CN102735753A - Preparation method of multilayer sensitive membrane for surface acoustic wave (SAW) gas sensor - Google Patents
Preparation method of multilayer sensitive membrane for surface acoustic wave (SAW) gas sensor Download PDFInfo
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- CN102735753A CN102735753A CN2012102253208A CN201210225320A CN102735753A CN 102735753 A CN102735753 A CN 102735753A CN 2012102253208 A CN2012102253208 A CN 2012102253208A CN 201210225320 A CN201210225320 A CN 201210225320A CN 102735753 A CN102735753 A CN 102735753A
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Abstract
The invention discloses a preparation method of a multilayer sensitive membrane for a surface acoustic wave (SAW) gas sensor, comprising the following steps of: selecting a piezoelectric substrate, coating a photoresist on the surface of the piezoelectric substrate, photoetching the surface of the piezoelectric substrate, revealing a sensitive membrane area on the surface of the piezoelectric substrate, processing the piezoelectric substrate which is coated with the photoresist and reveals the sensitive membrane area by the use of an MPS solution and a PAH solution, successively immersing the processed piezoelectric substrate into PSS, PPy, PPS and PANI solutions to grow a layer of PPy/PSS/PANI composite sensitive membrane on the piezoelectric substrate, repeating the immersion step and controlling the number of the repetition, so as to obtain the PPy/PSS/PANI composite sensitive membrane of different layers and different thicknesses, removing the photoresist and packaging. According to the invention, detection of NH3 and NO2 gases at room temperature is realized; in addition, the multilayer sensitive membrane has high sensitivity, requires low cost, and is simple and practical.
Description
Technical field
The present invention relates to surface acoustic wave (SAW) gas sensor technical field, particularly a kind ofly be used to detect NH
3And NO
2The preparation method of the SAW gas sensor multi-layer sensitive film of gas.
Background technology
Because NH
3And NO
2The high toxicity of gas, therefore for they in commercial production, environmental monitoring and medical treatment and nursing detection and monitor extremely important.Traditional gas sensor has big, the shortcomings such as portability is poor, sensitivity is low, working temperature height of volume.And hand-held SAW gas sensor volume little, in light weight, be easy to carry and detection sensitivity high, application prospect is very wide.
The SAW gas sensor relies on the adsorption reaction of sensitive membrane and gas; Reach the effect of detected gas and concentration thereof through the difference on the frequency that detects the absorption front and back; It is the core link of sensor; Therefore the choosing and make for the SAW transducer sensitivity and with selecting performance conclusive effect is arranged of sensitive membrane is so suitable sensitive membrane and preparation method thereof is the core work of SAW gas sensor.
Be used to detect NH at present
3And NO
2The membrane material of gas mainly is ZnO, SnO
2, TiO
2Deng conductor oxidate, though they are to NH
3And NO
2Gas has suction-operated, but its desorption process need could realize under higher temperature that be unfavorable for their application, therefore searching and making are applicable to that normal temperature detects NH
3And NO
2The sensitive membrane of gas is very important and urgent task.
Polypyrrole (PPy) and Polyaniline (PANI) are conducting polymers; Structure with conjugacy; Usually generate through chemistry or electrochemical polymerization; Their air stabilities are good, be easy to through mixing and control its electrology characteristics of condition control such as pH value, temperature, concentration of its polymeric solution, and they at normal temperatures just can be to NH
3And NO
2Gas produces response, so PPy and PANI relatively are fit to do the sensitive membrane of SAW gas sensor.
Summary of the invention
The technical matters that (one) will solve
In view of this, fundamental purpose of the present invention provides a kind of preparation method of sonic surface wave gas sensors multi-layer sensitive film, to realize at room temperature to NH
3And NO
2The detection of gas.
(2) technical scheme
For achieving the above object, the invention provides a kind of preparation method of sonic surface wave gas sensors multi-layer sensitive film, be used to detect NH
3And NO
2Gas comprises:
Select a piezoelectric substrate,, photoetching is carried out on this piezoelectric substrate surface, expose the sensitive membrane zone on this piezoelectric substrate surface at this piezoelectric substrate surface applied photoresist;
Adopt MPS solution and PAH solution to being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle;
This piezoelectric substrate after handling is immersed in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate; Repeat this immersion step and control multiplicity, on this piezoelectric substrate, obtain the PPy/PSS/PANI composite sensitive film of different number of plies different-thickness; And
Remove the PPy/PSS/PANI composite sensitive film of growing on surperficial photoresist of this piezoelectric substrate and the photoresist, and encapsulation.
In the such scheme, said piezoelectric substrate is selected quartz substrate for use, utilizes the piezoelectric effect of this substrate to make it under the interpolation transducer excitation, excite surface acoustic wave.
In the such scheme; Said employing MPS solution and PAH solution are to being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle; Comprise: this piezoelectric substrate was immersed in 3-Mercapto-1-propanesulfonic acid sodium salt (MPS) solution of 2mg/ml 2 hours; After drying up, washed with de-ionized water again this piezoelectric substrate was immersed in poly allylamine hydrochloride (PAH) solution that pH is 4 10mg/ml 10 minutes, and with washed with de-ionized water and dry up.
In the such scheme; This piezoelectric substrate after said will the processing immerses in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate; Specifically comprise: this piezoelectric substrate after will handling immerses the polyanion of 10mg/ml, and (poly styrene sulfonic acid sodium salt PSS) made its surface adsorption one deck PSS in 10 minutes in the solution, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate is immersed the FeCl of 0.006M
3, 0.026M p-toluene sulfonic acid (p-TSA) and 0.02M pyrrole stirring reaction 15 minutes and filter 10 minutes self assembly one deck Polypyrrole (PPy) on PSS in the good solution, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate was immersed in the PSS solution 10 minutes once more; Then this piezoelectric substrate was immersed in dimethyl acetamide (DMAc) solution of Polyaniline (PANI) of emeraldine base that pH is 2.8 20mg/ml 10 minutes one deck PPy/PSS/PANI composite sensitive film of then on this piezoelectric substrate, having grown after using deionization to clean to dry up.
In the such scheme, saidly rinse out the poor group of adhesiveness and dry up, be used to improve the homogeneity and the adhesiveness of film with deionized water.
(3) beneficial effect
Characteristics of the present invention are to utilize the electrostatic forcing of polyanion electrolyte and polycation electrolyte, through the composite sensitive film of the different numbers of plies of on piezoelectric substrate, growing in the mode of alternately dip-coating.The invention provides a kind of preparation method of sonic surface wave gas sensors multi-layer sensitive film, can access the stable multi-layer sensitive film that can be applicable to the SAW gas sensor of controllable thickness, realized at room temperature to NH
3And NO
2The detection of gas, and highly sensitive, cost is low, and is simple and practical.
Description of drawings
Fig. 1 is preparation method's process flow diagram of sonic surface wave gas sensors multi-layer sensitive film provided by the invention.
Fig. 2-1 accordings to the process chart of the preparation sonic surface wave gas sensors multi-layer sensitive film of the embodiment of the invention to Fig. 2-the 9th.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
The preparation method of sonic surface wave gas sensors multi-layer sensitive film provided by the invention at first selects substrate, and this substrate is quartz substrate or other piezoelectric substrate, its objective is that the piezoelectric effect of utilizing substrate makes it under the interpolation transducer excitation, excite surface acoustic wave; Then through photoetching on-chip sensitive membrane graph area is exposed, other places of substrate then cover photoresist and are used to protect interdigital transducer; The substrate that will be coated with photoresist then immersed in the MPS solution 2 hours, then substrate was immersed among the PAH 10 minutes, substrate is dried up the back immerse PSS and the FeCl that contains quantitative mol ratio
3, p-TSA and pyrrole reaction 15 minutes and filtered in the good solution deposit PPy each 10 minutes; Each take out the back with deionization clean up dry up after, substrate is immersed respectively just can obtain one deck PPy/PSS/PANI composite sensitive film in PSS and the PANI solution in 10 minutes then; Through repeating above step and controlling the number of times of dip-coating, just can obtain the PPy/PSS/PANI composite sensitive film of different number of plies different-thickness; Remove photoresist at last, and encapsulation.
As shown in Figure 1, Fig. 1 is preparation method's process flow diagram of sonic surface wave gas sensors multi-layer sensitive film provided by the invention, and this method may further comprise the steps:
Step 1: select a piezoelectric substrate,, photoetching is carried out on this piezoelectric substrate surface, expose the sensitive membrane zone on this piezoelectric substrate surface at this piezoelectric substrate surface applied photoresist;
Step 2: adopt MPS solution and PAH solution to being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle;
Step 3: this piezoelectric substrate after will handling immerses in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate; Repeat this immersion step and control multiplicity, on this piezoelectric substrate, obtain the PPy/PSS/PANI composite sensitive film of different number of plies different-thickness; And
Step 4: remove the PPy/PSS/PANI composite sensitive film of growing on surperficial photoresist of this piezoelectric substrate and the photoresist, and encapsulation.
Wherein, Adopt MPS solution and PAH solution to being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle described in the step 2; Comprise: this piezoelectric substrate was immersed in 3-Mercapto-1-propanesulfonic acid sodium salt (MPS) solution of 2mg/ml 2 hours; After drying up, washed with de-ionized water again this piezoelectric substrate was immersed in poly allylamine hydrochloride (PAH) solution that pH is 4 10mg/ml 10 minutes, and with washed with de-ionized water and dry up.
This piezoelectric substrate after will handling described in the step 3 immerses in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate; Specifically comprise: this piezoelectric substrate after will handling immerses polyanion (the poly styrene sulfonic acid sodium salt of 10mg/ml; PSS) made its surface adsorption one deck PSS in the solution in 10 minutes, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate is immersed the FeCl of 0.006M
3, 0.026M p-toluene sulfonic acid (p-TSA) and 0.02M pyrrole stirring reaction 15 minutes and filter 10 minutes self assembly one deck Polypyrrole (PPy) on PSS in the good solution, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate was immersed in the PSS solution 10 minutes once more; Then this piezoelectric substrate was immersed in dimethyl acetamide (DMAc) solution of Polyaniline (PANI) of emeraldine base that pH is 2.8 20mg/ml 10 minutes one deck PPy/PSS/PANI composite sensitive film of then on this piezoelectric substrate, having grown after using deionization to clean to dry up.Saidly rinse out the poor group of adhesiveness and dry up, be used to improve the homogeneity and the adhesiveness of film with deionized water.
Fig. 2-1 shows the process chart according to the preparation sonic surface wave gas sensors multi-layer sensitive film of the embodiment of the invention to Fig. 2-9.
Shown in Fig. 2-1, Fig. 2-the 1st, the synoptic diagram of piezoelectric substrate.This piezoelectric substrate is quartz substrate or other piezoelectric substrate, its objective is that the piezoelectric effect of utilizing substrate makes it under the interpolation transducer excitation, excite surface acoustic wave.
Shown in Fig. 2-2, Fig. 2-the 2nd, the synoptic diagram after applying photoetching on the piezoelectric substrate and carrying out photoetching.At this piezoelectric substrate surface applied photoresist, and the photoresist on this piezoelectric substrate surface carried out photoetching, expose the sensitive membrane zone on this piezoelectric substrate surface.
Shown in Fig. 2-3, the synoptic diagram after Fig. 2-the 3rd, piezoelectric substrate handle through MPS.This piezoelectric substrate was immersed in 3-Mercapto-1-propanesulfonic acid sodium salt (MPS) solution of 2mg/ml 2 hours, at piezoelectric substrate surface adsorption one deck MPS, after drying up with washed with de-ionized water then.
Shown in Fig. 2-4, Fig. 2-the 4th, the synoptic diagram on the piezoelectric substrate behind absorption one deck PAH.This piezoelectric substrate was immersed in poly allylamine hydrochloride (PAH) solution that pH is 4 10mg/ml 10 minutes, absorption one deck PAH on this MPS surface, and with washed with de-ionized water and dry up.
Shown in Fig. 2-5, Fig. 2-the 5th, the synoptic diagram on the piezoelectric substrate behind the absorption PSS.This piezoelectric substrate after handling is immersed polyanion (the poly styrene sulfonic acid sodium salt of 10mg/ml; PSS) made PAH surface adsorption one deck PSS in the solution in 10 minutes, rinse out the poor group of adhesiveness and dry up with deionized water.
Shown in Fig. 2-6, Fig. 2-the 6th, the synoptic diagram on the piezoelectric substrate behind deposition one deck PPy.This piezoelectric substrate is immersed the FeCl of 0.006M
3, 0.026M p-toluene sulfonic acid (p-TSA) and 0.02M pyrrole stirring reaction 15 minutes and filter 10 minutes self assembly one deck Polypyrrole (PPy) on PSS in the good solution, rinse out the poor group of adhesiveness and dry up with deionized water.
Shown in Fig. 2-7, Fig. 2-the 7th, the synoptic diagram on the piezoelectric substrate behind deposition one deck PANI.This piezoelectric substrate was immersed in the PSS solution 10 minutes once more; This PPy surface deposition one deck PSS; Then this piezoelectric substrate was immersed in dimethyl acetamide (DMAc) solution of Polyaniline (PANI) of emeraldine base that pH is 2.8 20mg/ml 10 minutes after using deionization to clean then to dry up, at this PSS surface deposition one deck PANI.
Shown in Fig. 2-8, Fig. 2-the 8th, the synoptic diagram on the piezoelectric substrate behind the deposit multilayer PPy/PSS/PANI.
Shown in Fig. 2-9, Fig. 2-the 9th, the synoptic diagram of the multilayer PPy/PSS/PANI after removing photoresist.Remove the PPy/PSS/PANI composite sensitive film of growing on surperficial photoresist of this piezoelectric substrate and the photoresist, obtain multilayer PPy/PSS/PANI composite sensitive film.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the preparation method of a sonic surface wave gas sensors multi-layer sensitive film is used to detect NH
3And NO
2Gas is characterized in that, comprising:
Select a piezoelectric substrate,, photoetching is carried out on this piezoelectric substrate surface, expose the sensitive membrane zone on this piezoelectric substrate surface at this piezoelectric substrate surface applied photoresist;
Adopt MPS solution and PAH solution to being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle;
This piezoelectric substrate after handling is immersed in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate; Repeat this immersion step and control multiplicity, on this piezoelectric substrate, obtain the PPy/PSS/PANI composite sensitive film of different number of plies different-thickness; And
Remove the PPy/PSS/PANI composite sensitive film of growing on surperficial photoresist of this piezoelectric substrate and the photoresist, and encapsulation.
2. the preparation method of sonic surface wave gas sensors multi-layer sensitive film according to claim 1 is characterized in that, said piezoelectric substrate is selected quartz substrate for use, utilizes the piezoelectric effect of this substrate to make it under the interpolation transducer excitation, excite surface acoustic wave.
3. the preparation method of sonic surface wave gas sensors multi-layer sensitive film according to claim 1 is characterized in that, said employing MPS solution and PAH solution comprise being coated with photoresist and exposing this regional piezoelectric substrate of sensitive membrane and handle:
This piezoelectric substrate was immersed in 3-Mercapto-1-propanesulfonic acid sodium salt (MPS) solution of 2mg/ml 2 hours; After drying up, washed with de-ionized water again this piezoelectric substrate was immersed in poly allylamine hydrochloride (PAH) solution that pH is 4 10mg/ml 10 minutes, and with washed with de-ionized water and dry up.
4. the preparation method of sonic surface wave gas sensors multi-layer sensitive film according to claim 1; It is characterized in that; This piezoelectric substrate after said will the processing immerses in PSS, PPy, PSS and the PANI solution successively; Growth one deck PPy/PSS/PANI composite sensitive film on this piezoelectric substrate specifically comprises:
This piezoelectric substrate after handling is immersed the polyanion of 10mg/ml, and (poly styrene sulfonic acid sodium salt PSS) made its surface adsorption one deck PSS in 10 minutes in the solution, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate is immersed the FeCl of 0.006M
3, 0.026M p-toluene sulfonic acid (p-TSA) and 0.02M pyrrole stirring reaction 15 minutes and filter 10 minutes self assembly one deck Polypyrrole (PPy) on PSS in the good solution, rinse out the poor group of adhesiveness and dry up with deionized water; Then this piezoelectric substrate was immersed in the PSS solution 10 minutes once more; Then this piezoelectric substrate was immersed in dimethyl acetamide (DMAc) solution of Polyaniline (PANI) of emeraldine base that pH is 2.8 20mg/ml 10 minutes one deck PPy/PSS/PANI composite sensitive film of then on this piezoelectric substrate, having grown after using deionization to clean to dry up.
5. the preparation method of sonic surface wave gas sensors multi-layer sensitive film according to claim 4 is characterized in that, saidly rinses out the poor group of adhesiveness and dries up with deionized water, is used to improve the homogeneity and the adhesiveness of film.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006043299A1 (en) * | 2004-10-22 | 2006-04-27 | Saes Getters S.P.A. | Surface acoustic wave gas sensor with sensitive getter layer and process for its manufacture |
| CN101354367A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Polypyrrole gas sensor and manufacturing method thereof |
| CN101776632A (en) * | 2010-03-09 | 2010-07-14 | 浙江大学 | Water dispersible polyaniline nano-particle gas-sensitive element and method for preparing same |
-
2012
- 2012-06-29 CN CN2012102253208A patent/CN102735753A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006043299A1 (en) * | 2004-10-22 | 2006-04-27 | Saes Getters S.P.A. | Surface acoustic wave gas sensor with sensitive getter layer and process for its manufacture |
| CN101354367A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Polypyrrole gas sensor and manufacturing method thereof |
| CN101776632A (en) * | 2010-03-09 | 2010-07-14 | 浙江大学 | Water dispersible polyaniline nano-particle gas-sensitive element and method for preparing same |
Non-Patent Citations (5)
| Title |
|---|
| 《传感器与微系统》 20110930 周文等 聚苯胺-多壁碳纳米管薄膜SAW NO2传感器 85-87 1-5 第30卷, 第9期 * |
| CHIA-YU LIN等: "Using a PEDOT:PSS modified electrode for detecting nitric oxide gas", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| X.F.YAN等: "Comparison of response towards NO2 and H2S of PPy and PPy/TiO2 as SAW sensitive films", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| 周文等: "聚苯胺—多壁碳纳米管薄膜SAW NO2传感器", 《传感器与微系统》 * |
| 翁宇峰等: "共轭聚合物在传感器上的应用", 《感光科学与光化学》 * |
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Application publication date: 20121017 |