CN101788520A - Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof - Google Patents
Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof Download PDFInfo
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- CN101788520A CN101788520A CN 201010125466 CN201010125466A CN101788520A CN 101788520 A CN101788520 A CN 101788520A CN 201010125466 CN201010125466 CN 201010125466 CN 201010125466 A CN201010125466 A CN 201010125466A CN 101788520 A CN101788520 A CN 101788520A
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Abstract
The invention discloses a polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon, which is characterized in that a humidity sensitive thin film is deposited on the surface of a surface acoustic wave resonance component using an ST-cut quartz crystal as a substrate material, the humidity sensitive thin film is 3-aminopropyl triethoxy silicon mono bromo n-hexane quaternary ammonium salt electrolyte thin film. The 3-aminopropyl triethoxy silicon mono bromo n-hexane quaternary ammonium salt is deposited by an electrostatic spraying method, and then is heated to condense and polymerize to form the polyelectrolyte humidity sensitive film containing silicon, which has a crosslink structure. The invention has simple preparation process and low cost. Uniform sensitive film with controllable deposition can be realized by the electrostatic spraying method, and the stability of the humidity sensitive element is obviously improved by the pyrocondensation polymerization; the manufactured humidity sensitive element is within the wide humidity range (11-95%RH), and has the advantages of high humidity sensitivity (400Hz/%RH), rapid response, good recoverability, good stability and the like. The invention can be widely used for the production process of agriculture and industry and storage, and can be used for monitoring the atmospheric environment, precisely measuring and controlling the environment humidity.
Description
Technical field
The present invention relates to a kind of siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element 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.The polymkeric substance humidity-sensitive element is mostly based on resistance-capacitance type at present, they can be fine compatible with present integrated circuit technique, be easy to realize in the integrated system moisture measurement and control, now become one of important directions of humidity sensor development, but there is also the too high mensuration that is difficult to of impedance under low humidity, high humidity environment is the not ideal enough deficiency that waits of stability down.The sonic surface wave type humidity-sensitive element, has the response sensitivity height, the Humidity Detection wide ranges is particularly suited for detecting low wet environment, size and is easy to integrated, response signal digitizing for a short time and is easy to realize advantages such as remote-wireless transmission, and wide application and bright development prospect are arranged.But the surface acoustic wave humidity photosensitive elements research that with the macromolecule is sensitive material at present is still rarely found, and this respect is well worth doing.
Summary of the invention
The purpose of this invention is to provide a kind of wet-sensitive sensitivity height, response is fast, siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that recovery is good and preparation method thereof.
Siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element of the present invention, be to be that the standby quartz crystal of SAW (Surface Acoustic Wave) resonator part of base material is that the SAW (Surface Acoustic Wave) resonator part surface deposition of base material has humidity sensitive thin film cut quartz crystal with ST, this humidity sensitive thin film is a 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt polyelectrolyte membrane.
Prepare the method for siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element, may further comprise the steps:
1) selects that to cut quartz crystal with ST be that the SAW (Surface Acoustic Wave) resonator part of base material is standby;
2) with 3～4: 2～3: 1～2 mixing by volume of 3-aminopropyl triethoxysilane, bromo normal hexane and absolute ethyl alcohol, mixed liquor reacted 24 hours under 40～50 ℃ of argon shields, be warming up to 60～70 ℃ then, the dropping volume is that the pH value of 0.6～0.8 times of absolute ethyl alcohol is 1 aqueous hydrochloric acid solution, continue reaction 1～2 hour, use ether sedimentation, filtration then, dry at normal temperatures, obtain 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt;
3) 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is joined in the absolute ethyl alcohol, stir at normal temperatures, being configured to concentration is the electrostatic spraying solution of 5～50 mg/ml;
4) electrostatic spraying solution is contained in the syringe of band syringe needle, the anode of injection needle and power supply links to each other, and the negative electrode of power supply links to each other with copper coin, places the SAW (Surface Acoustic Wave) resonator part of step 1) on the copper coin; Between syringe needle and copper coin, apply 5～25kV voltage, the distance of syringe needle and surface acoustic wave resonance type device surface is 5～20cm, the EFI time is 10～60 minutes, the flow velocity of solution is 0.1～0.2 milliliter/hour, environment temperature is 20～35 ℃, ambient humidity is 25～45%RH, and electrostatic spraying forms 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt film in surface acoustic wave resonance type device surface deposition;
5) the surface acoustic wave resonance type device that has 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt film that step 4) is made was 80～110 ℃ of heating 8～16 hours, make 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt generation thermal condensation polyreaction, the siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that obtains having cross-linked structure.
Advantage of the present invention is:
1) used electrode is the surface acoustic wave resonance type humidity-sensitive element, compare with traditional resistor-type, capacitor type humidity-sensitive element, element has very high response sensitivity, very wide Humidity Detection scope, is particularly suited for measuring low wet environment, and size is little, is easy to realize advantages such as wireless and long-distance transmissions;
2) to cut quartz crystal with ST be base material for prepared surface acoustic wave resonance type humidity-sensitive element, and it has zero-temperature coefficient, can reduce the influence of temperature variation for the wet quick response of element effectively;
3) siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element adopts the method preparation of electrostatic spraying, and is simple to operate, and efficiently solves the problem that realizes controlled film forming at small size, irregular electrode surface;
4) prepared siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element with by 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt condensation polymerization siliceous polyelectrolyte as humidity-sensitive material, itself and water function are stronger, have high wet-sensitive sensitivity in the humidity range of broad;
5) to utilize electrostatic spray to prepare siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element process simple in the present invention, can be neatly by changing technological parameter (distance of the offset voltage of electrostatic sprayer, syringe needle and receiver sheet, the flow velocity of solution and spray time), preparation has the homogeneous humidity sensitive thin film of different-thickness, realizes that high sensitivity responds fast;
6) siliceous polyelectrolyte membrane has cross-linked structure, and combines closely with substrate, can effectively improve the stability and the water tolerance of humidity-sensitive element;
7) to have a volume little for humidity-sensitive element of the present invention, low cost, advantage such as easy to use.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 scanning electron microscope picture of the sensitive thin film of surface acoustic wave resonance type humidity-sensitive element;
Fig. 2 is the wet quick resonse characteristic of siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element;
Fig. 3 is the response time curve of siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element;
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
Siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element of the present invention, be at the SAW (Surface Acoustic Wave) resonator part surface deposition that is base material humidity sensitive thin film to be arranged with the quartz crystal, this humidity sensitive thin film is a 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt polyelectrolyte membrane.
Embodiment 1:
1) selects that to cut quartz crystal with ST be that the SAW (Surface Acoustic Wave) resonator part of base material is standby;
2) in 50 milliliters of there-necked flasks, add 17.64 milliliters of 3-aminopropyl triethoxysilanes successively, 10.52 milliliters of bromo normal hexanes and 5 milliliters of absolute ethyl alcohols.Mixed liquor reacted 24 hours under 45 ℃ of argon shields, was warming up to 60 ℃ then, dripped 4.05 milliliters of pH values and be 1 aqueous hydrochloric acid solution, continued reaction and stopped in 1 hour.Reactant liquor dilutes with 15 milliliters of absolute ethyl alcohols, precipitates in 500 milliliters of ether, filters then, and vacuum drying at normal temperatures 24 hours obtains flaxen 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt (APTS-BH) at last;
3) APTS-BH is joined in the absolute ethyl alcohol, normal temperature stirred 5 hours down, and being configured to concentration is the electrostatic spraying solution of 25 mg/ml;
4) electrostatic spraying solution is contained in the syringe of band syringe needle, the anode of injection needle and power supply links to each other, and the negative electrode of power supply links to each other with copper coin, places the surface acoustic wave resonance type device of step 1) on the copper coin; Between syringe needle and copper coin, apply 10kV voltage, between syringe needle and the surface acoustic wave resonance type device upper surface apart from 5cm, 20 minutes EFI time, the flow velocity of solution is 0.1 milliliter/hour, environment temperature is 20～35 ℃, ambient humidity is 25～45%RH, and electrostatic spraying forms the APTS-BH film in surface acoustic wave resonance type device surface deposition;
5) the surface acoustic wave resonance type device that has the APTS-BH film with the step 4) preparation heated 10 hours at 100 ℃, made APTS-BH that thermal condensation polyreaction, the siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that obtains having cross-linked structure take place.
Embodiment 2:
1) selects that to cut quartz crystal with ST be that the SAW (Surface Acoustic Wave) resonator part of base material is standby;
2) in 50 milliliters of there-necked flasks, add 19 milliliters of 3-aminopropyl triethoxysilanes successively, 12 milliliters of bromo normal hexanes and 6 milliliters of absolute ethyl alcohols.Mixed liquor reacted 24 hours under 50 ℃ of argon shields, was warming up to 70 ℃ then, and Dropwise 5 milliliter pH value is 1 aqueous hydrochloric acid solution, continued reaction and stopped in 1 hour.Reactant liquor dilutes with 15 milliliters of absolute ethyl alcohols, precipitates in 500 milliliters of ether, filters then, and vacuum drying at normal temperatures 24 hours obtains flaxen 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt (APTS-BH) at last;
3) APTS-BH is joined in the absolute ethyl alcohol, normal temperature stirred 5 hours down, and being configured to concentration is the electrostatic spraying solution of 35 mg/ml;
4) electrostatic spraying solution is contained in the syringe of band syringe needle, the anode of injection needle and power supply links to each other, and the negative electrode of power supply links to each other with copper coin, places the surface acoustic wave resonance type device of step 1) on the copper coin; Between syringe needle and copper coin, apply 10kV voltage, between syringe needle and the surface acoustic wave resonance type device upper surface apart from 5cm, 15 minutes EFI time, the flow velocity of solution is 0.1 milliliter/hour, environment temperature is 20～35 ℃, ambient humidity is 25～45%RH, and electrostatic spraying forms the APTS-BH film in surface acoustic wave resonance type device surface deposition;
5) the surface acoustic wave resonance type device that has the APTS-BH film with the step 4) preparation heated 10 hours at 100 ℃, made APTS-BH that thermal condensation polyreaction, the siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that obtains having cross-linked structure take place.
Embodiment 3:
1) selects that to cut quartz crystal with ST be that the SAW (Surface Acoustic Wave) resonator part of base material is standby;
2) in 50 milliliters of there-necked flasks, add 35 milliliters of 3-aminopropyl triethoxysilanes successively, 21 milliliters of bromo normal hexanes and 10 milliliters of absolute ethyl alcohols.Mixed liquor reacted 24 hours under 45 ℃ of argon shields, was warming up to 65 ℃ then, dripped 8 milliliters of pH values and be 1 aqueous hydrochloric acid solution, continued reaction and stopped in 1 hour.Reactant liquor dilutes with 30 milliliters of absolute ethyl alcohols, precipitates in 1000 milliliters of ether, filters then, and vacuum drying at normal temperatures 24 hours obtains flaxen 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt (APTS-BH) at last;
3) APTS-BH is joined in the absolute ethyl alcohol, normal temperature stirred 5 hours down, and being configured to concentration is the electrostatic spraying solution of 25 mg/ml;
4) electrostatic spraying solution is contained in the syringe of band syringe needle, the anode of injection needle and power supply links to each other, and the negative electrode of power supply links to each other with copper coin, places the surface acoustic wave resonance type device of step 1) on the copper coin; Between syringe needle and copper coin, apply 15kV voltage, between syringe needle and the surface acoustic wave resonance type device upper surface apart from 5cm, 30 minutes EFI time, the flow velocity of solution is 0.1 milliliter/hour, environment temperature is 20～35 ℃, ambient humidity is 25～45%RH, and electrostatic spraying forms the APTS-BH film in surface acoustic wave resonance type device surface deposition;
5) the surface acoustic wave resonance type device that has the APTS-BH film with the step 4) preparation heated 10 hours at 100 ℃, made APTS-BH that thermal condensation polyreaction, the siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that obtains having cross-linked structure take place.
Figure 1 shows that the scanning electron microscope picture of surface acoustic wave resonance type humidity-sensitive element surface-sensitive material film, as seen from the figure, it is smooth that EFI is coated with the film surface smoother that makes;
As seen from Figure 2, the surface acoustic wave resonance type humidity-sensitive element is almost all having wet quick response in the full humidity range, also has more significantly at low wet zone especially to respond, and increases than the sensing range of conventional wet dependent sensor.Simultaneously, this sensor has higher sensitivity, the about 400Hz/%RH of output signal variable quantity;
Figure 3 shows that the response time curve of siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element, by the figure finding, the moisture absorption of element, dehumidification all show response speed faster, and the time that reaches stable state is all less than 10s, and have and respond reversibility preferably.
Claims (2)
1. siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element, it is characterized in that: it is to be that the SAW (Surface Acoustic Wave) resonator part surface deposition of base material has humidity sensitive thin film cut quartz crystal with ST, and this humidity sensitive thin film is a 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt polyelectrolyte membrane.
2. prepare the method for the described siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element of claim 1, may further comprise the steps:
1) selects that to cut quartz crystal with ST be that the SAW (Surface Acoustic Wave) resonator part of base material is standby;
2) with 3～4: 2～3: 1～2 mixing by volume of 3-aminopropyl triethoxysilane, bromo normal hexane and absolute ethyl alcohol, mixed liquor reacted 24 hours under 40～50 ℃ of argon shields, be warming up to 60～70 ℃ then, the dropping volume is that the pH value of 0.6～0.8 times of absolute ethyl alcohol is 1 aqueous hydrochloric acid solution, continue reaction 1～2 hour, use ether sedimentation, filtration then, dry at normal temperatures, obtain 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt;
3) 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt is joined in the absolute ethyl alcohol, stir at normal temperatures, being configured to concentration is the electrostatic spraying solution of 5～50 mg/ml;
4) electrostatic spraying solution is contained in the syringe of band syringe needle, the anode of injection needle and power supply links to each other, and the negative electrode of power supply links to each other with copper coin, places the SAW (Surface Acoustic Wave) resonator part of step 1) on the copper coin; Between syringe needle and copper coin, apply 5～25kV voltage, the distance of syringe needle and surface acoustic wave resonance type device surface is 5～20cm, the EFI time is 10～60 minutes, the flow velocity of solution is 0.1～0.2 milliliter/hour, environment temperature is 20～35 ℃, ambient humidity is 25～45%RH, and electrostatic spraying forms 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt film in surface acoustic wave resonance type device surface deposition;
5) the surface acoustic wave resonance type device that has 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt film that step 4) is made was 80～110 ℃ of heating 8～16 hours, make 3-aminopropyl-triethoxy silicon list bromo normal hexane quaternary ammonium salt generation thermal condensation polyreaction, the siliceous polyelectrolyte surface acoustic wave resonance type humidity-sensitive element that obtains having cross-linked structure.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102565146A (en) * | 2011-12-27 | 2012-07-11 | 郑州炜盛电子科技有限公司 | Resistance type humidity element and preparation method thereof |
| CN110411925A (en) * | 2019-07-26 | 2019-11-05 | 中节能天融科技有限公司 | A kind of superfine particulate matter measuring system and method based on surface acoustic wave techniques |
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| US6831340B2 (en) * | 2001-10-17 | 2004-12-14 | Murata Manufacturing Co., Ltd. | Surface acoustic wave device and method of producing the same |
| US20060131993A1 (en) * | 2004-12-21 | 2006-06-22 | Seiko Epson Corporation | Surface acoustic wave device and method of manufacturing a surface acoustic wave device |
| CN101135670A (en) * | 2007-10-12 | 2008-03-05 | 电子科技大学 | Two-channel sonic surface wave gas sensors having humidity compensate function |
| CN101324539A (en) * | 2008-07-22 | 2008-12-17 | 浙江大学 | Polymer compound resistor type humidity sensitive element with nanometer fiber structure and manufacturing method thereof |
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2010
- 2010-03-16 CN CN 201010125466 patent/CN101788520A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6831340B2 (en) * | 2001-10-17 | 2004-12-14 | Murata Manufacturing Co., Ltd. | Surface acoustic wave device and method of producing the same |
| US20060131993A1 (en) * | 2004-12-21 | 2006-06-22 | Seiko Epson Corporation | Surface acoustic wave device and method of manufacturing a surface acoustic wave device |
| CN101135670A (en) * | 2007-10-12 | 2008-03-05 | 电子科技大学 | Two-channel sonic surface wave gas sensors having humidity compensate function |
| CN101324539A (en) * | 2008-07-22 | 2008-12-17 | 浙江大学 | Polymer compound resistor type humidity sensitive element with nanometer fiber structure and manufacturing method thereof |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102565146A (en) * | 2011-12-27 | 2012-07-11 | 郑州炜盛电子科技有限公司 | Resistance type humidity element and preparation method thereof |
| CN102565146B (en) * | 2011-12-27 | 2014-06-04 | 郑州炜盛电子科技有限公司 | Resistance type humidity element and preparation method thereof |
| CN110411925A (en) * | 2019-07-26 | 2019-11-05 | 中节能天融科技有限公司 | A kind of superfine particulate matter measuring system and method based on surface acoustic wave techniques |
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Application publication date: 20100728 |