CN102072927A - Preparation method for fast-response and wide-range ceramic-based nano-fiber humidity sensor - Google Patents
Preparation method for fast-response and wide-range ceramic-based nano-fiber humidity sensor Download PDFInfo
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Abstract
The present invention belongs to the technical field of preparation of a humidity sensor, and particularly relates to a method for preparation of a fast-response and wide-range ceramic-based nano-fiber humidity sensor by adopting an electrospinning technique. Soluble metal salts, esters, conductive polymers and organic solvents are used as raw materials. The method comprises the following steps: preparing composite fibers containing the conductive polymers and composite metal oxide precursors by adopting the electrospinning technique, calcining the fibers to remove organic polymer components, and obtaining ceramic-based perovskite-type composite metal oxide nanofibers. The humidity sensor made with the one-dimensional, ultra-long and continuous perovskite-type composite metal oxide ceramic nanofibers has the advantages of wide range of humidity measurement, small humidity hysteresis, high linearity, rapid response and recovery and the like. The method is suitable for preparation of ceramic oxides and composite oxides with various soluble metal salts as the raw materials, has the advantages that the equipment has a simple structure, a good performance and a low cost, is easy to promote, can satisfy the requirements of industrial technologies, and is widely applied in such fields as the industry, agriculture, storage, meteorology and the like.
Description
Technical field
The invention belongs to Tao Ci Ji Calcium titanium ore type composite metal oxide humidity sensor preparing technical field, be specifically related to a kind of method of utilizing electrospinning silk technology to prepare fast-response, wide-range ceramic base nanometer fibre humidity sensor.
Background technology
In the environment of our life, the humidity of air or degree of drying have very big influence to our live and work, air is too wet or too dried all can to make us feel oppressiveness and suffocate, and the humidity of air or degree of drying also have very big influence to the quality of product on commercial production.Therefore no matter at life or production field, humidity sensor all plays a part very important.Commercially available humidity sensor mostly is to be sensitive layer with the macromolecular material at present, though this humidity sensor also has wide work range, its response recovery time is longer, and the fastest also got about 1 minute.But in many application of power industry, because the demand of aspects such as security requires the response of humidity sensor to want special sensitive.Therefore in order to be well positioned to meet the needs of life and production, a kind of humidity sensor that can in wide humidity range, work of exigence with quick response recovery characteristics.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of fast-response, wide-range ceramic base nanometer fibre humidity sensor.
Implementation procedure of the present invention comprises two parts, and the making of the making of nanofiber and ceramic base nm-humidity sensor may further comprise the steps:
(1) 0.5～5.0g water-soluble high-molecular compound is joined in 2～15ml ethanol or the dimethyl formamide (DMF), stirred 4～8 hours, it is dissolved fully at 20～30 ℃ of lower magnetic forces;
(2) 0.1～2g ester is joined in the mixed solution of 0.2～4ml glacial acetic acid and 0.2～4ml ethanol, or 0.1～2g ester is joined in the mixed solution of 0.2～4ml glacial acetic acid and 0.2～4ml DMF, 20～30 ℃ of lower magnetic forces stirred 20～50 minutes, and it is mixed;
(3) 0.1～2g soluble metallic salt is joined in 1～5ml deionized water, be stirred to dissolving fully; Then this metal salt solution is joined in the solution of step (2), 20～30 ℃ of lower magnetic forces stirred 20～50 minutes, and solution is mixed;
(4) mixed solution that step (3) is obtained joins in the solution of step (1), and 20～30 ℃ of lower magnetic forces stirred 30～60 minutes, and solution is mixed;
(5) in the solution injected plastic spray fiber tube that step (4) is obtained, plastics spray fiber tube head internal diameter is 1～1.5mm, with the copper wire is anode, receive product with aluminium foil as minus plate, distance is 10～30cm between anode and minus plate, apply 10～30kV voltage and carry out the electrospinning silk, after spinning in 12～36 hours, collect the nano fibrous membrane of the pbz polymer compound that obtains on the aluminium foil, then 750～900 ℃ of following sintering 2～6 hours to remove the macromolecule template, obtain the nanofiber of diameter 80～200nm.
(6) nanofiber that step (5) is obtained adds in the deionized water, the concentration that makes nanofiber is 0.1～0.3g/ml, obtain thick responsive slurry, then with responsive slurry for rotary coating to the interdigited electrode of ceramic base plane, 20～30 ℃ are descended dry 8～12 hours then, thereby obtain the ceramic base nanometer fibre humidity sensor.
The used ceramic base plane interdigited electrode substrate of the present invention is Al
2O
3Pottery, five couples of interdigitated Ag-Pd of serigraphy electrode on it, distance is 200 μ m between the electrode, entire electrode is of a size of 6mm * 3mm * 1mm.
In step (2), glacial acetic acid is identical with the volume of ethanol or glacial acetic acid and DMF, and the volume of glacial acetic acid and ethanol or glacial acetic acid and DMF and be a times of metal ester volume.
Water-soluble high-molecular compound described in the inventive method is polyvinylpyrrolidone or polyvinyl alcohol (PVA), and described ester is a butyl titanate, and described soluble metallic salt is soluble barium salt or strontium salt, as barium acetate, barium nitrate, strontium acetate, strontium nitrate.
Macromolecule raw material described in the inventive method, slaine and solvent all can obtain with commercial form from Chemical Reagent Co., Ltd., Sinopharm Group.
The fast-response that the present invention obtains, the ceramic base nanometer fibre humidity sensor in the wide-range have following characteristics:
1. electrical spinning method technology is simple, is convenient to operation, and is with low cost, and have good repeatability, preparation nanofiber that can be more or less freely.The ceramic base resistance type humidity sensor, simple in structure, with low cost, be easy to promotion and application.
2. the nano wire fiber has bigger specific surface area, effectively raises the speed of charge carrier radial transport, makes this ceramic base nanometer fibre humidity sensor that very high response resume speed be arranged;
3. the sensitive mechanism of nanofiber humidity sensor is: the hydrone quantity generation conversion that is adsorbed on the sensitive material surface along with the variation of ambient humidity, material surface and inner conducting particles quantity change, thereby make the resistance of humidity sensor change.
Description of drawings
Fig. 1: the ceramic base nanometer fibre humidity sensor synoptic diagram of made of the present invention;
Wherein Fig. 1 (a) is a three-dimensional view; Fig. 1 (b) is a front elevation;
The each several part name is called: alundum (Al substrate 1, silver-palladium interdigital electrode 2, nanofiber sensitive membrane 3;
Fig. 2: embodiment 1 prepared barium acetate/butyl titanate/macromolecule (PVP) potpourri nanofiber stereoscan photograph;
Fig. 3: embodiment 1 prepared barium titanate nano fiber stereoscan photograph;
Fig. 4: embodiment 2 prepared barium acetate/butyl titanate/macromolecule (PVP) potpourri nanofiber stereoscan photographs;
Fig. 5: embodiment 2 prepared barium titanate nano fiber stereoscan photographs;
Fig. 6: embodiment 3 prepared barium acetate/butyl titanate/macromolecule (PVP) potpourri nanofiber stereoscan photographs;
Fig. 7: embodiment 3 prepared barium titanate nano fiber stereoscan photographs;
Fig. 8: embodiment 4 prepared barium acetate/butyl titanate/macromolecule (PVP) potpourri nanofiber stereoscan photographs;
Fig. 9: embodiment 4 prepared barium titanate nano fiber stereoscan photographs;
Figure 10: embodiment 5 prepared strontium acetate/butyl titanate/macromolecule (PVP) potpourri nanofiber stereoscan photographs;
Figure 11: embodiment 5 prepared strontium titanates nanofiber stereoscan photographs;
The humidity hysteresis performance plot of the prepared humidity sensor based on the barium titanate nano fiber of Figure 12: embodiment 2;
The response recovery characteristics curve of the prepared humidity sensor based on the barium titanate nano fiber of Figure 13: embodiment 2.
The humidity hysteresis performance plot of the prepared humidity sensor based on the barium titanate nano fiber of Figure 14: embodiment 3;
The response recovery characteristics curve of the prepared humidity sensor based on the barium titanate nano fiber of Figure 15: embodiment 3.
As shown in Figure 1, the substrate of the used nanofiber humidity sensor of the present invention is Al2O
3Pottery is of a size of 6mm * 3mm * 1mm, five couples of interdigitated Ag-Pd of serigraphy electrode on it, and distance is 200 μ m between the electrode. The Ca-Ti ore type nanofiber sensitive membrane that applies preparation at this substrate namely makes the nanofiber humidity sensor.
As shown in Figure 2, the stereoscan photograph of embodiment 1 prepared barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber, can find out that the present invention makes barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber pattern is good, diameter is even, and specific area is big. Fibre diameter is distributed between 160～310nm substantially, and length is greater than 1mm.
As shown in Figure 3, embodiment 1 prepared mixture of nanofibers is through the stereoscan photograph after 800 ℃ of high temperature sinterings. Can find out that nanofiber does not change through pattern after the high temperature sintering, but along with the volatilization fibre diameter of macromolecular material diminishes. Between 100～220nm, length is greater than 1mm respectively for fibre diameter after the sintering.
As shown in Figure 4, the stereoscan photograph of embodiment 2 prepared barium acetate/butyl titanate/macromolecule (PVP) mixture nanofibers, can find out that the present invention makes barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber pattern is good, diameter is even, and specific area is big. Fibre diameter is distributed between 150～300nm substantially, and length is greater than 1mm.
As shown in Figure 5, embodiment 2 prepared mixture of nanofibers are through the stereoscan photograph after 800 ℃ of high temperature sinterings. Can find out that nanofiber does not change through pattern after the high temperature sintering, but along with the volatilization fibre diameter of macromolecular material diminishes. Between 80～200nm, length is greater than 1mm respectively for fibre diameter after the sintering.
As shown in Figure 6, the stereoscan photograph of embodiment 3 prepared barium acetate/butyl titanate/macromolecule (PVP) mixture nanofibers, can find out that the present invention makes barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber pattern is good, diameter is even, and specific area is big. Fibre diameter is distributed between 180～330nm substantially, and length is greater than 1mm.
As shown in Figure 7, embodiment 3 prepared mixture of nanofibers are through the stereoscan photograph after 800 ℃ of high temperature sinterings. Can find out that nanofiber does not change through pattern after the high temperature sintering, but along with the volatilization fibre diameter of macromolecular material diminishes. Between 120～250nm, length is greater than 1mm respectively for fibre diameter after the sintering.
As shown in Figure 8, the stereoscan photograph of embodiment 4 prepared barium acetate/butyl titanate/macromolecule (PVP) mixture nanofibers, can find out that the present invention makes barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber pattern is good, diameter is even, and specific area is big. Fibre diameter is distributed between 150～280nm substantially, and length is greater than 1mm.
As shown in Figure 9, embodiment 4 prepared mixture of nanofibers are through the stereoscan photograph after 800 ℃ of high temperature sinterings. Can find out that nanofiber does not change through pattern after the high temperature sintering, but along with the volatilization fibre diameter of macromolecular material diminishes. Between 90～210nm, length is greater than 1mm respectively for fibre diameter after the sintering.
As shown in figure 10, the stereoscan photograph of embodiment 5 prepared strontium acetate/butyl titanate/macromolecule (PVP) mixture nanofibers, can find out that the present invention makes barium acetate/butyl titanate/macromolecule (PVP) mixture nanofiber pattern is good, diameter is even, and specific area is big. Fibre diameter is distributed between 170～320nm substantially, and length is greater than 1mm.
As shown in figure 11, embodiment 5 prepared mixture of nanofibers are through the stereoscan photograph after 800 ℃ of high temperature sinterings. Can find out that nanofiber does not change through pattern after the high temperature sintering, but along with the volatilization fibre diameter of macromolecular material diminishes. Between 105～220nm, length is greater than 1mm respectively for fibre diameter after the sintering.
As shown in figure 12, the prepared humidity sensor based on the barium titanate nano fiber of embodiment 2 is along with the increase resistance value of relative humidity reduces, from 11%RH～95%RH change in impedance value 4 orders of magnitude, humidity hysteresis is about 3%RH in 54%RH.
As shown in figure 13, the response time of embodiment 2 prepared barium titanate nano fiber humidity sensors is 2s, and be 3s recovery time.
As shown in figure 14, the prepared humidity sensor based on the barium titanate nano fiber of embodiment 3 is along with the increase resistance value of relative humidity reduces, from 11%RH～95%RH change in impedance value 3 orders of magnitude, humidity hysteresis is about 4%RH in 54%RH.
As shown in figure 15, the response time of embodiment 3 prepared barium titanate nano fiber humidity sensors is 4s, and be 5s recovery time.
Embodiment
By following examples the inventive method is described further.
Embodiment 1:
In the 30ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 3ml ethanol, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 2ml ethanol successively, 2ml glacial acetic acid and 1g butyl titanate, and 25 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 0.75g barium acetate is added in the 1ml deionized water, is stirred to dissolving fully.To dissolve good barium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 18kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 100～220nm De Calcium titanium ore type barium titanate nano fiber 1.0g.0.1g nanofiber wherein is dissolved in the 1ml deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 3.5%RH in 54%RH.Response time is 4s, and be 5s release time.
Embodiment 2:
In the 30ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 3ml ethanol, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 2ml ethanol successively, 2ml glacial acetic acid and 1g butyl titanate, and 25 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 0.75g barium acetate is added in the 1ml deionized water, is stirred to dissolving fully.To dissolve good barium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 20kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 80～200nm De Calcium titanium ore type barium titanate nano fiber 1.0g.0.1g nanofiber wherein is dissolved in the deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 3%RH in 54%RH.Response time is 2s, and be 3s release time.
Embodiment 3:
In the 30ml conical flask, the 1.0g polyvinylpyrrolidone is added among the 3mlDMF, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 2mlDMF successively, 2ml glacial acetic acid and 1g butyl titanate, and 25 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 0.75g barium acetate is added in the 1ml deionized water, is stirred to dissolving fully.To dissolve good barium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is about 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 20kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 120～250nm De Calcium titanium ore type barium titanate nano fiber 1.0g.0.1g nanofiber wherein is dissolved in the deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 2%RH in 54%RH.Response time is 4s, and be 5s release time.
Embodiment 4:
In the 30ml conical flask, the 2.0g polyvinylpyrrolidone is added in the 6ml ethanol, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 4ml ethanol successively, 4ml glacial acetic acid and 2g butyl titanate, and 20～30 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 1..5g barium acetate is added in the 2ml deionized water, is stirred to dissolving fully.To dissolve good barium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is about 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 20kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 90～210nm De Calcium titanium ore type barium titanate nano fiber 2.0g.0.1g nanofiber wherein is dissolved in the deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 3%RH in 54%RH.Response time is 3s, and be 4s release time.
Embodiment 5:
In the 30ml conical flask, the 2.0g polyvinylpyrrolidone is added in the 6ml ethanol, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 4ml ethanol successively, 4ml glacial acetic acid and 2g butyl titanate, and 25 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 1..5g strontium acetate is added in the 2ml deionized water, is stirred to dissolving fully.To dissolve good strontium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is about 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 20kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 105～220nm De Calcium titanium ore type strontium titanates nanofiber 2.0g.0.1g nanofiber wherein is dissolved in the deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 4%RH in 54%RH.Response time is 3.5s, and be 5s release time.
Embodiment 6:
In the 30ml conical flask, the 4.0g polyvinyl alcohol (PVA) is added in the 6ml ethanol, stirred 4 hours at 25 ℃ of lower magnetic forces, it is dissolved fully.
Other gets a 30ml conical flask, adds 4ml ethanol successively, 4ml glacial acetic acid and 2g butyl titanate, and 25 ℃ of lower magnetic forces stirred 20 minutes, and it is mixed.
Other gets a 30ml conical flask, and the 1..5g barium acetate is added in the 2ml deionized water, is stirred to dissolving fully.To dissolve good barium solution then and join in the ester solution that mixes, 25 ℃ of lower magnetic forces stirred 20 minutes, and solution is mixed.At last this mixed solution is joined in the Polymer Solution, continue to stir 20 minutes, solution is mixed at 25 ℃ of lower magnetic forces;
With mix solution put into plastics sprays fiber tube, plastics spinning head internal diameter is about 1mm, with the copper wire is anode, receive product with aluminium foil as negative electrode, distance is 25cm between two-plate, applies 20kV voltage and carries out the electrospinning silk, after spinning in 36 hours, collect the nano fibrous membrane of pbz polymer template, put into muffle furnace then, slowly be warming up to 800 ℃ of constant temperature sintering 2 hours.Obtaining diameter is 105～220nm De Calcium titanium ore type barium titanate nano fiber 2.0g.0.1g nanofiber wherein is dissolved in the deionized water, obtains thick responsive slurry, it is spun on ceramic base silver-palladium interdigited electrode, 25 ℃ of dryings are 12 hours then.Obtain the nanofiber humidity sensor thus, its humidity hysteresis is about 3%RH in 54%RH.Response time is 3s, and be 5s release time.
Claims (6)
1. the preparation method of fast-response, wide-range ceramic base nanometer fibre humidity sensor, its step is as follows:
(1) 0.5～5.0g water-soluble high-molecular compound is joined among 2～15ml ethanol or the dimethyl formamide DMF, stirred 4～8 hours, it is dissolved fully at 20～30 ℃ of lower magnetic forces;
(2) 0.1～2g ester is joined in the mixed solution of 0.2～4ml glacial acetic acid and 0.2～4ml ethanol, or 0.1～2g ester is joined in the mixed solution of 0.2～4ml glacial acetic acid and 0.2～4ml DMF, 20～30 ℃ of lower magnetic forces stirred 20～50 minutes, and it is mixed;
(3) 0.1～2g soluble metallic salt is joined in 1～5ml deionized water, be stirred to dissolving fully; Then this metal salt solution is joined in the solution of step (2), 20～30 ℃ of lower magnetic forces stirred 20～50 minutes, and solution is mixed;
(4) mixed solution that step (3) is obtained joins in the solution of step (1), and 20～30 ℃ of lower magnetic forces stirred 30～60 minutes, and solution is mixed;
(5) solution that step (4) is obtained is injected in the plastics spray fiber tube, plastics spray fiber tube head internal diameter is 1～1.5mm, with the copper wire is anode, receive product with aluminium foil as minus plate, distance is 10～30cm between anode and minus plate, apply 10～30kV voltage and carry out the electrospinning silk, after spinning in 12～36 hours, collect the nano fibrous membrane of the pbz polymer compound that obtains on the aluminium foil, then 750～900 ℃ of following sintering 2～6 hours to remove the macromolecule template, obtain the nanofiber of diameter 80～200nm;
(6) nanofiber that step (5) is obtained joins in the deionized water, the concentration that makes nanofiber is 0.1～0.3g/ml, obtain thick responsive slurry, then with responsive slurry for rotary coating to the interdigited electrode of ceramic base plane, drying is 8～12 hours under 20～30 ℃, thereby obtains the ceramic base nanometer fibre humidity sensor.
2. the preparation method of fast-response as claimed in claim 1, wide-range ceramic base nanometer fibre humidity sensor is characterized in that: water-soluble high-molecular compound is polyvinylpyrrolidone or polyvinyl alcohol (PVA).
3. the preparation method of fast-response as claimed in claim 1, wide-range ceramic base nanometer fibre humidity sensor is characterized in that: described ester is a butyl titanate.
4. the preparation method of fast-response as claimed in claim 1, wide-range ceramic base nanometer fibre humidity sensor is characterized in that: described soluble metallic salt is barium acetate, barium nitrate, strontium acetate or strontium nitrate.
5. the preparation method of fast-response as claimed in claim 1, wide-range ceramic base nanometer fibre humidity sensor is characterized in that: ceramic base plane interdigited electrode substrate is Al
2O
3Pottery, five couples of interdigitated Ag-Pd of serigraphy electrode on it, distance is 200 μ m between the electrode, electrode size is 6mm * 3mm * 1mm.
6. the preparation method of fast-response as claimed in claim 1, wide-range ceramic base nanometer fibre humidity sensor, it is characterized in that: in step (2), glacial acetic acid is identical with the volume of ethanol or glacial acetic acid and DMF, and the volume of glacial acetic acid and ethanol or glacial acetic acid and DMF and be a times of ester volume.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102435636A (en) * | 2011-09-19 | 2012-05-02 | 青岛大学 | Quick response and recovery type barium titanate nanofiber humidity dependent sensor |
| CN102650083A (en) * | 2012-05-29 | 2012-08-29 | 上海大学 | Preparation method of high length-diameter-ratio Cadmium Indium 204 (CdIn204) nano fiber material |
| CN106868633A (en) * | 2017-03-07 | 2017-06-20 | 台州职业技术学院 | A kind of strontium titanates/dioxide composite nanofiber and preparation method thereof |
| CN107436314A (en) * | 2017-07-28 | 2017-12-05 | 韦德永 | One kind is based on TiO2The moisture sensor of composite |
| CN108872327A (en) * | 2018-04-08 | 2018-11-23 | 吉林大学 | A kind of mesoporous silicon oxide/capacitive dew cell of polypyrrole composite base and preparation method thereof |
| CN112098478A (en) * | 2020-09-17 | 2020-12-18 | 昆明理工大学 | All-inorganic lead-free double perovskite humidity sensor and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101178372A (en) * | 2007-11-28 | 2008-05-14 | 吉林大学 | Electrospinning preparing quick-speed response-recovery ceramic matrix nanometer fibre dew sensor |
| CN101285791A (en) * | 2008-05-23 | 2008-10-15 | 浙江大学 | Ampere type biosensor electrode and method for making same |
| CN101550335A (en) * | 2009-05-20 | 2009-10-07 | 中国科学院长春光学精密机械与物理研究所 | Composite nanofiber luminescent material sensitive to oxygen and application thereof |
| CN101845676A (en) * | 2010-05-18 | 2010-09-29 | 北京航空航天大学 | Multifunctional composite fiber and preparation method thereof |
-
2010
- 2010-11-12 CN CN 201010540888 patent/CN102072927A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101178372A (en) * | 2007-11-28 | 2008-05-14 | 吉林大学 | Electrospinning preparing quick-speed response-recovery ceramic matrix nanometer fibre dew sensor |
| CN101285791A (en) * | 2008-05-23 | 2008-10-15 | 浙江大学 | Ampere type biosensor electrode and method for making same |
| CN101550335A (en) * | 2009-05-20 | 2009-10-07 | 中国科学院长春光学精密机械与物理研究所 | Composite nanofiber luminescent material sensitive to oxygen and application thereof |
| CN101845676A (en) * | 2010-05-18 | 2010-09-29 | 北京航空航天大学 | Multifunctional composite fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《Sensors and Actuators B: Chemical》 20100213 Yuan He, Tong Zhang, Wei Zheng, Rui Wang, Xiangwei Liu, Yan Xia Humidity sensing properties of BaTiO3 nanofiber prepared via electrospinning 98－102 1－6 第146卷, * |
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| CN102435636A (en) * | 2011-09-19 | 2012-05-02 | 青岛大学 | Quick response and recovery type barium titanate nanofiber humidity dependent sensor |
| CN102650083A (en) * | 2012-05-29 | 2012-08-29 | 上海大学 | Preparation method of high length-diameter-ratio Cadmium Indium 204 (CdIn204) nano fiber material |
| CN106868633A (en) * | 2017-03-07 | 2017-06-20 | 台州职业技术学院 | A kind of strontium titanates/dioxide composite nanofiber and preparation method thereof |
| CN106868633B (en) * | 2017-03-07 | 2019-07-09 | 台州职业技术学院 | A kind of strontium titanates/dioxide composite nanofiber and preparation method thereof |
| CN107436314A (en) * | 2017-07-28 | 2017-12-05 | 韦德永 | One kind is based on TiO2The moisture sensor of composite |
| CN108872327A (en) * | 2018-04-08 | 2018-11-23 | 吉林大学 | A kind of mesoporous silicon oxide/capacitive dew cell of polypyrrole composite base and preparation method thereof |
| CN112098478A (en) * | 2020-09-17 | 2020-12-18 | 昆明理工大学 | All-inorganic lead-free double perovskite humidity sensor and preparation method thereof |
| CN112098478B (en) * | 2020-09-17 | 2021-07-20 | 昆明理工大学 | All-inorganic lead-free double perovskite humidity sensor and preparation method thereof |
| CN112485298A (en) * | 2020-11-06 | 2021-03-12 | 电子科技大学 | Manufacturing method of polyvinylidene fluoride-based flexible humidity sensor |
| CN113804731A (en) * | 2021-09-18 | 2021-12-17 | 宁波磁性材料应用技术创新中心有限公司 | Resistance type humidity-sensitive material, preparation method thereof and resistance type humidity sensor |
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Application publication date: 20110525 |