CN100523799C - Polyelectrolyte / intrinsic conducting polymer composite humidity sensor and its production method - Google Patents
Polyelectrolyte / intrinsic conducting polymer composite humidity sensor and its production method Download PDFInfo
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- CN100523799C CN100523799C CNB200710069735XA CN200710069735A CN100523799C CN 100523799 C CN100523799 C CN 100523799C CN B200710069735X A CNB200710069735X A CN B200710069735XA CN 200710069735 A CN200710069735 A CN 200710069735A CN 100523799 C CN100523799 C CN 100523799C
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Abstract
The invention discloses a humidity sensor of combination of polyelectrolyte and intrinsic conducting polymer and the fabricating method. It adopts glass ceramic as substrate and multiple pairs of interdigital golden electrodes are set on it. Humidity film of combination of poly 4-vinypyridine with cross-linking quaternary amination and polypyrole is coated on surface of glass ceramic and interdigital golden electrode. The invention is provided with simple preparing process and low cost. It is suitable for mass production especially. Prepared humidity sensors are all provided with moderate resistance, high sensitivity, good linearity, quick response, good recurrence, strong stability and measuring in room temperature so on in wide humidity range, especially in circumstance with middle-low humidity (0-60%). It can be applied in production process of industry and agriculture, storage and accurate measurement and control for circumstance humidity when air circumstance is monitored.
Description
Technical field
The present invention relates to a kind of polyelectrolyte/intrinsic conducting polymer composite humidity sensor and preparation method thereof.
Background technology
Accurately measure humidity and have vital role in industrial and agricultural production and environmental monitoring, this development for humidity sensor provides wide space.Macromolecular material humidity sensor development in recent years is very rapid, compares traditional stupalith humidity sensor, and it is good that it has response characteristic, and measurement range is wide, good stability, but room temperature detect, be easy to integratedly, miniaturization is produced in batches, lower-price characteristic.Macromolecule resistance type humidity sensor wherein, it can be fine compatible with present integrated circuit technique, is easy to realize moisture measurement and control in the integrated system, become one of important directions of humidity sensor development now.Yet the macromolecule resistance type humidity sensor of traditional polymer humidity-sensitive material preparation relies on pure ionic conduction, and ion mobility is low during low humidity, and resistance value is excessive and be difficult to measure, and has seriously hindered its development.
Summary of the invention
The purpose of this invention is to provide that a kind of (it is moderate, highly sensitive to have resistance value under 0～60%RH) environment, and the linearity is good at middle low humidity, response is fast, recovery is good, and stability is strong, but polyelectrolyte/intrinsic conducting polymer composite humidity sensor that room temperature detects and preparation method thereof.
Polyelectrolyte/intrinsic conducting polymer composite humidity sensor of the present invention has the devitrified glass matrix, have many in photoetching of devitrified glass matrix surface and evaporation to interdigital gold electrode, on interdigital gold electrode, be connected with lead-in wire, be coated with humidity sensitive thin film at devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity sensitive thin film is crosslinked quaternary ammoniated poly 4 vinyl pyridine and composite polypyrrole film.
The method for making of polyelectrolyte/intrinsic conducting polymer composite humidity sensor may further comprise the steps:
1) clean surface photoetching and evaporation have the glass-ceramic substrate of interdigital gold electrode, dry for standby;
2) will gather 4-vinylpyridine and 1,4-dibromobutane is dissolved in N, in N-dimethyl formamide, 4-vinylpyridine unit and 1 in the polymkeric substance, the mol ratio of 4-dibromobutane is 1: 0.5～2, be mixed with the solution that polymer concentration is 10～30 mg/ml, place 4～12h, obtain precursor solution at 30 ℃;
3) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 0.5～2 minute, lift taking-up after, crosslinked quaternary ammoniated 2～12h under 80～140 ℃ of temperature forms the polyelectrolyte basilar memebrane in the interdigital gold electrode surfaces of devitrified glass;
4) ammonium persulfate and 4-toluene sulfonic acide are dissolved in the deionized water simultaneously, the mass ratio of ammonium persulfate and 4-toluene sulfonic acide is 1:0.2～3, and ammonium persulfate concentration is 0.2～4 mg/ml, obtains solution A;
5) adopt dip coater will impregnated in the solution A 1～6 minute through the interdigital gold electrode of devitrified glass of step 3) processing, after drying, vapour phase polymerization 1～12h in saturated pyrroles's steam of 0～50 ℃, through absolute ethanol washing, 50～80 ℃ of oven dry obtain polyelectrolyte/intrinsic conducting polymer composite humidity sensor.
The interdigital gold electrode of above-mentioned microcrystalline glass matrix 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 polyelectrolyte/intrinsic conducting polymer composite humidity sensor is the advantages with polyelectrolyte humidity-sensitive material and intrinsic conducting polymer, utilize the good electric conductivity of intrinsic conducting polymer, especially in the electric conductivity of hanging down under the wet environment, with of the high sensitivity response of polyelectrolyte humidity-sensitive material to humidity, by regulating both ratio of componentss, make compound humidity sensing film in wide humidity range, particularly middle low humidity (also has suitable resistance, has good wet quick response characteristics such as higher wet-sensitive sensitivity simultaneously again under 0～60%RH);
2) prepared polyelectrolyte/intrinsic conducting polymer composite humidity sensor is the basilar memebrane material with crosslinked quaternary ammoniated poly-4-vinylpyridine.This basilar memebrane material is at the humidity range (〉 33%RH of broad) in have very high wet-sensitive sensitivity, and response linearity is good under semilog coordinate;
When 3) preparing the polyelectrolyte basilar memebrane, precursor solution can improve the stability of precursor solution through precrosslink, is beneficial to the consistance of raising preparation basilar memebrane and the yield rate of humidity-sensitive element;
Crosslinked quaternary ammonium reaction takes place through thermal treatment in 4) prepared basilar memebrane, has cross-linked structure, can effectively improve the stability and the water tolerance of basilar memebrane; Thermal treatment simultaneously also can be eliminated high boiling solvent remaining in the basilar memebrane, reduces its influence for the basilar memebrane pattern, improves the stability of basilar memebrane;
5) introduce polypyrrole in the prepared polyelectrolyte/intrinsic conducting polymer composite humidity sensor, it also has good electric conductivity under low humidity, can effectively reduce the impedance of composite humidity sensor.It is with to have a polyelectrolyte basilar memebrane of high wet-sensitive sensitivity compound, makes composite humidity sensor (also have good wet-sensitive sensitivity, response linearity and recovery 0～60%RH) time at middle low humidity;
6) conductive polymer membrane is to obtain by the vapour phase polymerization growth in the prepared polyelectrolyte/intrinsic conducting polymer composite humidity sensor, and vapour phase polymerization can make composite membrane more even, smooth, thereby improves the consistance and the yield rate of element; Simultaneously can be very easily by changing the vapour phase polymerization growth temperature, time, and parameters such as oxygenant ammonium persulfate and adulterant 4-toluene sulfonic acide concentration, the content of polypyrrole in the adjusting composite humidity sensor, the impedance of control composite humidity sensor;
7) dip-coating method of Cai Yonging and vapour phase polymerization growing method prepare element, and be simple and easy to do, the element high conformity, and the yield rate height is suitable for producing in batches;
8) to have a volume little for humidity-sensitive element of the present invention, low cost, advantage such as easy to use.Interdigital width is 20～200 μ m, and interdigital gap is that the electrode structure of 20～200 μ m can make humidity-sensitive element resistance reduce, and sensing range is widened, and response sensitivity improves, and also can improve its stability simultaneously.This humidity-sensitive element can be widely used in the industrial and agricultural production process, and storage is accurately measured and control for ambient humidity during atmosphere environment supervision.
Description of drawings
Fig. 1 is the structural representation of humidity-sensitive element of the present invention;
Fig. 2 is the wet quick resonse characteristic (semilog coordinate) of polyelectrolyte/intrinsic conducting polymer composite humidity sensor basilar memebrane and composite membrane;
Fig. 3 is the response time curve of polyelectrolyte/intrinsic conducting polymer composite humidity sensor;
Fig. 4 is that the polyelectrolyte/intrinsic conducting polymer composite humidity sensor that makes under the different vapour phase polymerization temperature is at wide humidity (the wet quick resonse characteristic (semilog coordinate) during 0～98%RH) scope;
Fig. 5 is the polyelectrolyte/intrinsic conducting polymer composite humidity sensor that makes under the different vapour phase polymerization temperature at middle low humidity (the wet quick resonse characteristic (linear coordinate) 0～60%RH) time;
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, polyelectrolyte/intrinsic conducting polymer composite humidity sensor has devitrified glass matrix 1, have many to interdigital gold electrode 2 at the devitrified glass matrix surface, on interdigital gold electrode, be connected with lead-in wire 4, be coated with humidity sensitive thin film 3 at devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity sensitive thin film 3 is crosslinked quaternary ammoniated poly 4 vinyl pyridine and composite polypyrrole film.
The interdigital gold electrode of said microcrystalline glass matrix 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.
Embodiment 1:
1) glass-ceramic substrate of interdigital gold electrode is arranged with absolute ethyl alcohol and acetone soaking and washing photomask surface and evaporation, dry for standby;
2) will gather 4-vinylpyridine and 1,4-dibromobutane is dissolved in N, in N-dimethyl formamide, 4-vinylpyridine unit and 1 in the polymkeric substance, the mol ratio of 4-dibromobutane is 1:0.5, be mixed with the solution that polymer concentration is 10 mg/ml, place 4h, obtain precursor solution at 30 ℃;
3) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 0.5 minute, lift taking-up, crosslinked quaternary ammoniated 12h under 80 ℃ of temperature forms the polyelectrolyte basilar memebrane in the interdigital gold electrode surfaces of devitrified glass;
4) ammonium persulfate and 4-toluene sulfonic acide are dissolved in the deionized water, the mass ratio of ammonium persulfate and 4-toluene sulfonic acide is 1:0.2, and ammonium persulfate concentration is 0.2 mg/ml, obtains solution A;
5) adopt dip coater will impregnated in the solution A 1 minute through the interdigital gold electrode of devitrified glass of step 3) processing, after drying, vapour phase polymerization 12h in saturated pyrroles's steam of 0 ℃ is through absolute ethanol washing, 50 ℃ of oven dry obtain polyelectrolyte/intrinsic conducting polymer composite humidity sensor.
Embodiment 2:
1) electrode cleans with embodiment 1;
2) will gather 4-vinylpyridine and 1,4-dibromobutane is dissolved in N, in N-dimethyl formamide, 4-vinylpyridine unit and 1 in the polymkeric substance, the mol ratio of 4-dibromobutane is 1:2, be mixed with the solution that polymer concentration is 30 mg/ml, place 12h, obtain precursor solution at 30 ℃;
3) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 2 minutes, lift taking-up, crosslinked quaternary ammoniated 2h under 140 ℃ of temperature forms the polyelectrolyte basilar memebrane in the interdigital gold electrode surfaces of devitrified glass;
4) ammonium persulfate and 4-toluene sulfonic acide are dissolved in the deionized water, the mass ratio of ammonium persulfate and 4-toluene sulfonic acide is 1:3, and ammonium persulfate concentration is 4 mg/ml, obtains solution A;
5) adopt dip coater will impregnated in the solution A 6 minutes through the interdigital gold electrode of devitrified glass of step 3) processing, after drying, vapour phase polymerization 1h in saturated pyrroles's steam of 50 ℃ is through absolute ethanol washing, 80 ℃ of oven dry obtain polyelectrolyte/intrinsic conducting polymer composite humidity sensor.
Embodiment 3:
1) electrode cleans with embodiment 1;
2) will gather 4-vinylpyridine and 1,4-dibromobutane is dissolved in N, in N-dimethyl formamide, 4-vinylpyridine unit and 1 in the polymkeric substance, the mol ratio of 4-dibromobutane is 1:1, be mixed with the solution of polymer concentration 24 mg/ml, place 12h, obtain the electrolyte precursor liquid solution at 30 ℃;
3) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 1 minute, lift taking-up, crosslinked quaternary ammoniated 10h under 110 ℃ of temperature forms the polyelectrolyte basilar memebrane in the interdigital gold electrode surfaces of devitrified glass;
4) ammonium persulfate and 4-toluene sulfonic acide are dissolved in the deionized water,, the mass ratio of ammonium persulfate and 4-toluene sulfonic acide is 1:2, ammonium persulfate concentration is 1.5 mg/ml, obtains solution A;
5) adopt dip coater will impregnated in the solution A 4 minutes through the interdigital gold electrode of devitrified glass of step 3) processing, after drying, vapour phase polymerization 4h in saturated pyrroles's steam of 25 ℃ is through absolute ethanol washing, 70 ℃ of oven dry obtain polyelectrolyte/intrinsic conducting polymer composite humidity sensor.The polyelectrolyte basilar memebrane of the humidity-sensitive element that this example makes and the wet quick response characteristic of polyelectrolyte/intrinsic conducting polymer composite membrane are seen Fig. 2, as seen from the figure, behind the complex eigen conducting polymer, all have moderate resistance value at middle low humidity, make things convenient for moisture measurement.The response time properties of humidity-sensitive element is seen Fig. 3, and as seen from the figure, humidity-sensitive element has response soon, the good characteristic of recovery.
Figure 4 shows that the vapour phase polymerization temperature is respectively 3 ℃, the wet quick resonse characteristic (semilog coordinate) of the polyelectrolyte/intrinsic conducting polymer composite membrane humidity-sensitive element in the time of 25 ℃, as seen from the figure, (it is higher all to have sensitivity in 0～98%RH) scope, and the linearity is characteristic preferably in wide humidity for composite humidity sensor.
Figure 5 shows that the vapour phase polymerization temperature is respectively 3 ℃, the wet quick resonse characteristic (linear coordinate) of the polyelectrolyte/intrinsic conducting polymer composite membrane humidity-sensitive element in the time of 25 ℃, as seen from the figure, composite humidity sensor (has the good linearity and sensitivity at linear coordinate time at middle low humidity under 0～60%RH).
Claims (4)
1. polyelectrolyte/intrinsic conducting polymer composite humidity sensor, it is characterized in that: it has devitrified glass matrix (1), have many in photoetching of devitrified glass matrix surface and evaporation to interdigital gold electrode (2), on interdigital gold electrode, be connected with lead-in wire (4), be coated with humidity sensitive thin film (3) at devitrified glass matrix and interdigital gold electrode surfaces, humidity sensitive thin film is crosslinked quaternary ammoniated poly 4 vinyl pyridine and composite polypyrrole film.
2. polyelectrolyte/intrinsic conducting polymer composite humidity sensor according to claim 1, the interdigital gold electrode that it is characterized in that the devitrified glass matrix surface has 8～16 pairs, 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 polyelectrolyte/intrinsic conducting polymer composite humidity sensor according to claim 1 is characterized in that: may further comprise the steps:
1) clean surface photoetching and evaporation have the devitrified glass matrix of interdigital gold electrode, dry for standby;
2) will gather 4-vinylpyridine and 1,4-dibromobutane is dissolved in N, in N-dimethyl formamide, 4-vinylpyridine unit and 1 in the polymkeric substance, the mol ratio of 4-dibromobutane is 1:0.5～1:2, be mixed with the solution that polymer concentration is 10～30 mg/ml, place 4～12h, obtain precursor solution at 30 ℃;
3) adopt dip coater that the interdigital gold electrode of devitrified glass matrix of step 1) be impregnated in the precursor solution 0.5～2 minute, after lifting taking-up, crosslinked quaternary ammoniated 2～12h under 80～140 ℃ of temperature forms the polyelectrolyte basilar memebrane in the interdigital gold electrode surfaces of devitrified glass matrix;
4) ammonium persulfate and 4-toluene sulfonic acide are dissolved in the deionized water simultaneously, the mass ratio of ammonium persulfate and 4-toluene sulfonic acide is 1:0.2～1:3, and ammonium persulfate concentration is 0.2～4 mg/ml, obtains solution A;
5) adopt dip coater will impregnated in the solution A 1～6 minute through the interdigital gold electrode of devitrified glass matrix of step 3) processing, after drying, vapour phase polymerization 1～12h in saturated pyrroles's steam of 0～50 ℃, through absolute ethanol washing, 50～80 ℃ of oven dry obtain polyelectrolyte/intrinsic conducting polymer composite humidity sensor.
4. according to the method for making of the described polyelectrolyte/intrinsic conducting polymer composite humidity sensor of claim 3, it is characterized in that: the interdigital width of said interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
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| CN101799441A (en) * | 2010-03-09 | 2010-08-11 | 浙江大学 | Polymer resistor type humidity element of water dispersion nano-polyaniline and manufacturing method thereof |
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| CN101799441A (en) * | 2010-03-09 | 2010-08-11 | 浙江大学 | Polymer resistor type humidity element of water dispersion nano-polyaniline and manufacturing method thereof |
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