CN102854222A - Moisture-sensitive sensor based on potassium tantalite sensitive membrane and preparation method thereof - Google Patents
Moisture-sensitive sensor based on potassium tantalite sensitive membrane and preparation method thereof Download PDFInfo
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- CN102854222A CN102854222A CN2012103665633A CN201210366563A CN102854222A CN 102854222 A CN102854222 A CN 102854222A CN 2012103665633 A CN2012103665633 A CN 2012103665633A CN 201210366563 A CN201210366563 A CN 201210366563A CN 102854222 A CN102854222 A CN 102854222A
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Abstract
The invention belongs to the technical field of a moisture sensitive device, and in particular relates to a moisture-sensitive sensor based on a potassium tantalite sensitive membrane and a preparation method thereof. The sensor consists of a ceramic substrate, a gold (Au) metal interdigital electrode and a potassium tantalite sensitive membrane, wherein the Au metal interdigital electrode is prepared on the ceramic substrate by adopting a silk screen printing method, the potassium tantalite sensitive membrane is prepared on the Au metal interdigital electrode by adopting a coating method, the thickness of the potassium tantalite sensitive membrane is 2 to 4 micrometers, and both the width and the interval space of the metal interdigital electrode is 0.15 to 0.20mm. The preparation method comprises following steps of firstly adopting the silk screen printing method to prepare the Au metal interdigital electrode on the ceramic substrate, adopting a hydrothermal method to prepare a potassium tantalite sensitive material, adopting a coating method to coat the potassium tantalite sensitive material onto the metal interdigital electrode to prepare a moisture-sensitive element. The potassium tantalite moisture-sensitive sensor is simple in preparation process, small in size, applicable to mass production, high in sensitivity to the moisture, small in hysteresis, fast in responding time and vast in application value on the aspect of the moisture sensitive detection aspect.
Description
Technical field
The invention belongs to the wet sensitive device technical field, be specifically related to a kind of moisture sensor take potassium tantalate as sensitive membrane and preparation method thereof.
Background technology
Humidity has close relationship to people's life, commercial production, scientific research, national defense construction and vegeto-animal growth.In the mankind's life, if air is too moist, can make the people feel dull, if air is too dry, Person's skin is done not feel like oneself, so will use instrument that humidity is detected control in the room; In commercial production, the control of humidity is directly connected to the quality of product; Aspect national defence, the storage of space missile, military equipment all be unable to do without the control of humidity, so military depot is essential to the detection of humidity; In addition, storage of the mildew-resistant of grain, aerological sounding, chamber planting, birds, beasts and eggs etc. also all be unable to do without Humidity Detection.
Humidity sensor is to be beneficial to the humidity sensitive material directly to adsorb hydrone in the atmosphere, so that the electrical properties of material etc. change, changes and measures humidity and change through detecting the output signal that connects the peripheral circuit sensitive element.Therefore humidity sensor becomes one of study hotspot in recent years.
The material that is used for humidity sensor has a lot, mainly concentrates at present semiconductor, in the materials such as pottery and macromolecule.In recent years, because good stability, perovskite material was used to the development of wet sensitive device gradually.A kind of as perovskite material, the physicochemical property of potassium tantalate are stable, and are widely used in photocatalysis brine electrolysis aspect, therefore, it can be applied in wet sensitive sensing aspect.At present, the wet sensitive performance study for potassium tantalate rarely has report.
Summary of the invention
The purpose of this invention is to provide a kind of moisture sensor based on potassium tantalate and preparation method.
Adopt the potassium tantalate material as sensitive material, not only used the advantage of perovskite material, can also effectively utilize potassium tantalate to the advantage of humidity sensitive.The technique that simultaneously the present invention adopts is simple, device volume is little, be suitable for production in enormous quantities, thereby has important using value.
The humidity sensor of potassium tantalate of the present invention, formed in the Au metal interdigital electrode on the ceramic substrate, the potassium tantalate sensitive membrane of employing cladding process preparation on Au metal interdigital electrode by ceramic substrate, the preparation of employing silk screen print method, wherein the thickness of potassium tantalate sensitive membrane is 2～4 μ m, and width and the spacing of metal interdigital electrode are 0.15～0.20mm.
The preparation method of the moisture sensor based on the potassium tantalate sensitive membrane of the present invention, its step is as follows:
1) processing of ceramic substrate
Wipe ceramic substrate to clean with acetone, ethanol cotton balls at first respectively, again ceramic substrate is placed acetone, ethanol and deionized water successively, ultrasonic cleaning is 5～10 minutes respectively, final drying;
2) preparation of metal interdigital electrode
Adopt screen printing technique to prepare Au metal interdigital electrode, according to printing ink: the Au powder: the mass ratio of thinning agent is 1:1.5:3, stirs to be modulated into paste; Then paste is infused on the silk-screen plate with the interdigital electrode pattern, scrapes paste with certain angle of inclination and pressure, then printed electrode and oven dry adopt ultraviolet light polymerization, prepare the metal interdigital electrode; Width and the electrode separation of metal interdigital electrode are 0.15～0.20mm.
3) preparation of nanometer potassium tantalate
Adopt hydro-thermal method to prepare the nanometer potassium tantalate: under the room temperature condition, 4.0～5.0g potassium hydroxide is dissolved in 8～12mL water, solution stirs to clarify, and then adds 0.03～0.05g tantalum pentoxide, continues to stir to obtain homogeneous solution; Again this solution is transferred in the reactor, is heated to 60～200 ℃, kept 12～16 hours, thereby obtain the potassium tantalate sample of white; This sample is washed till neutrality with deionized water, and then dry, the potassium tantalate that obtains being of a size of 150～300nm is nanocrystalline; As shown in Figure 1;
4) dried potassium tantalate is put into mortar, grind; Then in mortar, splash into deionized water, continue again to grind, deionized water is fully mixed with potassium tantalate, obtain the slurry of sticky shape; Pick a small amount of slurry with spoon, be coated on the interdigital electrode, then with it 60～80 ℃ of oven dry, thereby the thickness that obtains sensitive membrane is the element of 2～4 μ m; It is the environment of 100%RH that the above element that makes is placed relative humidity, and the alternating current that applies 1V, 100Hz in interdigital electrode is aging, thereby obtains take potassium tantalate as sensitive membrane, take the moisture sensor of Au as the metal interdigital electrode.
Further, step 2) printing ink described in is good magnificent JX07500487, and thinning agent is that ethanol and the ethyl acetate of mass ratio 1.5:1 mixes; The time of the ultraviolet light polymerization step 2) is 400s; Step 2) angle of inclination described in is 30 degree, and pressure is 5 Ns.Step 1) and step 3) are dry under 100 ℃ of environment.Digestion time described in the step 4) is 24 hours.Milling time described in the step 4) is 30 minutes.
It is simple, with low cost that the potassium tantalate moisture sensor of the present invention's preparation has the preparation method, is expected to the characteristics of large-scale production, and humidity is had good detection performance.
Description of drawings
Fig. 1: the shape appearance figure of potassium tantalate;
Fig. 2: the structural representation that the prepared device of the present invention is corresponding;
Under Fig. 3: 1V, the 100Hz alternating current, the impedance of device of the present invention-relative humidity family curve (thickness 2 μ m);
Under Fig. 4: 1V, the 100Hz alternating current, the impedance of device of the present invention-relative humidity family curve (thickness 3 μ m);
Under Fig. 5: 1V, the 100Hz alternating current, the impedance of device of the present invention-relative humidity family curve (thickness 4 μ m);
Under Fig. 6: 1V, the 100Hz alternating current, the behavior of hysteresis curve of device of the present invention (thickness 3 μ m);
Under Fig. 7: 1V, the 100Hz alternating current, device of the present invention is at the response recovery curve (thickness 3 μ m) of 11～95%RH;
As shown in Figure 1, the grain size of nanometer potassium tantalate is 150～300nm.
As shown in Figure 2, device is comprised of stupalith substrate 1, Au metal interdigital electrode 2, potassium tantalate sensitive membrane 3.
As shown in Figure 3, when device under 1V, 100Hz alternating current, the resistance value of device is larger with moisture curve, crosses over about 3 orders of magnitude, curve is not obvious in the humidity range linear relationship.
As shown in Figure 4, when device under 1V, 100Hz alternating current, the resistance value of device is larger with moisture curve, crosses over about 3 orders of magnitude, curve presents certain linear relationship at humidity range.
As shown in Figure 5, when device under 1V, 100Hz alternating current, the resistance value of device is larger with moisture curve, crosses over about 3 orders of magnitude, curve is not obvious in high humidity partial linear relation.
As shown in Figure 6, the humidity hysteresis of device is less than 1%RH.
As shown in Figure 7, the response time from 11%RH to 95%RH of device is 2s, and the release time of device from 95%RH to 11%RH is 30s.Humidity there is good detection.
Embodiment
Embodiment 1:
Wipe ceramic substrate to clean with acetone, ethanol cotton balls at first respectively, again substrate is placed acetone, ethanol and deionized water successively, ultrasonic cleaning is 5 minutes respectively, is put at last drying for standby in 100 ℃;
Adopt screen printing technique to prepare Au metal interdigital electrode, according to printing ink (good magnificent JX07500487): the Au powder: (mass ratio is ethanol: the mass ratio of ethyl acetate=1.5:1) is 1:1.5:3 to thinning agent, stirs and is modulated into paste; Then paste is infused on the silk-screen plate with the interdigital electrode pattern, scrapes paste take the angle of inclination as 30 degree and 5 Ns pressure, then printed electrode and oven dry adopt ultraviolet light polymerization 400s, prepare the metal interdigital electrode.
Adopt hydro-thermal method to prepare potassium tantalate: under the room temperature condition, 4g potassium hydroxide is dissolved in the 10mL water, solution stirs to clarify, and then adds the 0.0442g tantalum pentoxide, continues to stir to obtain homogeneous solution.This reactant transfer in reactor, is heated 180 ℃, kept 12 hours.Obtain the potassium tantalate sample of white.This sample is washed till neutrality with deionized water, is put in 100 ℃ after the drying, stand-by.
Dried potassium tantalate is put into mortar, grind 30min; Then splash into deionized water in mortar, continue to grind 30min again, deionized water is fully mixed with potassium tantalate, the slurry that is sticky shape gets final product.Pick a small amount of sensitive membrane slurry with spoon, be coated on the substrate, applying number of times is 1 time, and then 60 ℃ of oven dry, the thickness that namely obtains sensitive membrane is the element of 2 μ m.It is the environment of 100%RH that the above element that makes is placed relative humidity, applies the alternating current of 1V, 100Hz in interdigital electrode, aging 24 hours, obtains take potassium tantalate as sensitive membrane, take the moisture sensor of Au as the metal interdigital electrode.
Prepare after the device, its wet sensitive characteristic is tested.By shown in Figure 3, under 100Hz, 1V alternating current, the resistance value of device is larger with moisture curve, crosses over 3 orders of magnitude.When humidity range was 11%RH～95%RH, curve had some linear, but not obvious.
Embodiment 2:
Wipe substrate to clean with acetone, ethanol cotton balls at first respectively, again substrate is placed acetone, ethanol and deionized water successively, ultrasonic cleaning is 5 minutes respectively, is put at last drying for standby in 100 ℃;
The preparation process of Au metal interdigital electrode is with embodiment 1.
Adopt hydro-thermal method to prepare potassium tantalate: experimentation is with embodiment 1.
Dried potassium tantalate is put into mortar, grind 30min; Then splash into deionized water in mortar, continue to grind 30min again, deionized water is mixed fully with material, the slurry that is sticky shape gets final product.Pick a small amount of sensitive membrane slurry with spoon, be coated on the substrate, applying number of times is 2 times, and then 60 ℃ of oven dry, the thickness that namely obtains sensitive membrane is the element of 3 μ m.It is the humidity source of 100%RH that the above element that makes is placed relative humidity, applies the alternating current of 1V, 100Hz in interdigital electrode, aging 24 hours, obtains take potassium tantalate as sensitive membrane, take the moisture sensor of Au as the metal interdigital electrode.
Prepare after the device, its wet sensitive characteristic is tested.By shown in Figure 4, under 100Hz, 1V alternating current, the resistance value of device is larger with moisture curve, crosses over 3 orders of magnitude.When humidity range was 11%RH～95%RH, curve presented certain linear relationship at humidity range.By shown in Figure 6, the behavior of hysteresis of device is less than 1%RH.By shown in Figure 7, the response time from 11%RH to 95%RH of device is 2s, and the release time of device from 95%RH to 11%RH is 30s.Humidity there is good detection.
Embodiment 3:
Wipe substrate to clean with acetone, ethanol cotton balls at first respectively, again substrate is placed acetone, ethanol and deionized water successively, ultrasonic cleaning is 5 minutes respectively, is put at last drying for standby in 100 ℃;
The preparation process of Au metal interdigital electrode is with embodiment 1.
Adopt hydro-thermal method to prepare potassium tantalate: experimentation is with embodiment 1.
Dried potassium tantalate is put into mortar, grind 30min; Then splash into deionized water in mortar, continue to grind 30min again, deionized water is mixed fully with material, the slurry that is sticky shape gets final product.Pick a small amount of sensitive membrane slurry with spoon, be coated on the substrate, applying number of times is 3 times, and then 60 ℃ of oven dry, the thickness that namely obtains sensitive membrane is the element of 4 μ m.It is the humidity source of 100%RH that the above element that makes is placed relative humidity, applies the alternating current of 1V, 100Hz in interdigital electrode, aging 24 hours, obtains take potassium tantalate as sensitive membrane, take the moisture sensor of Au as the metal interdigital electrode.
Prepare after the device, its wet sensitive characteristic is tested.By shown in Figure 5, under 100Hz, 1V alternating current, the resistance value of device is larger with moisture curve, crosses over 3 orders of magnitude.When humidity range was 11%RH～95%RH, curve partly had some linear at high humidity, but not obvious.
Claims (9)
1. moisture sensor based on the potassium tantalate sensitive membrane, it is characterized in that: formed in the Au metal interdigital electrode on the ceramic substrate, the nanometer potassium tantalate sensitive membrane of preparation on Au metal interdigital electrode by ceramic substrate, preparation, wherein the thickness of potassium tantalate sensitive membrane is 2～4 μ m, and width and the spacing of metal interdigital electrode are 0.15～0.20mm.
2. a kind of moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 1, it is characterized in that: the grain size of nanometer potassium tantalate is 150～300nm.
3. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane claimed in claim 1, its step is as follows:
1) processing of ceramic substrate
Wipe ceramic substrate to clean with acetone, ethanol cotton balls at first respectively, again ceramic substrate is placed acetone, ethanol and deionized water successively, ultrasonic cleaning is 5～10 minutes respectively, final drying;
2) preparation of metal interdigital electrode
Adopt screen printing technique to prepare Au metal interdigital electrode, according to printing ink: the Au powder: the mass ratio of thinning agent is 1:1.5:3, stirs to be modulated into paste; Then paste is infused on the silk-screen plate with the interdigital electrode pattern, scrapes paste with certain angle of inclination and pressure, then printed electrode and oven dry adopt ultraviolet light polymerization, prepare the metal interdigital electrode; Width and the electrode separation of metal interdigital electrode are 0.15～0.20mm.
3) preparation of nanometer potassium tantalate
Adopt hydro-thermal method to prepare the nanometer potassium tantalate: under the room temperature condition, 4.0～5.0g potassium hydroxide is dissolved in 8～12mL water, solution stirs to clarify, and then adds 0.03～0.05g tantalum pentoxide, continues to stir to obtain homogeneous solution; Again this solution is transferred in the reactor, is heated to 60～200 ℃, kept 12～16 hours, thereby obtain the potassium tantalate sample of white; This sample is washed till neutrality with deionized water, and then dry, the potassium tantalate that obtains being of a size of 150～300nm is nanocrystalline;
4) dried potassium tantalate is put into mortar, grind; Then in mortar, splash into deionized water, continue again to grind, deionized water is fully mixed with potassium tantalate, obtain the slurry of sticky shape; Pick a small amount of slurry with spoon, be coated on the interdigital electrode, then with it 60～80 ℃ of oven dry, thereby the thickness that obtains sensitive membrane is the element of 2～4 μ m; It is the environment of 100%RH that the above element that makes is placed relative humidity, and the alternating current that applies 1V, 100Hz in interdigital electrode is aging, thus obtain take potassium tantalate as sensitive membrane moisture sensor.
4. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3 is characterized in that: step 2) described in printing ink be good magnificent JX07500487, thinning agent is that ethanol and the ethyl acetate of mass ratio 1.5:1 mixes.
5. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3 is characterized in that: step 2) described in time of ultraviolet light polymerization be 400s.
6. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3 is characterized in that: step 2) described in the angle of inclination be 30 degree, pressure is 5 Ns.
7. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3, it is characterized in that: step 1) and step 3) are dry under 100 ℃ of environment.
8. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3, it is characterized in that: the digestion time described in the step 4) is 24 hours.
9. the preparation method of the moisture sensor based on the potassium tantalate sensitive membrane as claimed in claim 3, it is characterized in that: the milling time described in the step 4) is 30 minutes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103439368A (en) * | 2013-09-16 | 2013-12-11 | 吉林大学 | Phosphate molecular sieve based humidity sensor and preparation method thereof |
| CN104714160A (en) * | 2015-03-27 | 2015-06-17 | 江苏峰工电气科技有限公司 | Multifunctional sensor and application of multifunctional sensor in aspect of GIS discharge and micro-water content detection |
| CN104937404A (en) * | 2013-01-17 | 2015-09-23 | 田中贵金属工业株式会社 | Biosensor and process for producing same |
| CN105044162A (en) * | 2015-08-21 | 2015-11-11 | 吉林大学 | Macromolecule-based resistance type humidity sensing element and preparation method thereof |
| CN108302376A (en) * | 2017-12-25 | 2018-07-20 | 潘荣兰 | Has the LED street lamp of colour temperature handoff functionality |
| CN111317476A (en) * | 2020-03-03 | 2020-06-23 | 重庆大学 | Sleep apnea syndrome detection device based on respiratory airflow signal |
| CN112611787A (en) * | 2020-12-15 | 2021-04-06 | 无锡豪帮高科股份有限公司 | High-molecular resistance type humidity sensitive element and preparation method thereof |
| WO2021187412A1 (en) * | 2020-03-19 | 2021-09-23 | 株式会社ニコン | Method for producing potassium tantalate particles, method for producing film, potassium tantalate particles, film, antireflective film, optical element, and optical apparatus |
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Cited By (10)
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|---|---|---|---|---|
| CN104937404A (en) * | 2013-01-17 | 2015-09-23 | 田中贵金属工业株式会社 | Biosensor and process for producing same |
| CN103439368A (en) * | 2013-09-16 | 2013-12-11 | 吉林大学 | Phosphate molecular sieve based humidity sensor and preparation method thereof |
| CN103439368B (en) * | 2013-09-16 | 2016-04-06 | 吉林大学 | A kind of humidity sensor based on phosphate molecule sieve and preparation method thereof |
| CN104714160A (en) * | 2015-03-27 | 2015-06-17 | 江苏峰工电气科技有限公司 | Multifunctional sensor and application of multifunctional sensor in aspect of GIS discharge and micro-water content detection |
| CN105044162A (en) * | 2015-08-21 | 2015-11-11 | 吉林大学 | Macromolecule-based resistance type humidity sensing element and preparation method thereof |
| CN105044162B (en) * | 2015-08-21 | 2017-08-22 | 吉林大学 | A kind of polymer-based electric resistance type humidity sensitive element and preparation method thereof |
| CN108302376A (en) * | 2017-12-25 | 2018-07-20 | 潘荣兰 | Has the LED street lamp of colour temperature handoff functionality |
| CN111317476A (en) * | 2020-03-03 | 2020-06-23 | 重庆大学 | Sleep apnea syndrome detection device based on respiratory airflow signal |
| WO2021187412A1 (en) * | 2020-03-19 | 2021-09-23 | 株式会社ニコン | Method for producing potassium tantalate particles, method for producing film, potassium tantalate particles, film, antireflective film, optical element, and optical apparatus |
| CN112611787A (en) * | 2020-12-15 | 2021-04-06 | 无锡豪帮高科股份有限公司 | High-molecular resistance type humidity sensitive element and preparation method thereof |
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