CN102279212A - Resistive moisture sensor capable of measuring humidity of low-humidity environment and manufacturing method thereof - Google Patents
Resistive moisture sensor capable of measuring humidity of low-humidity environment and manufacturing method thereof Download PDFInfo
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- CN102279212A CN102279212A CN2011102000939A CN201110200093A CN102279212A CN 102279212 A CN102279212 A CN 102279212A CN 2011102000939 A CN2011102000939 A CN 2011102000939A CN 201110200093 A CN201110200093 A CN 201110200093A CN 102279212 A CN102279212 A CN 102279212A
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Abstract
The invention discloses a resistive moisture sensor capable of measuring humidity of a low-humidity environment and a manufacturing method thereof. The resistive moisture sensor is characterized in that a substrate is made of ceramic; pairs of inter-digital gold electrodes are arranged on the ceramic substrate; humidity-sensitive films are coated on the surfaces of the ceramic substrate and the inter-digital gold electrodes; and the humidity-sensitive films are made of cross-linking (trihydroxy silica propyl) n-butyl ammonium bromide and graphene compound humidity-sensitive materials. The resistive moisture sensor is simply manufactured and is excellent in stability. The resistive moisture sensor can be used for realizing the measurement of relative humidity in almost all the humidity ranges. Particularly, the resistive moisture sensor has lower resistance in a dry environment with the relative humidity below 10% and can be used for sensitively measuring the humidity of the low-humidity environment. The resistive moisture sensor has the advantages of higher response sensitivity, excellent response linearity, small humidity hysteresis, quick response, excellent response repeatability, and the like. The resistive moisture sensor can be widely applied to accurately measuring and controlling the environmental humidity, particularly the dry environmental humidity, in the fields, such as industrial and agricultural production, storage, atmospheric environmental monitoring, and the like.
Description
Technical field
The present invention relates to a kind of electric resistance type humidity sensitive element and preparation method thereof, especially can measure electric resistance type humidity sensitive element of low humidity ambient humidity and preparation method thereof.
Background technology
Humidity is the important physical amount that characterizes water vapour content ubiquitous in the air.The same with temperature, humidity is also closely related with human being's production life Activities, and in departments such as scientific research, modern agriculture, HVAC, weaving, machine room, Aero-Space, national defence, electric power, the detection of humidity and control all have a very important role.For this reason, the research and development of humidity sensor also is subjected to the generally attention of various countries.As desirable humidity sensor, it should have wide sensing range, can realize that preferably relative humidity is the gamut detection of 0-100%.Yet many humidity sensors of institute's research and development are applicable to all that generally detecting relative humidity is the ambient humidity of 30-90% at present.When humidity is too high, easily dewfall takes place and make sensor because the sensitive material water tolerance is relatively poor, response drift taking place even damages lost efficacy, be difficult to realize accurate mensuration.And under low wet environment, though can not damage for the sensor sensing material, because moisture is very low, then can occur can't measuring because response sensitivity is lower for the capacitor type humidity sensor; For common resistance type humidity sensor then because under the low wet environment, the electric conductivity of humidity-sensitive material is relatively poor usually, too high in resistance and be difficult to measure.This shows that the accurate measurement of low humidity and high humidity environment has become humidity sensor research urgent problem.
Current, macromolecule resistance type humidity sensor is easy, cheap with its response sensitivity height, preparation, be easy to advantage such as modification regulation and control performance, become one of emphasis of humidity sensor research and development, but the same with other various kinds of sensors, it still exists deficiency for low humidity and high humidity environment Humidity Detection.Because it mainly adopts polyelectrolyte is sensitive material, and its electric conductivity when humidity is low is very low, embodies very high resistance, is difficult to measure., need improve for sensitive material for this reason, the most frequently used and one of effective method is compound.By compound with material with satisfactory electrical conductivity, can significantly reduce the resistance of macromolecule resistance type humidity sensor under low wet environment, realize Sensitive Detection for low wet environment.But this respect work report is still less, and its research is well worth doing.
Graphene is the hypernova of material science, is called as following material.Its good electrical conductivity and extremely low background noise are expected to be used to prepare high performance sensor, and currently reported Graphene is as sensitive material even can realize Single Molecule Detection.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have under low wet environment that response sensitivity height, response are fast, good reversibility, can measure electric resistance type humidity sensitive element of low humidity ambient humidity and preparation method thereof.
The electric resistance type humidity sensitive element of measuring the low humidity ambient humidity of the present invention, has ceramic matrix, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode, on interdigital gold electrode, be connected with lead-in wire, be coated with humidity sensitive thin film at ceramic matrix and interdigital gold electrode surfaces, humidity sensitive thin film is crosslinked (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium and the compound humidity-sensitive material of Graphene.
Can measure the method for making of the electric resistance type humidity sensitive element of low humidity ambient humidity, may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, add 10-20 gram 3-aminopropyl triethoxysilane successively, 10-20 gram bromination of n-butane and 1-10 milliliter absolute ethyl alcohol, under stirring at normal temperature, led to nitrogen 10-60 minute, be warming up to 20-80 ℃ then, and under nitrogen protection, reacted 10-30 hour, to obtain reactant and continue to be warming up to 40-80 ℃, dripping 2-6 milliliter pH value is the aqueous hydrochloric acid solution of 1-5, continues reaction 0.5-3 hour, and reactant liquor dilutes with 5-30 milliliter absolute ethyl alcohol, in ether, precipitate and separate out, filter then, vacuum drying 12-60 hour, get (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium;
3) 3-15 milligram graphene oxide sonic oscillation is scattered in the 1-5 ml water, adding 50-150 microlitre mass content is 85% hydrazine hydrate, add 0.5-1.5 gram (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium then, stirring makes it fully dissolve dispersion, makes precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 0.5~2 minute, lift taking-up after, 60-120
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
The invention has the advantages that:
1) crosslinked (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium is a kind of polyelectrolyte humidity-sensitive material of excellence, and it is little that it has a humidity hysteresis, responds advantages such as fast, and have higher response sensitivity in the humidity range of broad.In addition, its cross-linked structure has significantly improved the stability of humidity-sensitive element, especially stability under high humidity environment and long-time stability.But along with humidity reduces, its resistance increases sharply, and brings very big difficulty to measurement, has limited its practical application in low wet environment is measured.With Graphene as a kind of good conductive material, obviously reduced the low wet electric resistance of element after compound with cationic polyelectrolyte, make it under low humidity, have good linear response, its sensing range is expanded near 0-100%RH, can be implemented in the interior mensuration of almost whole humidity ranges for relative humidity, and it is compound to have a good Graphene of the cationic polyelectrolyte of cross-linked structure and chemical stability, can further improve the stability of composite humidity sensor.The introducing of Graphene does not simultaneously change other wet quick characteristic of material, and composite humidity sensor still has good wet quick responses such as very little humidity hysteresis, response faster.
2) the synthetic preparation process of cationic polyelectrolyte humidity-sensitive material is simple, and cost of material is cheap, and in monomer whose (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium (APSB) water soluble.The graphene oxide that employing has water dispersible directly mixes by aqueous solution with APSB, can prepare precursor solution, and the mode by dip-coating has on the interdigital gold electrode of ceramic bases directly film forming, avoided the Graphene processing difficulties, be difficult to directly and the difficult problem of the compound preparation film humidity-sensitive element of polymkeric substance humidity-sensitive material.By hydrazine hydrate in-situ chemical reduction Graphene subsequently, and the thermal condensation polymerization of APSB monomer while cross-linking reaction, the cationic polyelectrolyte and the preparation of Graphene composite resistance type thin film humidity sensor that can obtain to have cross-linked structure easily.Method is simple for this, the humidity-sensitive element high conformity of preparation, and the yield rate height is suitable for producing in batches;
3) to have a volume little for humidity-sensitive element of the present invention, low cost, advantage such as easy to use.Adopt pottery as substrate, can improve the contact of humidity sensitive thin film and electrode basement, improve the stability of element.
Description of drawings
Fig. 1 is the structural representation of composite humidity sensor of the present invention;
Fig. 2 is the humidity hysteresis curve of electric resistance type humidity sensitive element of the present invention;
Fig. 3 is the low humidity response curve of electric resistance type humidity sensitive element of the present invention;
Fig. 4 is the response time curve of electric resistance type humidity sensitive element of the present invention.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, can measure the electric resistance type humidity sensitive element of low humidity ambient humidity, has ceramic matrix 1, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode 2, on interdigital gold electrode, be connected with lead-in wire 4, be coated with humidity sensitive thin film 3 at ceramic matrix and interdigital gold electrode surfaces, humidity sensitive thin film is crosslinked (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium and the compound humidity-sensitive material of Graphene.
The interdigital interdigital width of said potsherd matrix surface is 20-200 μ m, and interdigital gap is 20-200 μ m.
Embodiment 1:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, and adds 10 gram 3-aminopropyl triethoxysilanes successively, 10 gram bromination of n-butane and 2 milliliters of absolute ethyl alcohols.Logical nitrogen is 10 minutes under stirring at normal temperature, is warming up to 30 ℃ then, and reacts 10 hours under nitrogen protection.To obtain reactant and continue to be warming up to 40 ℃, drip 2 milliliters of pH values and be 1 aqueous hydrochloric acid solution, continue reaction 0.5 hour.Afterwards, reactant liquor dilutes with 5 milliliters of absolute ethyl alcohols, precipitates in ether and separates out, and filters then, through vacuum drying 12 hours, promptly obtains faint yellow solid product (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium (APSB);
3) 3 milligrams of graphene oxides are scattered in 1 ml water through sonicated, add 50 microlitre mass content and be 85% hydrazine hydrate, add 0.5 gram APSB then, stir and make it fully dissolve dispersion, make precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 0.5 minute, lift taking-up after, 60
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
Embodiment 2:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, and adds 12 gram 3-aminopropyl triethoxysilanes successively, 12 gram bromination of n-butane and 5 milliliters of absolute ethyl alcohols.Logical nitrogen is 20 minutes under stirring at normal temperature, is warming up to 40 ℃ then, and reacts 12 hours under nitrogen protection.To obtain reactant and continue to be warming up to 45 ℃, drip 3 milliliters of pH values and be 1.5 aqueous hydrochloric acid solution, continue reaction 1 hour.Afterwards, reactant liquor dilutes with 8 milliliters of absolute ethyl alcohols, precipitates in ether and separates out, and filters then, through vacuum drying 15 hours, promptly obtains faint yellow solid product A PSB;
3) 4 milligrams of graphene oxides are scattered in 2 ml waters through sonicated, add 60 microlitre mass content and be 85% hydrazine hydrate, add 0.8 gram APSB then, stir and make it fully dissolve dispersion, make precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 1 minute, lift taking-up after, 80
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
Embodiment 3:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, and adds 15 gram 3-aminopropyl triethoxysilanes successively, 14 gram bromination of n-butane and 3 milliliters of absolute ethyl alcohols.Logical nitrogen is 25 minutes under stirring at normal temperature, is warming up to 50 ℃ then, and reacts 20 hours under nitrogen protection.To obtain reactant and continue to be warming up to 55 ℃, drip 3.5 milliliters of pH values and be 3 aqueous hydrochloric acid solution, continue reaction 1.5 hours.Afterwards, reactant liquor dilutes with 15 milliliters of absolute ethyl alcohols, precipitates in ether and separates out, and filters then, through vacuum drying 20 hours, promptly obtains faint yellow solid product A PSB;
3) 6 milligrams of graphene oxides are scattered in 3 ml waters through sonicated, add 75 microlitre mass content and be 85% hydrazine hydrate, add 1 gram APSB then, stir and make it fully dissolve dispersion, make precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 1.2 minutes, lift taking-up after, 100
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
Embodiment 4:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, and adds 20 gram 3-aminopropyl triethoxysilanes successively, 120 gram bromination of n-butane and 10 milliliters of absolute ethyl alcohols.Logical nitrogen is 60 minutes under stirring at normal temperature, is warming up to 70 ℃ then, and reacts 30 hours under nitrogen protection.To obtain reactant and continue to be warming up to 80 ℃, drip 6 milliliters of pH values and be 5 aqueous hydrochloric acid solution, continue reaction 3 hours.Afterwards, reactant liquor dilutes with 30 milliliters of absolute ethyl alcohols, precipitates in ether and separates out, and filters then, through vacuum drying 60 hours, promptly obtains faint yellow solid product A PSB;
3) 15 milligrams of graphene oxides are scattered in 5 ml waters through sonicated, add 150 microlitre mass content and be 85% hydrazine hydrate, add 1.5 gram APSB then, stir and make it fully dissolve dispersion, make precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 2 minutes, lift taking-up after, 120
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
The humidity hysteresis curve of electric resistance type humidity sensitive element of the present invention is seen Fig. 2, and by the figure finding, the humidity hysteresis of humidity-sensitive element is very little, is about 1%RH.
As seen from Figure 3, under low moisture conditions, electric resistance type humidity sensitive element of the present invention has good response linearity under linear coordinate, and sensitivity is higher, embodies well wet quick characteristic, can realize being low to moderate the Sensitive Detection of the low wet environment of 0.2%RH;
As seen from Figure 4, when the electric resistance type humidity sensitive element of the present invention preparation was changed under the height wet environment of 84%RH and 11%RH, humidity-sensitive element embodied than response speed faster, and its moisture absorption and dehumidification time are shorter, are respectively 32 seconds and 48 seconds.
Claims (2)
1. can measure the electric resistance type humidity sensitive element of low humidity ambient humidity, it is characterized in that: it has ceramic matrix ⑴, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode ⑵, on interdigital gold electrode, be connected with lead-in wire ⑷, be coated with humidity sensitive thin film ⑶ at ceramic matrix and interdigital gold electrode surfaces, humidity sensitive thin film is crosslinked (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium and the compound humidity-sensitive material of Graphene.
2. the method for making of measuring the electric resistance type humidity sensitive element of low humidity ambient humidity according to claim 1 is characterized in that may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) there-necked flask is dewatered deoxygenation is handled, add 10-20 gram 3-aminopropyl triethoxysilane successively, 10-20 gram bromination of n-butane and 1-10 milliliter absolute ethyl alcohol, under stirring at normal temperature, led to nitrogen 10-60 minute, be warming up to 20-80 ℃ then, and under nitrogen protection, reacted 10-30 hour, to obtain reactant and continue to be warming up to 40-80 ℃, dripping 2-6 milliliter pH value is the aqueous hydrochloric acid solution of 1-5, continues reaction 0.5-3 hour, and reactant liquor dilutes with 5-30 milliliter absolute ethyl alcohol, in ether, precipitate and separate out, filter then, vacuum drying 12-60 hour, get (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium;
3) 3-15 milligram graphene oxide sonic oscillation is scattered in the 1-5 ml water, adding 50-150 microlitre mass content is 85% hydrazine hydrate, add 0.5-1.5 gram (the silica-based propyl group of trihydroxy) normal-butyl bromination ammonium then, stirring makes it fully dissolve dispersion, makes precursor solution;
4) the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 0.5~2 minute, lift taking-up after, 60-120
oC is heating down, obtains measuring the electric resistance type humidity sensitive element of low humidity ambient humidity.
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CN103323498A (en) * | 2013-07-09 | 2013-09-25 | 山东师范大学 | Resistance type relative humidity sensor based on graphene carbon nanotube composite material |
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CN103323498A (en) * | 2013-07-09 | 2013-09-25 | 山东师范大学 | Resistance type relative humidity sensor based on graphene carbon nanotube composite material |
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CN104502420A (en) * | 2014-10-01 | 2015-04-08 | 浙江大学 | Humidity-sensitive composite membrane, preparation method of humidity-sensitive composite membrane and humidity sensor |
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CN106908514A (en) * | 2017-03-08 | 2017-06-30 | 电子科技大学 | A kind of humidity sensor film that reaction is redissolved based on microcell and preparation method thereof |
CN108195888A (en) * | 2017-12-27 | 2018-06-22 | 长春理工大学 | Impedance type dew cell using the compound wet sensory material of cross-linked polymer and preparation method thereof |
CN108593717A (en) * | 2018-04-26 | 2018-09-28 | 京东方科技集团股份有限公司 | A kind of humidity sensor and preparation method thereof, electronic equipment |
WO2020192318A1 (en) * | 2019-03-26 | 2020-10-01 | 京东方科技集团股份有限公司 | Method and apparatus for detecting ambient humidity |
CN115368501A (en) * | 2022-08-11 | 2022-11-22 | 中科检测技术服务(广州)股份有限公司 | Humidity-sensitive response material containing titanium carbide nano particles and having good temperature change stability and device thereof |
CN115368501B (en) * | 2022-08-11 | 2024-02-13 | 中科检测技术服务(广州)股份有限公司 | Humidity-sensitive response material containing titanium carbide nano particles and having good temperature change stability and device thereof |
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