19 | 2016-06-08 | 武汉工程大学 | Gas sensor based on polyaniline/stannic oxide composite nanofibers and preparation method thereof |
| CN108956717A (en) * | 2018-09-07 | 2018-12-07 | 吉林大学 | One kind being based on PANI@SnO2The flexible flat formula ammonia gas sensor of nano sensitive material and its application |
Non-Patent Citations (2)
| Title |
|---|
| ANAND M. SHRIVASTAV等: "Hypersensitive and Selective Interferometric Nose for Ultratrace Ammonia Detection with Fast Response Utilizing PANI@SnO2 Nanocomposite", ACS PHOTONICS, vol. 5, no. 11, 28 September 2018 (2018-09-28), pages 2 - 3 * |
| 蒋娟等: "聚苯胺及其氧化锡复合材料的气敏特性研究", 传感技术学报, vol. 26, no. 12, 15 December 2013 (2013-12-15), pages 1655 - 1660 * |
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