CN104697879A - Polyaniline/titanium dioxide film QCM gas sensor and preparation method of gas sensor - Google Patents
Polyaniline/titanium dioxide film QCM gas sensor and preparation method of gas sensor Download PDFInfo
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Abstract
The invention discloses a polyaniline/titanium dioxide film QCM gas sensor and a preparation method of the gas sensor. The preparation method includes the following steps: 10MHz AT-cut quartz crystal microbalance (QCM) is regarded as a substrate; a gas sensor film is prepared by adopting an electrostatic layer-by-layer assembly method for a polyaniline/titanium dioxide nanocomposite, and a polyaniline/titanium dioxide nanocomposite frequency film gas sensor is prepared after moisture is removed through heat treatment. Sensitivity and resolution of measured frequency signals are far better than these of resistance signals, and the room temperature gas sensitivity response of elements can be greatly improved through polymerized nanocomposite polyaniline/titanium dioxide assembly layers. According to the preparation method, the process is simple in process, the cost is low, and the gas sensor is particularly applied to batch production. The gas sensor has high response sensitivity and good resilience for ammonia gas and hydrogen sulfide, and can be used for detection at the room temperature and can retain long term stability, and thus the gas sensor can be widely used for precisely measuring and controlling the room temperature of the low-concentration toxic gas in industrial and agricultural production processes and atmospheric environment.
Description
Technical field
The present invention relates to a kind of polyaniline/titanium dioxide frequency type film gas sensor based on QCM (Quartz Crystal Microbalance) substrate (QCM) and preparation method thereof.
Background technology
Gas sensor is the important chemical sensor of a class, has a wide range of applications in storage, commercial production, process control, environmental monitoring etc., and plays a part to become more and more important in modern development in science and technology and people's life.Constantly pursue high-performance, low cost, small size etc. become a sensor difficult problem urgently to be resolved hurrily.The simultaneously introducing of new material new technology and innovation, make these difficult problems of solution become possibility.Traditional gas sensor sensitive material has inorganic semiconductor material and the large class of organic conductive polymer two usually.Inorganic semiconductor material needs just to be used under the high temperature conditions to detect gas (just can have good vapor sensitivity under often needing that sensor element is heated to the operating temperature of hundreds of degree Celsius) usually, but high temperature detects and brings much inconvenience to the operation of reality, the gas sensor that research and development high sensitivity has again room temperature response characteristic seems particularly important.Conducting polymer is again because its long-time stability, and the factors such as sensitivity is low limit its widespread use.
Summary of the invention
The object of this invention is to provide a kind of polyaniline/titanium dioxide film QCM gas sensor and preparation method thereof.
A kind of polyaniline/titanium dioxide film QCM gas sensor, take QCM as matrix, evaporation on matrix surface, the symmetrical gold electrode of photoetching, gold electrode is connected with lead-in wire, quartz crystal matrix and gold electrode surfaces are coated with air-sensitive film, and air-sensitive film is the self-assembled nanometer compound of polyaniline/titanium dioxide.
Described quartz crystal matrix is AT cut type, and fundamental frequency is 10MHz.
Described air-sensitive film is obtained by the polyaniline adulterated with QCM upper substrate layer layer electrostatic self-assembled titanium dioxide nano-particle and the polystyrolsulfon acid of modified.
The method of modifying of described QCM substrate, step is as follows:
1) QCM substrate Pierre's card agent treated 10 ~ 30 min, makes it bring the negative charge groups such as carboxyl, and substrate deionization drip washing 1 ~ 2 min handled well is dried up with nitrogen;
2) immerse 5 ~ 10 min, taking-up deionization drip washing 1 ~ 2 min in 1 ~ 3%wt PDDA (PDDA) aqueous solution also to dry up with nitrogen;
3) substrate is immersed 5 ~ 10 min in kayexalate (PSS) again, taking-up deionization drip washing 1 ~ 2 min also dries up with nitrogen;
4) step 2 is repeated again successively) and step 3) 2 ~ 3 times, make on-chip gold electrode modify upper 2 ~ 5 double-deck PDDA and PSS, obtain the QCM substrate of modified.
5. gas sensor according to claim 3, is characterized in that: described self assembly step is as follows:
5) the QCM substrate of modified is immersed titanium dioxide nano-particle aqueous solution 5 ~ 10 min of 1 ~ 3 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
6) the QCM substrate of modified is immersed polyaniline aqueous solution 5 ~ 10 min of the polystyrolsulfon acid doping of 1 ~ 3 mg/mL, adulterate by styrene sulfonic acid monomer and aniline monomer mol ratio 1:1, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
7) step 5) and step 6) 10 ~ 40 times is repeated successively again, QCM substrate is made to modify upper 10 ~ 40 double-deck polyanilines and titania, directly dry up without drip washing after the self assembly of last one deck polyaniline, obtained polyaniline/titanium dioxide combination frequency type film gas sensor.
A preparation method for described gas sensor, step is as follows:
1) QCM substrate Pierre's card agent treated 10 ~ 30 min, makes it bring the negative charge groups such as carboxyl, and substrate deionization drip washing 1 ~ 2 min handled well is dried up with nitrogen;
2) immerse 5 ~ 10 min, taking-up deionization drip washing 1 ~ 2 min in 1 ~ 3%wt PDDA (PDDA) aqueous solution also to dry up with nitrogen;
3) substrate is immersed 5 ~ 10 min in kayexalate (PSS) again, taking-up deionization drip washing 1 ~ 2 min also dries up with nitrogen;
4) step 2 is repeated again successively) and step 3) 2 ~ 3 times, make on-chip gold electrode modify upper 2 ~ 5 double-deck PDDA and PSS, obtain the QCM substrate of modified;
5) the QCM substrate of modified is immersed titanium dioxide nano-particle aqueous solution 5 ~ 10 min of 1 ~ 3 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
6) the QCM substrate of modified is immersed polyaniline aqueous solution 5 ~ 10 min of the polystyrolsulfon acid doping of 1 ~ 3 mg/mL, adulterate by styrene sulfonic acid monomer and aniline monomer mol ratio 1:1, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
7) step 5) and step 6) 10 ~ 40 times is repeated successively again, QCM substrate is made to modify upper 10 ~ 40 double-deck polyanilines and titania, directly dry up without drip washing after the self assembly of last one deck polyaniline, obtained polyaniline/titanium dioxide combination frequency type film gas sensor.
the invention has the beneficial effects as follows:
1) the polyaniline/titanium dioxide compound sensitive membrane prepared by has very thin thickness (100 ~ 600 nm), (10 ~ 60 s) to make sensor have very high sensitivity (can have accurate response to the gas of 10ppm, frequency change is 10Hz-20Hz) and pole short response time;
2) adopt LBL self-assembly legal system for polyaniline/titanium dioxide compound sensitive membrane, the method is simple to operate, with low cost, simple.And by controlling the number of plies of self assembly, can control the thickness preparing sensitive membrane accurately, thus reach adjustment sensor sensing performance;
3) have certain water-soluble with the polyaniline of polystyrolsulfon acid doping, well can be dispersed in water, solve the unmanageable difficulty of polyaniline;
4) prepare titanium dioxide nano-particle with sol-gal process, well can control size and the concentration of growth nano-particle, and can stable existence some months in aqueous;
5) sensitive membrane adopting LBL self-assembly to prepare is highly stable, and has good adhesiveness on QCM substrate, and make device after use some months, its performance is also very stable.
Accompanying drawing explanation
Fig. 1 is the self assembly XRD collection of illustrative plates of the polyaniline/titanium dioxide composite sensitive film described in the embodiment of the present invention;
Fig. 2 is the self assembly FTIR collection of illustrative plates of the polyaniline/titanium dioxide composite sensitive film described in the embodiment of the present invention;
Fig. 3 is polyaniline and the double-deck effect diagram to qcm sensor response characteristic of titania of the different number of plies of self assembly described in the embodiment of the present invention;
Fig. 4 is that the QCM gas sensor of preparation described in the embodiment of the present invention is to the dynamic response figure of NH3;
Fig. 5 be the sensor prepared described in the embodiment of the present invention respectively to ethanol, sulfuretted hydrogen, the resonse characteristic figure of trimethylamine.
Embodiment
The invention provides polyaniline/titanium dioxide frequency type film gas sensor that one is base based on QCM (Quartz Crystal Microbalance) (QCM) and preparation method thereof.The present invention is further illustrated below in conjunction with drawings and Examples.This polyaniline/titanium dioxide frequency type film gas sensor, air-sensitive film is the nano-complex film of polyaniline and titania, and it is obtained on QCM substrate by polyaniline and titania self assembly layer by layer.Layer upon layer electrostatic self assembly a kind ofly utilizes the electrostatic attraction between material to prepare the self-assembled composite film of nano-level.Utilize this technology can prepare the nano-complex of polyaniline and titania easily, thus increase its complex effect.
Embodiment
The present embodiment is that 8M Hz AT cuts gas sensor for example with fundamental frequency, according to the content synthesized polyaniline/titania sensitive membrane described in claims, and the relevant corresponding QCM gas sensor of preparation.Concrete preparation method processed is as described below:
1) QCM substrate cleaning
First by ready QCM substrate through absolute ethyl alcohol and acetone soaking and washing 2 hours, dry 3 hours, for subsequent use.
2) modification of QCM substrate
1. say ready QCM substrate Pierre's card agent treated 10 min, make it bring the negative charge groups such as carboxyl, QCM substrate deionization drip washing 1 min handled well is dried up with nitrogen.2. immerse 5 min, taking-up deionization drip washing 1 min in 1%wt PDDA (PDDA) aqueous solution also to dry up with nitrogen.3. QCM substrate is immersed 5 min in kayexalate (PSS) again, taking-up deionization drip washing 1 min also dries up with nitrogen.Repeat step 2 and step 3 twice successively, make QCM substrate modify upper two double-deck PDDA and PSS, obtain the QCM substrate of modified.
3) polyaniline/titanium dioxide compound gas sensor preparation
1. the QCM substrate of modified is immersed titanium dioxide nano-particle aqueous solution 5 min of 1 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 min of 1.5 and dries up with nitrogen.2. the QCM substrate of modified is immersed polyaniline (adulterating by styrene sulfonic acid monomer and aniline monomer mol ratio 1:1) aqueous solution 5 min of the polystyrolsulfon acid doping of 1 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 min of 1.5 and dries up with nitrogen.Repeat step 1 and step 2 10 times successively, make QCM substrate modify upper 10 double-deck polyanilines and titania, directly dry up without drip washing after the self assembly of last one deck polyaniline, obtained polyaniline/titanium dioxide combination frequency type film gas sensor.
4) nano composite material of preparation is characterized.
Repeat step 1), 2) and 3) method on potsherd, apply the dispersing polyaniline liquid and titanium oxide dispersion that prepare respectively, for the sign of original solution X-ray diffraction.These two kinds of characterization results for the synthesis of material as shown in Figure 1.Clearly, polyaniline and titania show its characteristic of correspondence peak.Wherein polyaniline has obvious peak at about 22 degree, but whether very strong, and wider.This is the not obvious and performance of confusion of polyaniline molecule chain crystallization.There is not any characteristic peak in TiO 2 particles, illustrates that TiO 2 particles is still amorphous state, do not generate crystal formation.
With self assembly last layer PDDA again on the silicon plate of three bilayer (PDDA/PSS) 3 modifieds, make silicon plate surface band positive electricity.Because with a large amount of negative charge on the polyaniline chain adulterated with PSSA, then last layer PANI-PSSA can be adsorbed by electrostatic self-assembled on silicon plate.Observe homogeneity and the surface topography of the film of individual layer PANI-PSSA particle assembling, its result is as shown in Fig. 2 (part a is the micro-structure diagram of PSSA doped polyaniline, and part b is titanium dioxide nanostructure figure).Surface distributed shown in Fig. 2 is very even, and PANI-PSSA particle almost individual layer at silicon plate unfolded surface.Same, we more also can TiO2 nano particle in self assembly in self assembly after the silicon plate of three bilayer (PDDA/PSS) 3 modifieds, because PSS is electronegative, and TiO2 nano particle in acid condition positively charged (pH=1.5).Also to tile the uniform TiO2 nano particle of last layer with the silicon plate surface of TiO2 assembling, particle size is slightly larger than PANI-PSSA, but also very even.Illustrate that PANI-PSSA and TiO2 nano particle is well suited for for layer upon layer electrostatic self assembly.If we assemble the nano particle of polyaniline and these two kinds of oppositely chargeds of titania successively, the nano lamellar compound that just can be replaced layer by layer.
Because the response of thickness to sensor of film has a great impact, we have studied the impact of different film thickness on prepared sensor response characteristic.According to step 1), 2) and 3) alternately assembling 5 layers in the QCM substrate handled well respectively, 10 layers, 20 layers, 30 layers, 40 strata aniline and titanium deoxid films. say that the QCM gas sensor assembled is placed in the gas-sensitive property test macro of laboratory, pass into the NH3 gas of variable concentrations, observe and record the change of QCM gas sensor response frequency.Result is as shown in Fig. 3 (polyaniline of the different number of plies of self assembly and the double-deck impact on qcm sensor response characteristic of titania), and in figure clearly, wherein, the air-sensitive response characteristic of preparation 10 layers of sensitive membrane is best, and it presents good linear characteristic.
5) gas-sensitive property test is carried out to the gas sensing response characteristic of preparation
Choosing the self assembly number of plies is the real-time detection that 10 double-deck QCM gas sensors carry out ammonia, its result as shown in Figure 4, in order to reduce the interference of humidity on sensor performance test, we select nitrogen as carrier gas, at room temperature condition, this sensor all has good response to the ammonia of 10 ppm, the minimum ammonia that can detect 5 ppm.Certainly this sensor can also carry out duplicate detection to the ammonia of high concentration (hundreds of ppm), and sensitive property is not destroyed.This sensor response time and turnaround time are all less than 1 min, and this brings convenience to the practical application of sensor.After repeatedly testing, sensor response change is little, and the baseline of this self assembly organo-mineral complexing thin film sensor is very flat.
We carry out 3 repeated tests to carrying out prepared gas sensor with the ammonia of 50 ppm equally, and as shown in Figure 4, reperformance test shows good recovery characteristic to result, and fundamental sum first time test is consistent.
6) selectivity test is carried out to the gas sensor of preparation
According to embodiment 5) in method, change ethanol respectively, sulfuretted hydrogen, trimethylamine gas as object gas, the sensor prepared by mensuration carry out selective determination.Pass into above three kinds of gases of 100ppm, the linear characteristic of sensor being carried out respectively to the tested gas of variable concentrations measures and repeatability mensuration.Its result as shown in Figure 5.In contrast to the characteristic of the response of ammonia, the QCM gas sensor of preparation is to ethanol, and sulfuretted hydrogen, the response of trimethylamine gas is more weak, and the sensor prepared by explanation has good selectivity to ammonia.
Claims (6)
1. a polyaniline/titanium dioxide film QCM gas sensor, it is characterized in that: take QCM as matrix, evaporation on matrix surface, the symmetrical gold electrode of photoetching, gold electrode is connected with lead-in wire, quartz crystal matrix and gold electrode surfaces are coated with air-sensitive film, and air-sensitive film is the self-assembled nanometer compound of polyaniline/titanium dioxide.
2. gas sensor according to claim 1, is characterized in that: described quartz crystal matrix is AT cut type, and fundamental frequency is 10MHz.
3. gas sensor according to claim 1, is characterized in that: described air-sensitive film is obtained by the polyaniline adulterated with QCM upper substrate layer layer electrostatic self-assembled titanium dioxide nano-particle and the polystyrolsulfon acid of modified.
4. gas sensor according to claim 3, is characterized in that: the method for modifying of described QCM substrate, and step is as follows:
1) QCM substrate Pierre's card agent treated 10 ~ 30 min, makes it bring the negative charge groups such as carboxyl, and substrate deionization drip washing 1 ~ 2 min handled well is dried up with nitrogen;
2) immerse 5 ~ 10 min, taking-up deionization drip washing 1 ~ 2 min in 1 ~ 3%wt PDDA (PDDA) aqueous solution also to dry up with nitrogen;
3) substrate is immersed 5 ~ 10 min in kayexalate (PSS) again, taking-up deionization drip washing 1 ~ 2 min also dries up with nitrogen;
4) step 2 is repeated again successively) and step 3) 2 ~ 3 times, make on-chip gold electrode modify upper 2 ~ 5 double-deck PDDA and PSS, obtain the QCM substrate of modified.
5. gas sensor according to claim 3, is characterized in that: described self assembly step is as follows:
5) the QCM substrate of modified is immersed titanium dioxide nano-particle aqueous solution 5 ~ 10 min of 1 ~ 3 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
6) the QCM substrate of modified is immersed polyaniline aqueous solution 5 ~ 10 min of the polystyrolsulfon acid doping of 1 ~ 3 mg/mL, adulterate by styrene sulfonic acid monomer and aniline monomer mol ratio 1:1, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
7) step 5) and step 6) 10 ~ 40 times is repeated successively again, QCM substrate is made to modify upper 10 ~ 40 double-deck polyanilines and titania, directly dry up without drip washing after the self assembly of last one deck polyaniline, obtained polyaniline/titanium dioxide combination frequency type film gas sensor.
6. a preparation method for the gas sensor according to any one of claim 1-5, is characterized in that: step is as follows:
1) QCM substrate Pierre's card agent treated 10 ~ 30 min, makes it bring the negative charge groups such as carboxyl, and substrate deionization drip washing 1 ~ 2 min handled well is dried up with nitrogen;
2) immerse 5 ~ 10 min, taking-up deionization drip washing 1 ~ 2 min in 1 ~ 3%wt PDDA (PDDA) aqueous solution also to dry up with nitrogen;
3) substrate is immersed 5 ~ 10 min in kayexalate (PSS) again, taking-up deionization drip washing 1 ~ 2 min also dries up with nitrogen;
4) step 2 is repeated again successively) and step 3) 2 ~ 3 times, make on-chip gold electrode modify upper 2 ~ 5 double-deck PDDA and PSS, obtain the QCM substrate of modified;
5) the QCM substrate of modified is immersed titanium dioxide nano-particle aqueous solution 5 ~ 10 min of 1 ~ 3 mg/mL, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
6) the QCM substrate of modified is immersed polyaniline aqueous solution 5 ~ 10 min of the polystyrolsulfon acid doping of 1 ~ 3 mg/mL, adulterate by styrene sulfonic acid monomer and aniline monomer mol ratio 1:1, taking-up pH value is hydrochloric acid drip washing 1 ~ 2 min of 1.5 and dries up with nitrogen;
7) step 5) and step 6) 10 ~ 40 times is repeated successively again, QCM substrate is made to modify upper 10 ~ 40 double-deck polyanilines and titania, directly dry up without drip washing after the self assembly of last one deck polyaniline, obtained polyaniline/titanium dioxide combination frequency type film gas sensor.
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| CN110715957A (en) * | 2019-09-10 | 2020-01-21 | 中国科学院宁波材料技术与工程研究所 | Polystyrene sulfonic acid doped polyaniline composite flexible membrane based high-efficiency ammonia gas sensor and preparation method thereof |
| CN114577864A (en) * | 2022-05-09 | 2022-06-03 | 成都晟铎传感技术有限公司 | MEMS hydrogen sulfide sensor for improving metal salt poisoning effect and preparation method thereof |
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