CN102937621A - Passive high-molecular polymer matrix humidity sensor and preparation and detection methods thereof - Google Patents
Passive high-molecular polymer matrix humidity sensor and preparation and detection methods thereof Download PDFInfo
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- CN102937621A CN102937621A CN2012104341129A CN201210434112A CN102937621A CN 102937621 A CN102937621 A CN 102937621A CN 2012104341129 A CN2012104341129 A CN 2012104341129A CN 201210434112 A CN201210434112 A CN 201210434112A CN 102937621 A CN102937621 A CN 102937621A
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Abstract
The invention discloses a passive high-molecular polymer matrix humidity sensor and preparation and detection methods thereof. The humidity sensor comprises a humidity-sensitive material layer, metal electrode layers and lead terminals, the humidity-sensitive material layer is arranged in the middle and formed by curing a Nafion solution, AG film is chemically plated on upper and lower surfaces of the humidity-sensitive material layer to serve as the metal electrode layers, and vacuum titanium plating film is used on the surface of the metal electrode layers to form lead terminals with areas in a range from 2mm2 to 3mm2. The humidity-sensitive material layer prepared by curing the Nafion solution, and AG is chemically plated on upper and lower surfaces of the humidity-sensitive material layer; and the lead terminals are prepared on titanium plated film on the surface layers of the metal electrode layers by a vacuum evaporation coating method. Passive conduction can be achieved, the environmental suitability is high, and miniaturization is facilitated.
Description
Technical field
The invention belongs to the Novel humidity sensor, can be used for the fields such as commercial production, biology, medical treatment, Aero-Space.
Background technology
Humidity sensor is the important chemical sensor of a class, has a wide range of applications in fields such as commercial production, process control, environmental monitoring, meteorology, Aero-Space, as: the storage of precision electronic element manufacturing, space missile, rocket.In order to create better medical environment, the industrial experiment environment, the Aero-Space production environment, to detection, the control of humidity or adjust essential.
The organic polymer humidity-sensitive material is abundant with its material source, the relative humidity wide ranges, and the excellent properties such as hysteresis is little, fast response time and obtained increasing development is the tool class humidity-sensitive material of development prospect.Mostly early stage humidity sensing polymer materials is cellulose material, and at present commonly used have a cellulose acetate class, phenylethylene, polyamine amide class, the derivant of polymethyl methacrylate class and these materials, with the multipolymer of other monomers etc.These materials all are to contain polar group, and namely hydrophilic group can be combined with hydrone interaction formation hydrogen bond or with Van der Waals force, reaches the moisture absorption purpose.
The HS1101 that common humidity sensor such as Humirel company produce, the HIH-3602 that Honeywell company produces all needs active monitoring.
Summary of the invention
The present invention proposes a kind of passive high molecular polymer base humidity sensor and preparation and determination methods method thereof, adopts perfluorinated sulfonic resin (PFSI) as humidity-sensitive material, has better application prospect.
Technical scheme of the present invention is: a kind of passive high molecular polymer base humidity sensor, comprise humidity-sensitive material layer, metal electrode layer and lead terminal, be layer structure, the centre is the humidity-sensitive material layer, described humidity-sensitive material layer is that the curing of Nafion solution forms, as metal electrode layer, adopt plating titanium film in vacuum on the surface of metal electrode layer at the upper and lower surface electroless plating Ag of humidity-sensitive material layer film, the formation area is 2 ~ 3mm
2Lead terminal.
The method for preparing described passive high molecular polymer base humidity sensor is solidified preparation humidity-sensitive material layer with Nafion solution, and humidity-sensitive material layer upper and lower surface adopts electroless plating Ag again through after alligatoring, activating, and reaction equation is:
2Ag (NH 3 ) 2 OH+C 6 H 12 O 6 → 2Ag ↓+C 6 H 11 O 7 NH 4 + 3NH 3 + H 2 OAdopt at last vacuum evaporatation at metal electrode layer top layer titanizing film preparation lead terminal.
Humidity is changed the Voltage-output that brings amplify by amplifying circuit, measure, measurement is closed and is:
,
Expression humidity,
Be the moisture sensor output voltage,
Be the amplifying circuit gain,
Be humidity-voltage transitions coefficient.
Beneficial effect:
Humidity sensor of the present invention, humidity-sensitive material high molecular polymer perfluorinated sulfonic resin (PFSI) in wet environment, can planar water self produce H
+And H
3O
+, form conductive channel at material internal, have intensive, uniform molecular level distribution form, need not external power supply, can feel wet output voltage signal, can realize passive monitoring.Output voltage is near-linear with the water cut changing law of humidity-sensitive material simultaneously, can realize the Humidity Detection of high precision, high response under particular surroundings.And humidity-sensitive material layer of the present invention and its have very strong repellence to chemical reagent, can be used for containing in the rugged surroundings such as organic gas, highly acid, strong basicity, and operating temperature range wide (50 ℃～190 ℃) is more suitable for the monitoring in particular surroundings.Designability is strong, and preparation is simple, and dynamic response is excellent, can select according to demand different types, but the size autonomous Design, structure is easy to miniaturization, and precision is high, the response time is short, and stability is high.Can satisfy the high precision Humidity Detection of all kinds of small spaces.
Description of drawings
Fig. 1 is structural upright schematic diagram of the present invention.
Wherein 1 is the humidity-sensitive material layer, and 2 is metal electrode layer, and 3 is lead terminal.
Fig. 2 is structure schematic top plan view of the present invention.
Fig. 3 is detection scheme schematic diagram of the present invention.
4 ac amplifier circuits wherein, 5 is the indicating value instrument.
Fig. 4 is humidity-voltage match family curve (V).
Embodiment
(1) sensor production
As shown in Figure 1, this humidity sensor is comprised of humidity-sensitive material layer 1, metal electrode 2 and lead terminal 3.
Described humidity-sensitive material layer 1 is perfluorinated sulfonic resin (PFSI), plays in total and experiences the effect that humidity changes; Described metal electrode 2 plays the effect of the two-plate of sensor for adopting chemical plating method to make; The titanium terminal that described lead terminal 3 is made for vacuum coating technology plays that the voltage across poles variation characteristic is passed to outside effect.
The method, the step that prepare described humidity sensor are:
The first step prepares high wet sensitive material layer 1:
A. be humidity-sensitive material layer 1 with Nafion solution according to the thickness conventional method curing molding that designs.
Second step, preparation metal electrode 2:
It is electrode material that electrode is selected metal A g.
Humidity sensitive material behind the surface coarsening is pressed the following formula chemical silvering,
2Ag(NH 3 ) 2 OH＋C 6 H 12 O 6 →2Ag↓＋C 6 H 11 O 7 NH 4 ＋3NH 3 ＋H 2 O (1)
The 3rd step: Vacuum Deposition lead terminal 3
Cut out according to size sensor.Adopt vacuum evaporatation that the titanium plated film is carried out at the electrode middle part, form 2 ~ 3mm
2Lead terminal 3, check circuit and load.So far humidity sensor completes.
(2) detection scheme
The present invention selects the common voltage amplifying circuit to carry out the measurement of micro voltage, thereby carries out moisture measurement.As shown in Figure 3,
U o Be the humidity sensor output voltage of preparation, connect micro voltage ac amplifier circuit 4 commonly used output voltage is amplified, and link to each other with indicating value instrument 5.The indicating value instrument can be selected oscillograph, registering instrument, data acquisition equipment etc.Finally the voltage that gathers can be converted into humidity value.
Measure to close and be:
Preparation size is the sensor of 5mm * 5mm * 5mm:
As shown in Figure 1, this humidity sensor is comprised of humidity-sensitive material layer 1, metal electrode 2 and lead terminal 3.
Described humidity-sensitive material layer 1 is perfluorinated sulfonic resin (PFSI), plays in total and experiences the effect that humidity changes; Described metal electrode 2 plays the effect of the two-plate of sensor for adopting chemical plating method to make; The titanium terminal that described lead terminal 3 is made for vacuum coating technology plays the change in voltage features convey to outside effect.
The method, the step that prepare described humidity sensor are:
The first step prepares high wet sensitive material layer 1:
With Nafion solution according to the design thickness conventional method curing molding be humidity-sensitive material layer 1.
Raw material: Nafion solution, sec-butyl alcohol, dimethyl sulfoxide (DMSO)
A. calculate the consumption 300mL of Nafion solution according to the size of required humidity-sensitive material layer 1.The glass mold that fills a certain amount of solution is put into vacuum drying chamber, described solution is Nafion DES 520cs, concentration is 5%wt, solute is Nafion, solvent is the potpourri of sec-butyl alcohol and water 1:1, control vacuum drying chamber temperature be 50～60 ℃, with solution dry by the fire to concentration be 20～50%.
B. dripping an amount of DMSO(volume ratio in solution is DMSO:Nafion ≈ 1:20～50) be made into casting solution, stirring 10～20 min mixes solution, casting solution is put into approximately 20～30 min of supersonic wave cleaning machine concussion, remove the bubble in the solution.Again casting solution is placed 50～60 ℃ of baking ovens, until dry tack free.
C. oven temperature is risen to 100 ℃ and also keep greater than 1h, again temperature is increased to 120～140 ℃ of maintenances greater than 3h, close baking oven, naturally cool to room temperature.So far humidity-sensitive material layer 1 preparation finished.
Second step, preparation metal electrode 2:
A. pre-service
Choose the solubility sand grains to the 1 polishing alligatoring of humidity-sensitive material layer, make the surface be the frosted shape; Activate through Ultrasonic Cleaning, watery hydrochloric acid, hydrogen peroxide successively again.Adopt afterwards conventional chemical plating method to plate Ag and form electrode;
B. electrode moulding
It is electrode material that electrode is selected metal A g.
Pretreated humidity sensitive material 1 is put into 0.03 ~ 0.06mol/L silver ammonia complex solution, leave standstill approximately 14 ~ 24h.
2Ag(NH 3 ) 2 OH＋C 6 H 12 O 6 →2Ag↓＋C 6 H 11 O 7 NH 4 ＋3NH 3 ＋H 2 O (1)
Pretreated amberplex is positioned in the ultrapure water, and the control temperature of reaction is 20 ℃, drips 1 ~ 3mL reductive agent glucose dropping (5g/L) every 10min in reaction solution, and the reaction time continues 3 ~ 5h.Reduction mechanism is (1)
So far, the electrode preparation is finished.
The 3rd step: Vacuum Deposition lead terminal 3
Cut out according to size sensor.Adopt vacuum evaporatation that the titanium plated film is carried out at the electrode middle part, form 2 ~ 3mm
2Lead terminal 3, check circuit and load.So far humidity sensor completes.
Under the useful test condition, humidity sensor to be tested, specification value is changed to benchmark with 60%RH humidity, and 25 ℃ of lower experimental fit curves are as shown in Figure 4.
Claims (3)
1. passive high molecular polymer base humidity sensor, comprise humidity-sensitive material layer (1), metal electrode layer (2) and lead terminal (3), it is characterized in that, be layer structure, the centre is humidity-sensitive material layer (1), and described humidity-sensitive material layer (1) forms for Nafion solution solidifies, at the upper and lower surface electroless plating Ag of humidity-sensitive material layer (1) film as metal electrode layer (2), plating titanium film in vacuum is adopted on surface at metal electrode layer (2), and the formation area is 2 ~ 3mm
2Lead terminal (3).
2. the method for preparing passive high molecular polymer base humidity sensor claimed in claim 1 is solidified preparation humidity-sensitive material layer with Nafion solution, it is characterized in that, humidity-sensitive material layer upper and lower surface adopts electroless plating Ag again through after alligatoring, activating, and reaction equation is:
2Ag (NH 3 ) 2 OH+C 6 H 12 O 6 → 2Ag ↓+C 6 H 11 O 7 NH 4 + 3NH 3 + H 2 OAdopt at last vacuum evaporatation at metal electrode layer (2) top layer titanizing film preparation lead terminal (3).
3. the detection method of passive high molecular polymer base humidity sensor claimed in claim 1 is characterized in that, humidity is changed the Voltage-output that brings amplify by amplifying circuit, measures, and measures to close to be:
,
Expression humidity,
Be the moisture sensor output voltage,
Be the amplifying circuit gain,
Be humidity-voltage transitions coefficient.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2116906U (en) * | 1992-03-05 | 1992-09-23 | 清华大学 | Pressure-control moisture-detected instrument |
| CN2339988Y (en) * | 1998-09-08 | 1999-09-22 | 新疆农业科学院中心实验室 | Passive soil-water-content quickly detecting instrument |
| US20110072899A1 (en) * | 2008-05-30 | 2011-03-31 | Nxp. B.V. | Sensor for determining humidity |
| CN102175730A (en) * | 2011-02-13 | 2011-09-07 | 中国科学院南京地理与湖泊研究所 | Device for measuring soil moisture |
-
2012
- 2012-11-05 CN CN201210434112.9A patent/CN102937621B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2116906U (en) * | 1992-03-05 | 1992-09-23 | 清华大学 | Pressure-control moisture-detected instrument |
| CN2339988Y (en) * | 1998-09-08 | 1999-09-22 | 新疆农业科学院中心实验室 | Passive soil-water-content quickly detecting instrument |
| US20110072899A1 (en) * | 2008-05-30 | 2011-03-31 | Nxp. B.V. | Sensor for determining humidity |
| CN102175730A (en) * | 2011-02-13 | 2011-09-07 | 中国科学院南京地理与湖泊研究所 | Device for measuring soil moisture |
Non-Patent Citations (2)
| Title |
|---|
| F.TAILOKA ET AL.: "Application of Nafion electrolytes for the detection of humidity in a corrosive atmosphere", 《SOLID STATE IONICS》, vol. 161, 31 December 2003 (2003-12-31), pages 267 - 277, XP004454917, DOI: doi:10.1016/S0167-2738(03)00145-0 * |
| 卞侃 等: "银基离子聚合物金属复合材料的制备和驱动特性", 《材料研究学报》, vol. 24, no. 5, 31 October 2010 (2010-10-31), pages 520 - 524 * |
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