CN101324539A - Polymer compound resistor type humidity sensitive element with nanometer fiber structure and manufacturing method thereof - Google Patents
Polymer compound resistor type humidity sensitive element with nanometer fiber structure and manufacturing method thereof Download PDFInfo
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- CN101324539A CN101324539A CNA2008100632006A CN200810063200A CN101324539A CN 101324539 A CN101324539 A CN 101324539A CN A2008100632006 A CNA2008100632006 A CN A2008100632006A CN 200810063200 A CN200810063200 A CN 200810063200A CN 101324539 A CN101324539 A CN 101324539A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
Abstract
The invention discloses a polymer composite resistance-type humidity sensing element with a nanofiber structure and the preparation method thereof. The humidity sensing element adopts ceramics as a matrix, a plurality of pairs of interdigitated gold electrodes are arranged on the matrix, the surface of the ceramic matrix and the interdigitated gold electrodes are coated with poly (diallyldimethyl ammonium chloride) (PDDA) modifying film, and a poly-3-aminopropyl-triethoxysilane mono-brominated n-hexane quaternary ammonium salt, polyanion and polyoxyethylene composite nanofiber humidity sensing film with a cross-linked structure is settled on the modifying film. The humidity sensing film is in a good contact with an electrode substrate by means of the modifying film. The manufacturing method has the advantages of simple process and low cost. The prepared humidity sensing element has the characteristics of moderate impedance value in a wide humidity range, high sensitivity, good linearity, rapid response, good resilience, good stability, etc., and is widely applicable in precise measurement and control of ambient humidity in industrial and agricultural production process, storage, and atmospheric environment monitoring.
Description
Technical field
The present invention relates to a kind of polymer compound resistor type humidity sensitive element and preparation method thereof with nanofibrous structures.
Background technology
The accurate measurement of humidity has vital role in industrial and agricultural production and environmental monitoring, this development for humidity sensor provides wide space.The polymer electrolyte humidity sensor is a development in recent years class humidity sensor very rapidly, compares traditional ceramic mould humidity sensor, and it is good that it has response characteristic, measurement range is wide, good stability, but room temperature detects, 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, be easy to realize moisture measurement and control in the system of being integrated in, and preparation is very easy, has become the important directions of humidity sensor development now.Yet, the humidity-sensitive material of present most of polymer electrolyte humidity-sensitive element is that the form with dense film exists, therefore humidity-sensitive material is when perception external environment humidity changes, hydrone adsorbs, diffuses into sensitive membrane inside, and in the dehumidification process hydrone remove relatively slowly, this causes sensitivity, the response time of element to be subjected to great restriction.And the employing electrostatic spinning technique, can be than being easier to prepare responsive fibrous material with sub-micron or even nanostructured, make humidity-sensitive material pile up the three-dimensional open structure development that forms to multi-layer fiber by individual layer, plane compact texture, improved the contact gear ratio surface area of humidity-sensitive material and external environment greatly, help absorption, diffusion and the desorption of hydrone on sensitive membrane, thereby improve response sensitivity, accelerate the response time, reduce humidity hysteresis.Therefore, prepare nanofiber high molecule humidity sensor, be expected to become a kind of novel method for preparing the high-performance humidity sensor with high-specific surface area by electrostatic spinning technique.
Summary of the invention
The purpose of this invention is to provide a kind of polymer compound resistor type humidity sensitive element and preparation method thereof with nanofibrous structures.
Polymer compound resistor type humidity sensitive element with nanofibrous structures of the present invention, has ceramic matrix, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode, on interdigital gold electrode, be connected with lead-in wire, be coated with modified membrane at ceramic matrix and interdigital gold electrode surfaces, the modified membrane surface deposition has the humidity sensitive thin film of nanofibrous structures, said modified membrane is a diallyl dimethyl ammoniumchloride, and the humidity sensitive thin film of nanofibrous structures is to have the poly-3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt of cross-linked structure and the compound of polyaniline and polyoxyethylene.
Have the method for making of the polymer compound resistor type humidity sensitive element of nanofibrous structures, may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic matrix of interdigital gold electrode, oven dry;
2) the interdigital gold electrode of the ceramic matrix of step 1) be impregnated in the aqueous solution that mass concentration is 0.1%～0.25% diallyl dimethyl ammoniumchloride, lift, dry;
3) adopt method of electrostatic spinning that the nano-fiber composite film that spinning solution is spun into is deposited on step 2) on the interdigital gold electrode of the ceramic matrix that is coated with the diallyl dimethyl ammoniumchloride modified membrane that makes, 80～110 ℃ of following thermal treatments 8～16 hours, obtain having the polymer compound resistor type humidity sensitive element of nanofibrous structures, spinning solution is the mixed liquor of following component, each component is by weight percentage: 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is 5.2～6.1%, polyoxyethylene is 5.2～6.1%, water soluble alkali formula polyaniline is 0.75～2.3%, and camphorsulfonic acid 0.75～2.3%, absolute ethyl alcohol is 28.8～30.6%, and chloroform is 54.4～57.5%.
The interdigital width of the above-mentioned interdigital gold electrode in ceramic matrix surface is 20～200 μ m, and interdigital gap is 20～200 μ m.
Advantage of the present invention is:
1) has the polymer compound resistor type humidity sensitive element of nanofibrous structures, it is the method preparation of adopting electrostatic spinning, it has multi-layer fiber and piles up the three-dimensional open structure that forms, improved the specific surface area of humidity-sensitive material greatly, be beneficial to absorption, diffusion and the desorption of hydrone, advantages such as the humidity-sensitive element of feasible preparation has the response sensitivity height, response speed is fast, and humidity hysteresis is little;
2) have in the process of polymer compound resistor type humidity sensitive element of nanofibrous structures in preparation, adopt diallyl dimethyl ammoniumchloride that electrode is modified, thereby effectively improved electrostatic spinning and prepared contacting of nanofiber and electrode matrix, obviously reduce component resistance, solved the problem of the resistor-type air humidity photosensitive elements application of this obstruction method of electrostatic spinning preparation;
3) it is simple to utilize method of electrostatic spinning to prepare the polymer compound resistor type humidity sensitive element process of nanofibrous structures, can be easily by changing technological parameter (distance of the spinning voltage of electrostatic spinning apparatus, syringe needle and receiver sheet, the composition of solution, flow velocity and spinning time etc.), preparation has the nanofiber humidity sensing film that different-diameter, difference are piled up thickness, realizes the regulation and control to its wet quick response characteristic;
4) the prepared polymer compound resistor type humidity sensitive element with nanofibrous structures as humidity-sensitive material, has higher response sensitivity and response linearity preferably with poly-this siliceous polyelectrolyte of 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt with cross-linked structure in the humidity range of broad;
5) prepared nanofiber sensitive membrane makes the polymerization of 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt self-crosslinking through thermal treatment, can effectively improve the stability and the water tolerance of humidity-sensitive film; Thermal treatment simultaneously can be eliminated solvent remaining in the nanofiber sensitive membrane, reduces its influence for nanofiber sensitive membrane pattern, improves its stability;
6) contain the intrinsic conducting polymer polyaniline in the prepared compound humidity-sensitive material of high polymer nanometer fiber, it has good intrinsic electronic conduction characteristic, can effectively reduce the impedance of composite humidity sensor under low humidity, make the nanofiber composite humidity sensor when middle low humidity, have good wet-sensitive sensitivity and response linearity;
7) 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 the interdigital gold electrode structure of 20～200 μ m, and ceramic matrix can improve the contact of nano fibrous membrane and electrode matrix, the stability of raising element.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 scanning electron microscope picture of humidity sensitive thin film with polymer compound resistor type humidity sensitive element of nanofibrous structures;
Fig. 3 is before and after the coating modified membrane, has the wet quick resonse characteristic (semilog coordinate) of the polymer compound resistor type humidity sensitive element of nanofibrous structures;
Fig. 4 is the wet quick resonse characteristic (semilog coordinate) that adopts the polymer compound resistor type humidity sensitive element of traditional dip-coating method and electrospinning process preparation;
Fig. 5 is the response time curve with polymer compound resistor type humidity sensitive element of nanofibrous structures;
Fig. 6 is the humidity hysteresis curve with polymer compound resistor type humidity sensitive element of nanofibrous structures.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, polymer compound resistor type humidity sensitive element with nanofibrous structures of the present invention, has ceramic matrix 1, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode 2, on interdigital gold electrode, be connected with lead-in wire 5, be coated with diallyl dimethyl ammoniumchloride modified membrane 3 at ceramic matrix and interdigital gold electrode surfaces, at the modified membrane surface deposition the compound humidity sensitive thin film 4 of nanofiber is arranged, humidity sensitive thin film is to have the poly-3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt of cross-linked structure and the compound of polyaniline and polyoxyethylene.
The interdigital width of the interdigital gold electrode in above-mentioned ceramic matrix surface is 20～200 μ m, and interdigital gap is 20～200 μ m.
Embodiment 1:
1) ceramic matrix that photoetching and evaporation are had an interdigital gold electrode with absolute ethyl alcohol and acetone soak, ultrasonic cleaning, dry for standby;
2) with dip coater the interdigital gold electrode of ceramic matrix be impregnated in the aqueous solution that mass concentration is 0.25% diallyl dimethyl ammoniumchloride, lift, take out, dry;
3) nano-fiber composite film that adopts method of electrostatic spinning that spinning solution is spun into is deposited on and is being coated with on the ceramic interdigital gold electrode of modified membrane, then, 80 ℃ of following thermal treatments 16 hours, obtains having the polymer compound resistor type humidity sensitive element of nanofibrous structures.Each component of the spinning liquid of electrostatic spinning is by weight percentage: 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is 5.2%, polyoxyethylene is 5.2%, and water soluble alkali formula polyaniline is 0.75%, and camphorsulfonic acid 0.75%, absolute ethyl alcohol is 30.6%, and chloroform is 57.5%.The electrostatic spinning condition is: 20 minutes spinning time, and 10 kilovolts of electrostatic spinning voltages, 10 centimetres of the distances of syringe needle and receiver sheet, 0.1 milliliter/hour of spinning solution flow velocity, spinning temperature: 20～35 ℃, ambient humidity: 25～45%RH.
Embodiment 2:
1) ceramic matrix that photoetching and evaporation are had an interdigital gold electrode with absolute ethyl alcohol and acetone soak, ultrasonic cleaning, dry for standby;
2) with dip coater the interdigital gold electrode of pottery be impregnated in the aqueous solution that mass concentration is 0.1% diallyl dimethyl ammoniumchloride, lift, take out, dry;
3) nano-fiber composite film that adopts method of electrostatic spinning that spinning solution is spun into is deposited on and is being coated with on the ceramic interdigital gold electrode of modified membrane, then, 100 ℃ of following thermal treatments 12 hours, obtain having the polymer compound resistor type humidity sensitive element of nanofibrous structures.Each component of the spinning liquid of electrostatic spinning is by weight percentage: 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is 6.1%, polyoxyethylene is 6.1%, and water soluble alkali formula polyaniline is 2.3%, and camphorsulfonic acid 2.3%, absolute ethyl alcohol is 28.8%, and chloroform is 54.4%.The electrostatic spinning condition is: 30 minutes spinning time, and 10 kilovolts of electrostatic spinning voltages, 10 centimetres of the distances of syringe needle and receiver sheet, 0.2 milliliter/hour of spinning solution flow velocity, spinning temperature: 20～35 ℃, ambient humidity: 25～45%RH.
Embodiment 3:
1) ceramic matrix that photoetching and evaporation are had an interdigital gold electrode with absolute ethyl alcohol and acetone soak, ultrasonic cleaning, dry for standby;
2) with dip coater the interdigital gold electrode of pottery be impregnated in the aqueous solution that mass concentration is 0.2% diallyl dimethyl ammoniumchloride, lift, take out, dry;
3) nano-fiber composite film that adopts method of electrostatic spinning that spinning solution is spun into is deposited on and is being coated with on the ceramic interdigital gold electrode of modified membrane, then, 90 ℃ of following thermal treatments 14 hours, obtains having the polymer compound resistor type humidity sensitive element of nanofibrous structures.Each component of the spinning liquid of electrostatic spinning is by weight percentage: 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is 5.6%, polyoxyethylene is 5.6%, and water soluble alkali formula polyaniline is 1.5%, and camphorsulfonic acid 1.5%, absolute ethyl alcohol is 29.6%, and chloroform is 56.2%.The electrostatic spinning condition is: 40 minutes spinning time, and 15 kilovolts of electrostatic spinning voltages, 15 centimetres of the distances of syringe needle and receiver sheet, 0.1 milliliter/hour of spinning solution flow velocity, spinning temperature: 20～35 ℃, ambient humidity: 25～45%RH.
The humidity sensitive thin film scanning electron microscope picture of the polymer compound resistor type humidity sensitive element with nanofibrous structures that the inventive method makes is seen Fig. 2, and as seen from the figure, the humidity sensitive thin film of preparation is piled up by nanofiber and formed, and the diameter of fiber is about 300 nanometers;
As seen from Figure 3, after the diallyl dimethyl ammoniumchloride modified electrode, the polymer compound resistor type humidity sensitive element of the nanofibrous structures of preparation has very high sensitivity, and have good response linearity under semilog coordinate in the humidity range of broad;
As seen from Figure 4, compare with the method for traditional dip-coating film forming, with the polymer compound resistor type humidity sensitive element of the nanofibrous structures of electrospinning process preparation, wet quick characteristic such as sensitivity, the linearity has all obtained tangible improvement;
Figure 5 shows that the response time curve of the polymer compound resistor type humidity sensitive element with nanofibrous structures, by the figure finding, the nanofiber composite humidity sensor has than response speed faster, and moisture absorption and dehumidification time are all shorter;
Figure 6 shows that the humidity hysteresis curve of the polymer compound resistor type humidity sensitive element with nanofibrous structures, by the figure finding, nanofiber composite humidity sensor humidity hysteresis is less, and response has good recovery.
Claims (4)
1. polymer compound resistor type humidity sensitive element with nanofibrous structures, it is characterized in that it has ceramic matrix (1), have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode (2), on interdigital gold electrode, be connected with lead-in wire (5), be coated with modified membrane (3) at ceramic matrix and interdigital gold electrode surfaces, the modified membrane surface deposition has the humidity sensitive thin film (4) of nanofibrous structures, said modified membrane (3) is a diallyl dimethyl ammoniumchloride, and the humidity sensitive thin film of nanofibrous structures (4) is for having the poly-3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt of cross-linked structure and the compound of polyaniline and polyoxyethylene.
2. the polymer compound resistor type humidity sensitive element with nanofibrous structures according to claim 1, the interdigital width that it is characterized in that the interdigital gold electrode on ceramic matrix surface are 20～200 μ m, and interdigital gap is 20～200 μ m.
3. the method for making with polymer compound resistor type humidity sensitive element of nanofibrous structures according to claim 1 is characterized in that may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic matrix of interdigital gold electrode, oven dry;
2) the interdigital gold electrode of the ceramic matrix of step 1) be impregnated in the aqueous solution that mass concentration is 0.1%～0.25% diallyl dimethyl ammoniumchloride, lift, dry;
3) adopt method of electrostatic spinning that the nano-fiber composite film that spinning solution is spun into is deposited on step 2) on the interdigital gold electrode of the ceramic matrix that is coated with the diallyl dimethyl ammoniumchloride modified membrane that makes, 80～110 ℃ of following thermal treatments 8～16 hours, obtain having the polymer compound resistor type humidity sensitive element of nanofibrous structures, spinning solution is the mixed liquor of following component, each component is by weight percentage: 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is 5.2～6.1%, polyoxyethylene is 5.2～6.1%, water soluble alkali formula polyaniline is 0.75～2.3%, and camphorsulfonic acid 0.75～2.3%, absolute ethyl alcohol is 28.8～30.6%, and chloroform is 54.4～57.5%.
4. the method for making with polymer compound resistor type humidity sensitive element of nanofibrous structures according to claim 3, it is characterized in that the electrostatic spinning condition is: 20～80 minutes spinning time, 10～25 kilovolts of electrostatic spinning voltages, 5～20 centimetres of the distances of syringe needle and receiver sheet, 0.1～0.2 milliliter/hour of spinning solution flow velocity, spinning temperature: 20～35 ℃, ambient humidity: 25～45%RH.
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| CN101788520A (en) * | 2010-03-16 | 2010-07-28 | 浙江大学 | Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof |
| 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 |
| 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 |
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| US4681855A (en) * | 1985-08-05 | 1987-07-21 | The United States Of America As Represented By The Secretary Of Commerce | Humidity sensing and measurement employing halogenated organic polymer membranes |
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| CN101788520A (en) * | 2010-03-16 | 2010-07-28 | 浙江大学 | Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof |
| 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 |
| CN102323300A (en) * | 2011-07-18 | 2012-01-18 | 浙江大学 | Polyelectrolyte and graphene composite resistive moisture sensor and manufacturing method thereof |
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| CN102519504A (en) * | 2011-12-19 | 2012-06-27 | 浙江大学 | Acoustic surface wave type humidity sensor based on conductive polymer composite nano-fibre and preparation method thereof |
| CN104502420A (en) * | 2014-10-01 | 2015-04-08 | 浙江大学 | Humidity-sensitive composite membrane, preparation method of humidity-sensitive composite membrane and humidity sensor |
| CN107533027A (en) * | 2015-02-17 | 2018-01-02 | 霍尼韦尔国际公司 | Humidity sensor and the method for manufacturing the sensor |
| CN107179337A (en) * | 2017-05-25 | 2017-09-19 | 郑州大学 | A kind of bimodulus humidity sensor and preparation method thereof |
| CN108414584A (en) * | 2018-03-05 | 2018-08-17 | 北京化工大学 | A kind of preparation method of flexible, wearable moisture sensor and its application in breathing detection |
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