CN102435636A - Quick response and recovery type barium titanate nanofiber humidity dependent sensor - Google Patents
Quick response and recovery type barium titanate nanofiber humidity dependent sensor Download PDFInfo
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- CN102435636A CN102435636A CN2011102766774A CN201110276677A CN102435636A CN 102435636 A CN102435636 A CN 102435636A CN 2011102766774 A CN2011102766774 A CN 2011102766774A CN 201110276677 A CN201110276677 A CN 201110276677A CN 102435636 A CN102435636 A CN 102435636A
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Abstract
The invention belongs to the technical field of sensor manufacture and relates to a quick response and recovery type barium titanate nanofiber humidity dependent sensor. Humidity response layers formed by a collection method on a base plate using a glass, mica or sapphire material as a non-conducting substrate is barium titanate nanofibers prepared by electrostatic spinning; the base plate is encapsulated in a sealed cavity type housing; electrode lead wires are led out through electrodes by using coaxial cables; two electrodes are fixed on the humidity response layers at two ends of the base plate respectively; and one electrode is connected in series with a current meter through a lead wire and then is connected with an end point of a rheostat, which is connected in parallel with a direct current power supply, while the other electrode is connected with the other end point of the rheostat, which is connected in parallel with the direct current power supply, so that the humidity sensor is formed. The quick response and recovery type barium titanate nanofiber humidity dependent sensor is characterized by simple manufacturing method, low cost, high production efficiency, large humidity sensitive width, high sensitivity and quick recovery and can be widely applied in various fields such as forestry and animal husbandry and the like.
Description
Technical field:
The invention belongs to the sensor preparing technical field, relate to a kind of nano material moisture sensor device that utilizes perovskite structure can to respond fast and can recover immediately, particularly a kind of quick response and recovery formula barium titanate nano fiber moisture sensor.
Background technology:
Usually; Moisture sensor is a kind of to the responsive detection property device of humidity reaction; At present, all be widely used in fields such as industry manufacturing, health care, forestry and animal husbandry, along with the development of society; People use more humidity sensor and mainly contain lithium chloride humidity sensor, carbon humidity-sensitive element, aluminium oxide hygrometer and ceramic base humidity sensor etc. the demand sustainable growth of high-performance moisture sensor.The basic role mechanism of ceramic base humidity sensor is when hydrone collides ceramic surface, and the part hydrone dissociates (or react with active ion in the pottery), produces wet quick activity thereby material resistance is reduced rapidly.The barium titanate block body ceramic material of perovskite structure is applied in last century just by wide coverage as the moisture sensor material.But; The wet quick characteristic of barium titanate bulk is also imperfect; Shortcomings such as humidity hysteresis is big such as existing, reaction and release time are long; Although methods such as people take to mix have overcome the big shortcoming of humidity hysteresis, reaction and aspect release time still be not significantly improved (Sensors andActuators B:Chemical 94 (2003) 290-293 and Thin Solid Films 515 (2007) 8776-8779).In recent years; Monodimension nanometer material is because of having the big focus that waits the quantum effect to become people's research of specific surface area; Particularly the active characteristics such as big of big, the surface atom of specific surface area help to improve the sensitivity of sensor and reduce response and release time; Chinese patent (application number 200710056363.7 for example; " electrical spinning method preparation response with recover the ceramic base nanometer fibre moisture sensor " fast) reported multiple titania-based, Zinc oxide-base and iron oxide based electrospinning fibre moisture sensor, be 1-10 second its reaction-release time, this time span can't be launched in the detection that requires shorter response time occasion.Therefore, the wet sensing performance of seeking the good humidity-sensitive material of a kind of wet sensing performance and improving current material has profound significance for the research and development of moisture sensor.
Summary of the invention:
The objective of the invention is to overcome the slow shortcoming of moisture sensor response speed that prior art exists; Seek to research and develop a kind of signal that when ambient humidity changes, can directly have a resistance; Sense wet zone big (scope is from 12%RH to 98%RH), the super fast response humidity sensor that reaction time and release time all make less than 1 second perovskite structure barium titanate nano fiber.
To achieve these goals, the quick response that the present invention relates to comprises substrate, humidity response layer, electrode, reometer, rheostat and direct supply with the agent structure of recovering the formula moisture sensor; By glass, mica or sapphire material is the barium titanate nano fiber of electrostatic spinning preparation as the humidity response layer that forms through collecting method on the substrate of non-conductive substrate; Its thickness is 100 nanometers to 1 micron; Collection has the substrate package of the nonwoven fabric construct barium titanate nano fiber humidity response layer that electrostatic spinning forms in the enclosed cavity type shell, with concentric cable through electrode extraction electrode lead-in wire; Electrode is point-like, wire or plane structure, and the employing elargol connects or welds with indium, or adopts Vacuum Coating method vapor deposition platinum, gold, silver or aluminium electrode; The rheostat of adjustable resistor formula structure mainly is for improving the common rheostat or the potentiometer of response speed; Because nonwoven fabrics barium titanate nano fiber has capacitive character, rheostat has had discharge process to the electric current that the humidity response layer produces, and rheostatic resistance is a 0.05-1M Ω scalable; Evenly collect on the substrate and form the humidity response layer; Fixedly be shaped on two electrodes of symmetrical structure on the humidity response layer at substrate two ends respectively; One of them electrode is connected to an end points after rheostat and the direct supply parallel connection after through lead serial connection reometer; Another electrode is connected to rheostat and another parallelly connected end points of direct supply through lead, whole formation humidity sensor.
When the moisture sensor that the present invention relates to prepares, earlier by optimized mix proportion scheme preparation barium titanate precursor solution; Adjustment and selection spinning condition, barium titanate nano fiber and the annealed barium titanate nano fiber humidity response layer that forms polycrystalline structure of on substrate, collecting of utilizing method of electrostatic spinning to prepare; Prepare electrode and weld out contact conductor with conventional filming technology again, adopt conventional semiconductor packaging process encapsulation then in the enclosure, prepare barium titanate nano fiber moisture sensor monomer; Connecting reometer, rheostat and direct supply by electrical principles at last constitutes response fast and recovers the formula moisture sensor.
The present invention compared with prior art, the one, directly spin the barium titanate electrocatalyst precursor solution on the substrate of glass, mica or sapphire material, its preparation method is simple, cheap, production efficiency is high; The 2nd, the barium titanate nano fiber is the polycrystalline structure that is made up of a lot of nanocrystals, compares with mono-crystlling fibre or film, has bigger specific surface area and more crystal boundary, and performance is better aspect wet quick sensing capabilities; The 3rd, when ambient humidity changed, this sensor directly produced impedance signal, surveyed humidity, and its sense is wet interval for 12%RH arrives 98%RH, and wet quick width is big; The 4th, detection process is highly sensitive, recovers rapidly, and its response time is 10
0Second-time; Can be widely used in a plurality of fields such as industrial manufacturing, health care, traffic safety, forestry and animal husbandry.
Description of drawings:
The moisture sensor syndeton principle schematic that Fig. 1 constitutes for the present invention is comprising substrate 1, humidity response layer 2, electrode 3, reometer 4, rheostat 5 and direct supply 6.
Fig. 2 be the moisture sensor that the present invention relates at the stereoscan photograph of 800 ℃ of annealing after 3 hours, wherein (a) is enlargement factor * 3500, (b) is enlargement factor * 15000.
Fig. 3 is the humidity sensing characteristic curve of the moisture sensor that the present invention relates to.
Fig. 4 is the response of the moisture sensor that the present invention relates to and is the impedance signal that produces in 1 second release time.
Embodiment:
Below through embodiment and combine accompanying drawing to further specify.
Embodiment:
The quick response that present embodiment relates to comprises substrate 1, humidity response layer 2, electrode 3, reometer 4, rheostat 5 and direct supply 6 with the agent structure of recovering the formula moisture sensor; The barium titanate nano fiber for preparing for electrostatic spinning as the humidity response layer 2 that forms through collecting method on the substrate 1 of non-conductive substrate by glass, mica or sapphire material; Its thickness is 100 nanometers to 1 micron; Collection has the substrate 1 of the nonwoven fabric construct barium titanate nano fiber humidity response layer 2 of electrostatic spinning formation to be encapsulated in the enclosed cavity type shell, goes between through electrode 3 extraction electrodes with concentric cable; Electrode 3 is point-like, wire or plane structure, and the employing elargol connects or welds with indium, or adopts Vacuum Coating method vapor deposition platinum, gold, silver or aluminium electrode; The rheostat 5 of adjustable resistor formula structure mainly is for improving the common rheostat or the potentiometer of response speed; Because nonwoven fabrics barium titanate nano fiber has capacitive character, the electric current that 5 pairs of humidity response layer of rheostat 2 produce has had discharge process, and the resistance of rheostat 5 is a 0.05-1M Ω scalable; Evenly collect on the substrate 1 and form humidity response layer 2; Fixedly be shaped on two electrodes 3 of symmetrical structure on the humidity response layer 2 at substrate 1 two ends respectively; One of them electrode 3 is connected to an end points after rheostat 5 and direct supply 6 parallel connections after through lead serial connection reometer; Another electrode 3 is connected to another end points of rheostat 5 and direct supply 6 parallel connections through lead, wholely constitutes humidity sensor.
When present embodiment is realized, earlier by optimized proportioning preparation barium titanate precursor solution; Choose spinning condition more on demand, utilize the annealed fiber humidity response layer 2 that on substrate, forms polycrystalline structure of electrospinning device and mode; Prepare electrode 3 and weld out contact conductor with conventional filming technology again, adopt conventional semiconductor packaging process encapsulation then in the enclosure, constitute the barium titanate nano fiber moisture sensor of monomer; Its concrete preparation process is:
Elder generation's weighing 1.5 gram barium acetates, 5 gram ethanol, 4 gram acetate and 1 gram deionized water mix and stir after 30 minutes, add 2 gram butyl titanates, stir 20 minutes again; Add 3.3 gram polyvinylpyrrolidones (PVP), stirred 1.5 hours, be the electrostatic spinning precursor solution after stirring; In air, carry out spinning with the electrospinning device method again, spinning condition is: 20 kilovolts of voltages, spinning nozzle interior diameter are 0.42 millimeter; Shower nozzle is 15 centimetres to the distance between the collector (substrate of the present invention); 25 ℃ of temperature, air humidity are 25%RH, and the spinning time is 10 minutes; Solvent evaporates promptly obtains the nonwoven fabrics of synthetic attitude barium titanate micro nanometer fiber in spinning process, and fibre diameter is about 300 nanometers; After annealing 3 hours through 800 ℃, PVP decomposes fully, has generated polycrystalline fibre; Barium titanate fibre diameter after the annealing is between the 120-200 nanometer; Though diameter reduces, from figure, can see that most of fiber remains continuous, and fiber is made up of fine and close crystallite; Fibre length can reach hundreds of micron or millimeter magnitude, constitutes nonwoven fabrics humidity response layer 2; There is collection the substrate sample of spinning fibre to cut into and is of a size of 1 * 1cm
2As humidity-sensitive element, fixedly be about the electrode 3 of Φ=2 millimeter on barium titanate nano fabric nonwoven cloth surface with indium; Make lead-in wire with two fine copper wires, and it is fixing to go between with elargol, measures humidity-sensitive element and change in humidity environment middle impedance value; The resistance that rheostat 5 is selected for use is 2k Ω; That reometer and direct voltage source adopt is Keithley 6487; Survey humidity environment 12%RH and 98%RH with above-mentioned barium titanate moisture sensor; Fig. 3 has shown the humidity hysteresis loop line at 10 volts of voltage lower sensors; Fig. 4 is its response-recovery curve, the response-recovery time all in 1 second, about 0.5 second; It is thus clear that this sensor not only has the super fast response process, and has very high sensitivity.
Claims (2)
1. a response and recovery formula barium titanate nano fiber moisture sensor fast is characterized in that agent structure comprises substrate, humidity response layer, electrode, reometer, rheostat and direct supply; By glass, mica or sapphire material is the barium titanate nano fiber of electrostatic spinning preparation as the humidity response layer that forms through collecting method on the substrate of non-conductive substrate; Its thickness is 100 nanometers to 1 micron; Collection has the substrate package of the nonwoven fabric construct barium titanate nano fiber humidity response layer that electrostatic spinning forms in the enclosed cavity type shell, with concentric cable through electrode extraction electrode lead-in wire; Electrode is point-like, wire or plane structure, and the employing elargol connects or welds with indium, or adopts Vacuum Coating method vapor deposition platinum, gold, silver or aluminium electrode; The rheostat of adjustable resistor formula structure is common rheostat or potentiometer; Nonwoven fabrics barium titanate nano fiber has capacitive character, and rheostat has had discharge process to the electric current that the humidity response layer produces, and rheostatic resistance is a 0.05-1M Ω scalable; Evenly collect on the substrate and form the humidity response layer; Fixedly be shaped on two electrodes of symmetrical structure on the humidity response layer at substrate two ends respectively; One of them electrode is connected to an end points after rheostat and the direct supply parallel connection after through lead serial connection reometer; Another electrode is connected to rheostat and another parallelly connected end points of direct supply through lead, whole formation humidity sensor.
2. based on described quick response of claim 1 and recovery formula barium titanate nano fiber moisture sensor, when it is characterized in that the moisture sensor that relates to prepares, press earlier mix proportion scheme preparation barium titanate precursor solution; Adjustment and selection spinning condition, barium titanate nano fiber and the annealed barium titanate nano fiber humidity response layer that forms polycrystalline structure of on substrate, collecting of utilizing method of electrostatic spinning to prepare; Prepare electrode and weld out contact conductor with conventional filming technology again, adopt the semiconductor packaging process encapsulation then in the enclosure, prepare barium titanate nano fiber moisture sensor monomer; Connecting ammeter, rheostat and dc source by electrical principles at last constitutes response fast and recovers the formula moisture sensor.
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Cited By (6)
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CN102692430A (en) * | 2012-06-07 | 2012-09-26 | 青岛大学 | Preparation method of carbon monoxide gas sensitive sensor operating in room temperature environment |
CN103412035A (en) * | 2013-08-01 | 2013-11-27 | 南京信息工程大学 | Method and device for measuring atmospheric humidity through dark current generated by electrion |
CN105160830A (en) * | 2014-06-09 | 2015-12-16 | 健安华夏(北京)科技有限公司 | Intelligent alarm device based on Internet-of-Things technology |
CN108931569A (en) * | 2018-06-28 | 2018-12-04 | 海南师范大学 | A kind of preparation and its electrochemical analysis application of hemoglobin and metatitanic acid nanofiber modified carbon ionic liquid electrode |
CN110133068A (en) * | 2019-03-28 | 2019-08-16 | 南通纺织丝绸产业技术研究院 | A kind of humidity sensor based on electrostatic spinning nano fiber fabric |
CN110702738A (en) * | 2019-09-12 | 2020-01-17 | 南京理工大学 | Capacitance/impedance type humidity sensor based on barium strontium titanate nanotube structure |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102692430A (en) * | 2012-06-07 | 2012-09-26 | 青岛大学 | Preparation method of carbon monoxide gas sensitive sensor operating in room temperature environment |
CN103412035A (en) * | 2013-08-01 | 2013-11-27 | 南京信息工程大学 | Method and device for measuring atmospheric humidity through dark current generated by electrion |
CN105160830A (en) * | 2014-06-09 | 2015-12-16 | 健安华夏(北京)科技有限公司 | Intelligent alarm device based on Internet-of-Things technology |
CN108931569A (en) * | 2018-06-28 | 2018-12-04 | 海南师范大学 | A kind of preparation and its electrochemical analysis application of hemoglobin and metatitanic acid nanofiber modified carbon ionic liquid electrode |
CN110133068A (en) * | 2019-03-28 | 2019-08-16 | 南通纺织丝绸产业技术研究院 | A kind of humidity sensor based on electrostatic spinning nano fiber fabric |
CN110133068B (en) * | 2019-03-28 | 2021-07-20 | 南通纺织丝绸产业技术研究院 | Humidity sensor based on electrostatic spinning nanofiber fabric |
CN110702738A (en) * | 2019-09-12 | 2020-01-17 | 南京理工大学 | Capacitance/impedance type humidity sensor based on barium strontium titanate nanotube structure |
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Application publication date: 20120502 |