CN101354367A - Polypyrrole gas sensor and manufacturing method thereof - Google Patents
Polypyrrole gas sensor and manufacturing method thereof Download PDFInfo
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- CN101354367A CN101354367A CNA2008101205516A CN200810120551A CN101354367A CN 101354367 A CN101354367 A CN 101354367A CN A2008101205516 A CNA2008101205516 A CN A2008101205516A CN 200810120551 A CN200810120551 A CN 200810120551A CN 101354367 A CN101354367 A CN 101354367A
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Abstract
The invention discloses a polypyrrole gas sensor and a manufacturing method thereof. The manufacturing method of the polypyrrole gas sensor uses a ceramic glass as a substrate, multiple pairs of interdigital gold electrodes are arranged on the substrate, modified films of diallyl dimethyl ammonium chloride and poly sodium styrenesulfonate are orderly deposited on the surfaces of the ceramic substrate and the interdigital gold electrodes, and a polypyrrole gas sensing film is deposited on the modified films which are used for leading the polypyrrole and the surfaces of the substrate and the electrodes to be well contacted. The manufacturing method of the polypyrrole gas sensor has simple preparation technique and low cost, and is especially applicable to batch production. The prepared gas sensor can be used for measuring ammonia concentration at room temperature, is characterized by high sensitivity, good recoverability and quick response in responding to ammonia gas, and can be used for the ammonia detection in industrial and agricultural production as well as environment monitoring.
Description
Technical field
The present invention relates to a kind of polypyrrole gas sensor and preparation method thereof.
Background technology
Ammonia is a kind of colourless toxic gas, and excessive concentrations may be brought out human body diseases or death, and it detects environmental quality monitoring, industry, agricultural and pharmaceutical industry etc. all significant.This has proposed higher requirement for the ammonia gas sensor, also provides wide prospect for its development simultaneously.Gas sensor commonly used at present mainly contains inorganic semiconductor gas sensor and organic polymer gas sensor two big classes.Than the inorganic ceramic material gas sensor that the needs heating at high temperature detects, the macromolecule gas sensor can at room temperature be realized the detection for gas concentration, has energy-efficient characteristics, and the response favorable reproducibility.In addition, the macromolecule gas sensor has also that volume is little, sensitivity, high conformity, advantage such as cheap, therefore is expected to become a kind of gas sensor of novel high-performance based on the ammonia gas sensor of macromolecular material, and its research also just receives publicity.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can at room temperature detect ammonia in the broad concentration range, and have the response good reversibility, highly sensitive, respond polypyrrole gas sensor and preparation method thereof faster.
Polypyrrole gas sensor of the present invention has ceramic substrate, have many at ceramic substrate photomask surface and evaporation to interdigital gold electrode, on interdigital gold electrode, be connected with lead-in wire, be coated with PDDA modified membrane and kayexalate modified membrane successively at ceramic substrate and interdigital gold electrode surfaces, the polypyrrol gas sensitive film arranged in kayexalate modified membrane surface-coated.
The method for making of polypyrrole gas sensor may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) preparing concentration expressed in percentage by weight respectively is 1～5% the PDDA aqueous solution and the kayexalate aqueous solution of concentration expressed in percentage by weight 1～5%;
3) add pyrrole monomer solution and stir 2～30min in the aqueous solution that contains ferric trichloride and p-toluenesulfonic acid, filter paper filtering obtains precursor solution, wherein in concentration expressed in percentage by weight, ferric trichloride is 0.02～0.2%, and p-toluenesulfonic acid is 0.4～2%, and the pyrroles is 0.1～0.3%;
4) the interdigital gold electrode of the ceramic substrate of step 1) be impregnated in successively each 10～30min in PDDA aqueous solution and the kayexalate aqueous solution, after finishing, each dipping, dries up with nitrogen stream with the interdigital gold electrode of ceramic substrate rinsed with deionized water 10～40s; Subsequently the interdigital gold electrode of ceramic substrate be impregnated in 15～120min in the precursor solution of step 3) preparation, take out and use rinsed with deionized water, through the nitrogen fluidized drying, obtain polypyrrole gas sensor again.
The interdigital gold electrode on ceramic substrate of the present invention surface has 8～16 pairs, and the interdigital width of interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
Advantage of the present invention is:
1) prepared polypyrrole gas sensor is the method by the solution growth in situ, obtain at the ceramic substrate that is coated with the polyelectrolyte modified membrane and interdigital gold electrode surfaces deposition polypyrrol gas sensitive film, solve polypyrrole thus and be difficult to process the difficult problem of film forming, and be not subjected to the restriction of substrate size and shape; Not only film forming is even for the film of poly pyrrole that method by solution growth makes, and can be attached to ceramic substrate and interdigital gold electrode surfaces well, and film thickness also is easy to control;
2) prepared polypyrrole gas sensor, be coated with poly-PDDA and kayexalate modified membrane successively at ceramic substrate and interdigital gold electrode surfaces, the introducing of modified membrane oxygenant, the adulterant on the one hand can adsorbent solution, induce polymerization at modified membrane surface pyrrole monomer, form uniform polypyrrol gas sensitive film, also help contacting between polypyrrol gas sensitive film and electrode and the substrate on the other hand, reduce contact resistance, improve the stability of gas sensor;
When 3) adopting solution growth to prepare film of poly pyrrole, the employing p-toluenesulfonic acid is an adulterant, and its introducing has improved the stability of polypyrrol gas sensitive film;
4) adopt solution polymerization process to prepare polypyrrole, can pass through to change the regulation and control of solution polymerization conditions such as the composition realization of polymerization time, precursor solution easily for the gas sensor response characteristic;
5) polypyrrole gas sensor that makes at room temperature has higher response sensitivity to ammonia;
6) much smaller than the ammonia with concentration, its response to ammonia has certain selectivity to prepared polypyrrole gas sensor to the response of various organic steams;
7) adopt the method for solution growth in situ to prepare gas sensor, simple and easy to do, the yield rate height, high conformity is suitable for producing in batches;
8) to have a volume little for gas sensor of the present invention, and advantage such as cost is low, and is easy to use can be widely used in commercial production, the environmental monitoring of measurement and control to(for) ammonia.
Description of drawings
Fig. 1 is the structural representation of gas sensor of the present invention;
Fig. 2 is the stereoscan photograph of the polypyrrole sensitive membrane of gas sensor of the present invention;
Fig. 3 is the response return curve of gas sensor of the present invention to the variable concentrations ammonia;
Fig. 4 is the response sensitivity curve of gas sensor of the present invention to ammonia;
Fig. 5 is the round robin curve of gas sensor of the present invention to ammonia.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, polypyrrole gas sensor of the present invention has ceramic substrate 1, have many at ceramic substrate photomask surface and evaporation to interdigital gold electrode 2, on interdigital gold electrode, be connected with lead-in wire 3, be coated with PDDA modified membrane 4 and kayexalate modified membrane 5 successively at ceramic substrate and interdigital gold electrode surfaces, polypyrrol gas sensitive film 6 arranged in kayexalate modified membrane surface-coated.
The interdigital gold electrode on said ceramic substrate surface has 8～16 pairs, and the width of interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
Embodiment 1:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) preparing concentration expressed in percentage by weight respectively is 1% the PDDA aqueous solution and the kayexalate aqueous solution of concentration expressed in percentage by weight 5%;
3) add pyrrole monomer solution and stir 2min in the aqueous solution that contains ferric trichloride and p-toluenesulfonic acid, filter paper filtering obtains precursor solution, and wherein in concentration expressed in percentage by weight, ferric trichloride is 0.02%, and p-toluenesulfonic acid is 0.4%, and the pyrroles is 0.1%;
4) adopt dip coater that the interdigital gold electrode of the ceramic substrate of step 1) be impregnated in each 10min in PDDA aqueous solution and the kayexalate aqueous solution successively, after finishing, each dipping, dries up with nitrogen stream with the interdigital gold electrode of ceramic substrate rinsed with deionized water 10s; Subsequently the interdigital gold electrode of ceramic substrate be impregnated in 15min in the precursor solution of step 3) preparation, take out and use rinsed with deionized water, promptly obtain polypyrrole gas sensor through the nitrogen fluidized drying again.
Embodiment 2:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) preparing concentration expressed in percentage by weight respectively is 5% the PDDA aqueous solution and the kayexalate aqueous solution of concentration expressed in percentage by weight 1%;
3) add pyrrole monomer solution and stir 20min in the aqueous solution that contains ferric trichloride and p-toluenesulfonic acid, filter paper filtering obtains precursor solution, and wherein in concentration expressed in percentage by weight, ferric trichloride is 0.2%, and p-toluenesulfonic acid is 2%, and the pyrroles is 0.3%;
4) adopt dip coater that the interdigital gold electrode of the ceramic substrate of step 1) be impregnated in each 20min in PDDA aqueous solution and the kayexalate aqueous solution successively, after finishing, each dipping, dries up with nitrogen stream with the interdigital gold electrode of ceramic substrate rinsed with deionized water 40s; Subsequently the interdigital gold electrode of ceramic substrate be impregnated in 60min in the precursor solution of step 3) preparation, take out and use rinsed with deionized water, promptly obtain polypyrrole gas sensor through the nitrogen fluidized drying again.
Embodiment 3:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) preparing concentration expressed in percentage by weight respectively is 2% the PDDA aqueous solution and the kayexalate aqueous solution of concentration expressed in percentage by weight 2%;
3) add pyrrole monomer solution and stir 15min in the aqueous solution that contains ferric trichloride and p-toluenesulfonic acid, filter paper filtering obtains precursor solution, wherein in concentration expressed in percentage by weight, ferric trichloride is 0.05%, and p-toluenesulfonic acid is 0.5%, and the pyrroles is 0.15%;
4) adopt dip coater that the interdigital gold electrode of the ceramic substrate of step 1) be impregnated in each 20min in PDDA aqueous solution and the kayexalate aqueous solution successively, after finishing, each dipping, dries up with nitrogen stream with the interdigital gold electrode of ceramic substrate rinsed with deionized water 20s; Subsequently the interdigital gold electrode of ceramic substrate be impregnated in 30min in the precursor solution of step 3) preparation, take out and use rinsed with deionized water, promptly obtain polypyrrole gas sensor through the nitrogen fluidized drying again.
The stereoscan photograph of the polypyrrole sensitive membrane of gas sensor, as shown in Figure 2.
Figure 3 shows that the polypyrrole gas sensor that makes response return curve to the variable concentrations ammonia; As seen from the figure, gas sensor has very high response sensitivity to ammonia, and response is replied better.
Figure 4 shows that the polypyrrole gas sensor that the makes response sensitivity curve to ammonia, as seen from the figure, polypyrrole gas sensor shows higher response sensitivity in whole measurement concentration range for ammonia.
Figure 5 shows that the polypyrrole gas sensor that the makes round robin curve to low concentration ammonia, as seen from the figure, polypyrrole gas sensor to the response reversibility of ammonia and repeatability better.
Claims (4)
1. polypyrrole gas sensor, it is characterized in that it has ceramic substrate (1), have many at ceramic substrate photomask surface and evaporation to interdigital gold electrode (2), on interdigital gold electrode, be connected with lead-in wire (3), be coated with PDDA modified membrane (4) and kayexalate modified membrane (5) successively at ceramic substrate and interdigital gold electrode surfaces, polypyrrol gas sensitive film (6) arranged in kayexalate modified membrane surface-coated.
2. polypyrrole gas sensor according to claim 1 is characterized in that the interdigital gold electrode on ceramic substrate surface has 8～16 pairs, and the interdigital width of interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
3. the method for making of polypyrrole gas sensor according to claim 1 is characterized in that step is as follows:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) preparing concentration expressed in percentage by weight respectively is 1～5% the PDDA aqueous solution and the kayexalate aqueous solution of concentration expressed in percentage by weight 1～5%;
3) add pyrrole monomer solution and stir 2～30min in the aqueous solution that contains ferric trichloride and p-toluenesulfonic acid, filter paper filtering obtains precursor solution, wherein in concentration expressed in percentage by weight, ferric trichloride is 0.02～0.2%, and p-toluenesulfonic acid is 0.4～2%, and the pyrroles is 0.1～0.3%;
4) the interdigital gold electrode of the ceramic substrate of step 1) be impregnated in successively each 10～30min in PDDA aqueous solution and the kayexalate aqueous solution, after finishing, each dipping, dries up with nitrogen stream with the interdigital gold electrode of ceramic substrate rinsed with deionized water 10～40s; Subsequently the interdigital gold electrode of ceramic substrate be impregnated in 15～120min in the precursor solution of step 3) preparation, take out and use rinsed with deionized water, through the nitrogen fluidized drying, obtain polypyrrole gas sensor again.
4. according to the method for making of the described polypyrrole gas sensor of claim 3, the interdigital width that it is characterized in that said interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907593A (en) * | 2010-07-20 | 2010-12-08 | 浙江大学 | Polypyrrole/polyvinylidene fluoride nano fiber composite resistance type film gas-sensitive element and manufacturing method thereof |
| CN102375028A (en) * | 2010-08-06 | 2012-03-14 | 中国科学院微电子研究所 | Method for manufacturing high-selectivity semiconductor film |
| CN102735753A (en) * | 2012-06-29 | 2012-10-17 | 中国科学院微电子研究所 | Preparation method of multilayer sensitive membrane for surface acoustic wave (SAW) gas sensor |
| CN103033538A (en) * | 2012-12-20 | 2013-04-10 | 中国科学院微电子研究所 | Preparation method for flexible substrate-based sensitive film for detecting gas at normal temperature |
| CN103713019A (en) * | 2013-12-23 | 2014-04-09 | 浙江大学 | Zinc oxide/polypyrrole nano composite resistance-type film gas sensor and production method thereof |
| CN104034432A (en) * | 2014-06-18 | 2014-09-10 | 中国人民大学 | Near-infrared sensing chip, preparation method and application thereof |
| CN104833701A (en) * | 2015-05-06 | 2015-08-12 | 江苏大学 | Preparation method of nano film ammonia gas sensor |
| CN106855526A (en) * | 2017-03-20 | 2017-06-16 | 长春工业大学 | A kind of gas sensor for loading polypyrrole and preparation method thereof |
| CN107865654A (en) * | 2017-12-19 | 2018-04-03 | 南京工业大学 | A kind of method that the dry electrode of cardioelectric monitor is prepared based on leather |
| CN108303449A (en) * | 2017-01-11 | 2018-07-20 | 天津大学 | The quick element of room temperature high sensitivity ammonia based on tungsten oxide-polypyrrole core sheath nano wire |
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2008
- 2008-08-19 CN CNA2008101205516A patent/CN101354367A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907593A (en) * | 2010-07-20 | 2010-12-08 | 浙江大学 | Polypyrrole/polyvinylidene fluoride nano fiber composite resistance type film gas-sensitive element and manufacturing method thereof |
| CN102375028A (en) * | 2010-08-06 | 2012-03-14 | 中国科学院微电子研究所 | Method for manufacturing high-selectivity semiconductor film |
| CN102735753A (en) * | 2012-06-29 | 2012-10-17 | 中国科学院微电子研究所 | Preparation method of multilayer sensitive membrane for surface acoustic wave (SAW) gas sensor |
| CN103033538B (en) * | 2012-12-20 | 2015-01-21 | 中国科学院微电子研究所 | Preparation method for flexible substrate-based sensitive film for detecting gas at normal temperature |
| CN103033538A (en) * | 2012-12-20 | 2013-04-10 | 中国科学院微电子研究所 | Preparation method for flexible substrate-based sensitive film for detecting gas at normal temperature |
| CN103713019A (en) * | 2013-12-23 | 2014-04-09 | 浙江大学 | Zinc oxide/polypyrrole nano composite resistance-type film gas sensor and production method thereof |
| CN103713019B (en) * | 2013-12-23 | 2015-09-16 | 浙江大学 | Nano combined resistance type thin film gas sensor of zinc paste/polypyrrole and preparation method thereof |
| CN104034432A (en) * | 2014-06-18 | 2014-09-10 | 中国人民大学 | Near-infrared sensing chip, preparation method and application thereof |
| CN104034432B (en) * | 2014-06-18 | 2017-02-15 | 中国人民大学 | Near-infrared sensing chip, preparation method and application thereof |
| CN104833701A (en) * | 2015-05-06 | 2015-08-12 | 江苏大学 | Preparation method of nano film ammonia gas sensor |
| CN104833701B (en) * | 2015-05-06 | 2018-08-28 | 江苏大学 | A kind of preparation method of nano thin-film ammonia gas sensor |
| CN108303449A (en) * | 2017-01-11 | 2018-07-20 | 天津大学 | The quick element of room temperature high sensitivity ammonia based on tungsten oxide-polypyrrole core sheath nano wire |
| CN106855526A (en) * | 2017-03-20 | 2017-06-16 | 长春工业大学 | A kind of gas sensor for loading polypyrrole and preparation method thereof |
| CN107865654A (en) * | 2017-12-19 | 2018-04-03 | 南京工业大学 | A kind of method that the dry electrode of cardioelectric monitor is prepared based on leather |
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Open date: 20090128 |