CN100385703C - Siliceous copolymer resistor type thin film humidity sensitive element and method for making same - Google Patents
Siliceous copolymer resistor type thin film humidity sensitive element and method for making same Download PDFInfo
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- CN100385703C CN100385703C CNB2005100489305A CN200510048930A CN100385703C CN 100385703 C CN100385703 C CN 100385703C CN B2005100489305 A CNB2005100489305 A CN B2005100489305A CN 200510048930 A CN200510048930 A CN 200510048930A CN 100385703 C CN100385703 C CN 100385703C
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Abstract
The present invention discloses a siliceous copolymer resistance type thin film humidity sensitive element and a manufacture method thereof. The resistance type film humidity sensitive element containing silicon copolymer has a microcrystalline glass film base body, and a surface of the microcrystalline glass film base body is provided with multiple pairs of interdigital gold electrodes via evaporation and photolithography. The interdigital gold electrodes are connected with lead wires, the surfaces of the microcrystalline glass film base body and the interdigital gold electrodes are coated with humidity sensitive films, and the humidity sensitive films are copolymers of silicon containing cationic polyelectrolyte. The method has the steps: 1, a treater dips the microcrystalline glass interdigital gold electrodes into humidity sensitive liquid, and the gold electrodes are manufactured into the humidity sensitive films after pulled, taken out and heat treatment; 2, the microcrystalline glass interdigital gold electrodes with the humidity sensitive films are energized for ageing in certain humidity and temperature, and the resistance type film humidity sensitive element containing silicon copolymer can be manufactured. The present invention is a resistance type humidity sensitive element with the advantages of wide humidity range, high sensitivity and rapid response speed, the manufacture method is simple and has low cost, and the present invention can be widely used for the accurate measurement and control in processes and environmental humidity.
Description
Technical field
The present invention relates to a kind of silicon-containing copolymer resistance type thin film humidity-sensitive element and preparation method thereof.
Background technology
The developing into us and opened up a wide transducer space of the progress of society and technology, humidity sensor is the important chemical sensor of a class, have a wide range of applications at aspects such as storage, industrial production, process control, environmental monitoring, household electrical appliance, meteorologies, and in modern development in science and technology and people's life, play a part to become more and more important.High molecule humidity sensor is to use the wider novel humidity sensor of a class at present, mainly contains capacitor type and resistor-type two big classes.Macromolecule resistance type humidity sensor wherein, more with its good response characteristic, the hygrometric wide ranges is made simply, is easy to integratedly, and miniaturization is produced in batches, and lower-price characteristic becomes the trend of research and development.The main humidity-sensitive material of its application is exactly a complex polyelectrolyte particle.Advantages such as complex polyelectrolyte particle has cheap, makes simply, and is highly sensitive, and the moisture absorption response is fast develop very fast.But it also exists the dehumidification response speed and owes to be difficult to measure low wet environment soon, not anti-high humidity, and problem such as response sensitivity is low under the high humidity environment, and long-time stability and reliability are not ideal enough hinders and has restricted its practical application and further develop.This is main because of the easy adsorbed water molecule of polyelectrolyte, but is not easy to free hydrone, and humidity-sensitive film and electrode base materials caking property are bad simultaneously, the event of expanding easily in high humidity environment and come off.
Summary of the invention
The purpose of this invention is to provide a kind of silicon-containing copolymer resistance type thin film humidity-sensitive element and preparation method thereof.
The silicon-containing copolymer resistance type thin film humidity-sensitive element has the devitrified glass sheet matrix, evaporation, photoetching have many to interdigital gold electrode on the microcrystalline glass matrix surface, on interdigital gold electrode, be connected with lead-in wire, be coated with humidity-sensitive film on devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity-sensitive film is siliceous cationic polyelectrolyte copolymer.
The step of the manufacture method of silicon-containing copolymer resistance type thin film humidity-sensitive element is as follows:
1) with dip coater the interdigital gold electrode of devitrified glass is immersed in the wet-sensitive liquid 1～4 minute, after lifting, take out by the speed of 2～8mm/ second, made humidity-sensitive film in 5～15 hours 80～120 ℃ of heat treatments;
2) the interdigital gold electrode of devitrified glass that will have humidity-sensitive film is at 30～40 ℃, and humidity is under 60～90%RH environment, 100～800mv in addition, and the alternating voltage of 1kHz, aging 20～50 hours of energising makes the silicon-containing copolymer resistance type thin film humidity-sensitive element.
Advantage of the present invention is:
1. adopt the interdigital gold electrode of particular design devitrified glass: interdigital is 8～16 pairs, and interdigital width is 20～80 μ m, and interdigital gap is 40～80 μ m, each interdigital length is 2～3mm, and electrode size is 6mm * 5mm * 0.5mm, and it is little to have a volume, low cost, advantage such as easy to use.The kind electrode structure reduces the dew cell impedance owing to interdigital thin and close, and sensitivity improves, thereby can measure the humidity under the low wet environment, and detection range is widened;
2. when the preparation humidity-sensitive film, composition by the control silicon-containing copolymer, get final product polymerizing cationically monomer-dimethylaminoethyl methacrylate NBB quaternary amine and functional form siloxanyl monomers-methyl allyl acyloxypropyl trimethoxysilane, the concentration of mol ratio that both are appropriate and control preparation wet-sensitive liquid makes dew cell have express moisture absorption and dehumidification response speed;
3. the introducing of functional form siloxanyl monomers in the silicon-containing copolymer, utilize alkoxyl (Si-OR) hydrolysis in wet-sensitive liquid-aqueous solution in the siloxanes, change into silanol base (Si-OH), the latter can be further with the devitrified glass sheet matrix on hydroxyl (OH) forming hydrogen bond combines, thereby can strengthen the caking property of humidity sensing film and devitrified glass sheet matrix, improve the ability of the anti-high humidity environment of dew cell;
4. the introducing of the functional form siloxanyl monomers in the silicon-containing copolymer, by regulating its ratio in copolymer is formed, utilize the hydrophobic property of siloxanes, the speed of the dehumidification of scalable dew cell, it is fast to have overcome general high molecule electric resistance type humidity sensitive element moisture absorption, the disadvantage that dehumidification is slow;
5. under 30～40 ℃ and 60～90%RH humidity environment, element is passed to certain alternating voltage, carry out burin-in process, can make element reach stable state within a short period of time, have high stability and anti-high humidity environment ability;
6. adopt the humidity-sensitive material of the present invention's design and the dew cell of method preparation, be to combine as wet sensory material and with the interdigital gold electrode of the devitrified glass with particular design with the copolymer of functional form siloxanyl monomers with the polymerizable cationic monomer, constitute the advanced high molecule electric resistance type humidity sensitive element that has the two advantage concurrently, have excellent humidity sensing characteristic.(5～100%RH), highly sensitive, not only anti-high humidity environment ability is strong for its hygrometric wide ranges, and still have good humidity sensing characteristic in the low humidity scope, and have the response speed that is exceedingly fast and little humidity hysteresis especially, and simple and easy to do, the element high conformity, cost is low, is suitable for producing in batches.
Description of drawings
Fig. 1 is the structural representation of dew cell of the present invention;
Fig. 2 is the typical response characteristic figure of dew cell of the present invention;
Fig. 3 is the typical humidity hysteresis performance plot of dew cell of the present invention;
Fig. 4 is dew cell typical response time response figure of the present invention.
Embodiment
The principle of the invention is to adopt the polymerizable cationic monomer to combine as wet sensory material and with the interdigital gold electrode of the devitrified glass with particular design with the copolymer of functional form siloxanyl monomers, constitutes the high molecule electric resistance type humidity sensitive element that has the two advantage concurrently.Provide transportable ion by the quaternary amine in the copolymer, utilize its hydrophobic property to regulate the dehumidification speed of dew cell by the siloxanes in the copolymer, utilize its siloxane group in wet-sensitive liquid to change into the silanol base simultaneously, can form hydrogen bond with the hydroxyl on the devitrified glass sheet matrix combines, thereby strengthen the caking property of humidity sensing film and devitrified glass sheet matrix, be equipped with on the devitrified glass sheet matrix thin and close golden interdigitally again, the dew cell impedance is reduced, sensitivity improves.Thereby make the high molecule electric resistance type humidity sensitive element of humidity sensing characteristic excellence, and easy row simple for production, cost is low.
The silicon-containing copolymer resistance type thin film humidity-sensitive element has devitrified glass sheet matrix 1, evaporation, photoetching have many to interdigital gold electrode 2 on the microcrystalline glass matrix surface, on interdigital gold electrode, be connected with lead-in wire 4, be coated with humidity-sensitive film 3 on microcrystalline glass and interdigital gold electrode surfaces, humidity-sensitive film is siliceous cationic polyelectrolyte copolymer.
Evaporation, photoetching have 8～16 pairs of interdigital gold electrodes on the microcrystalline glass matrix surface, and the interdigital width of interdigital gold electrode is 20～80 μ m, and interdigital gap is 40～80 μ m, and each interdigital length is 2～3mm, and electrode size is 6mm * 5mm * 0.5mm.Humidity-sensitive film is siliceous cationic polyelectrolyte copolymer, it is by polymerizable cationic monomer-dimethylaminoethyl methacrylate NBB quaternary amine and functional form siloxanyl monomers-methyl allyl acyloxypropyl trimethoxysilane, by 1～6: 1 mol ratio copolymerization forms.Wet-sensitive liquid is made up of the deionized water of 1～6 part of heavy silicon-containing copolymer and 100 parts of weights.
Embodiment 1:
1. electrode cleans
With the interdigital gold electrode of devitrified glass through absolute ethyl alcohol and acetone soaking and washing, dry for standby
2. dip-coating prepares humidity-sensitive film and reprocessing
(the batching mol ratio of 20 parts of heavy silicon-containing copolymer-quaternary amines and siloxanes is 4: 1 to adopt dip coater that the interdigital gold electrode of devitrified glass is immersed wet-sensitive liquid, 100 parts heavy deionized waters) in, after 4 minutes, lift with 8mm/ speed second, taking-up is inserted in the constant temperature oven, 80 ℃ of heat treatments 15 hours, make humidity-sensitive film;
3. burin-in process
With having the dew cell of humidity-sensitive film on the interdigital gold electrode of devitrified glass, place climatic chamber, at 40 ℃, under the 60%RH environment, add 800mv, the alternating voltage of 1kHz, aging 20 hours of energising.
Embodiment 2:
1. electrode cleans with embodiment 1
2. dip-coating prepares humidity-sensitive film and reprocessing
(the batching mol ratio of 40 parts of heavy silicon-containing copolymer-quaternary amines and siloxanes is 2: 1 to adopt dip coater that the interdigital gold electrode of devitrified glass is immersed wet-sensitive liquid, 100 parts heavy deionized waters) in, after 2 minutes, lift with 6mm/ speed second, taking-up is inserted in the constant temperature oven, 110 ℃ of heat treatments 8 hours, make humidity-sensitive film;
3. burin-in process
With having the dew cell of humidity-sensitive film on the interdigital gold electrode of devitrified glass, at 30 ℃, under the 90%RH environment, add 300mv, the alternating voltage of 1kHz, aging 30 hours of energising.
Its wet quick response characteristic such as Fig. 2, humidity hysteresis characteristic such as Fig. 3, response time properties such as Fig. 4.
Embodiment 3:
1. electrode cleans with embodiment 1
2. dip-coating prepares humidity-sensitive film and reprocessing
(the batching mol ratio of 60 parts of heavy silicon-containing copolymer-quaternary amines and siloxanes is 6: 1 to adopt dip coater that the interdigital gold electrode of devitrified glass is immersed wet-sensitive liquid, 100 parts heavy deionized waters) in, after 1 minute, lift with 2mm/ speed second, taking-up is inserted in the constant temperature oven, 120 ℃ of heat treatments 5 hours, make humidity-sensitive film;
3. burin-in process
With having the dew cell of humidity-sensitive film on the interdigital gold electrode of devitrified glass, at 30 ℃, under the 80%RH environment, add 100mv, the alternating voltage of 1kHz, aging 50 hours of energising.
Embodiment 4:
1. electrode cleans with embodiment 1
2. dip-coating prepares humidity-sensitive film and reprocessing
(the batching mol ratio of 40 parts of heavy silicon-containing copolymer-quaternary amines and siloxanes is 1: 1 to adopt dip coater that the interdigital gold electrode of devitrified glass is immersed wet-sensitive liquid, 100 parts heavy deionized waters) in, after 3 minutes, lift with 4mm/ speed second, taking-up is inserted in the constant temperature oven, 90 ℃ of heat treatments 12 hours, make humidity-sensitive film;
3. burin-in process
With having the dew cell of humidity-sensitive film on the interdigital gold electrode of devitrified glass, at 35 ℃, under the 80%RH environment, add 600mv, the alternating voltage of 1kHz, aging 25 hours of energising.
Claims (5)
1. silicon-containing copolymer resistance type thin film humidity-sensitive element, it is characterized in that: it has devitrified glass sheet matrix (1), on the microcrystalline glass matrix surface, evaporate, photoetching has many to interdigital gold electrode (2), on interdigital gold electrode, be connected with lead-in wire (4), on devitrified glass sheet matrix and interdigital gold electrode surfaces, be coated with humidity-sensitive film (3), humidity-sensitive film (3) is siliceous cationic polyelectrolyte copolymer, evaporate on the described microcrystalline glass matrix surface, photoetching has 8～16 pairs of interdigital gold electrodes, the interdigital width of interdigital gold electrode is 20～80 μ m, interdigital gap is 40～80 μ m, and each interdigital length is 2～3mm.
2. a kind of silicon-containing copolymer resistance type thin film humidity-sensitive element according to claim 1, it is characterized in that: described humidity-sensitive film is siliceous cationic polyelectrolyte copolymer, it is by polymerizable cationic monomer-dimethylaminoethyl methacrylate NBB quaternary amine and functional form siloxanyl monomers-methyl allyl acyloxypropyl trimethoxysilane, by 1～6: 1 mol ratio copolymerization forms.
3. the manufacture method of a silicon-containing copolymer resistance type thin film humidity-sensitive element as claimed in claim 1, it is characterized in that: the step of method is as follows:
1) with dip coater the interdigital gold electrode of devitrified glass is immersed in the wet-sensitive liquid 1～4 minute, after lifting, take out by the speed of 2～8mm/ second, made humidity-sensitive film in 5～15 hours 80～120 ℃ of heat treatments;
2) the interdigital gold electrode of devitrified glass that will have humidity-sensitive film is at 30～40 ℃, and humidity is under 60～90%RH environment, 100～800mv in addition, and the alternating voltage of 1kHz, aging 20～50 hours of energising makes the silicon-containing copolymer resistance type thin film humidity-sensitive element.
4. the manufacture method of a kind of silicon-containing copolymer resistance type thin film humidity-sensitive element according to claim 3, it is characterized in that: the interdigital gold electrode of described devitrified glass is that evaporation, photoetching have 8～16 pairs of interdigital gold electrodes on the devitrified glass sheet matrix, the interdigital width of interdigital gold electrode is 20～80 μ m, interdigital gap is 40～80 μ m, and each interdigital length is 2～3mm.
5. the manufacture method of a kind of silicon-containing copolymer resistance type thin film humidity-sensitive element according to claim 3 is characterized in that: described wet-sensitive liquid is made up of the deionized water of 1～6 part of heavy silicon-containing copolymer and 100 parts of weights.
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| CNB2005100489305A CN100385703C (en) | 2005-01-18 | 2005-01-18 | Siliceous copolymer resistor type thin film humidity sensitive element and method for making same |
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| CNB2005100489305A CN100385703C (en) | 2005-01-18 | 2005-01-18 | Siliceous copolymer resistor type thin film humidity sensitive element and method for making same |
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| CN100385703C true CN100385703C (en) | 2008-04-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439910C (en) * | 2006-09-29 | 2008-12-03 | 浙江大学 | High-polymer resistance type thin film humidity-sensitive element with high water-proofing performance and producing method thereof |
| CN101692329B (en) * | 2009-09-10 | 2012-07-11 | 福建华映显示科技有限公司 | Impedance value detection method for display and display carrying structure |
| CN102304199B (en) * | 2011-05-25 | 2014-06-18 | 广州海谷电子科技有限公司 | Humidity and heat resistant water sensitive resin and humidity and heat resistant polymer resistance type humidity sensitive film and preparation methods thereof |
| CN106896141B (en) * | 2017-03-22 | 2019-05-28 | 吉林大学 | A kind of dew cell and preparation method based on polymer-modified silicon dioxide granule |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61147142A (en) * | 1984-12-20 | 1986-07-04 | Mitsubishi Electric Corp | Moisture sensitive material |
| EP1139092A2 (en) * | 2000-03-31 | 2001-10-04 | TDK Corporation | Humidity sensor and method for making |
| CN1459876A (en) * | 2002-12-19 | 2003-12-03 | 李扬 | Orgaic polymer-inorganic nano composite resistance type thin film humidity sensitive element and its manufacturing method |
| CN2788362Y (en) * | 2005-01-18 | 2006-06-14 | 黄德欢 | Resistance-type film humidity-sensitive element containing silicon copolymer |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61147142A (en) * | 1984-12-20 | 1986-07-04 | Mitsubishi Electric Corp | Moisture sensitive material |
| EP1139092A2 (en) * | 2000-03-31 | 2001-10-04 | TDK Corporation | Humidity sensor and method for making |
| CN1459876A (en) * | 2002-12-19 | 2003-12-03 | 李扬 | Orgaic polymer-inorganic nano composite resistance type thin film humidity sensitive element and its manufacturing method |
| CN2788362Y (en) * | 2005-01-18 | 2006-06-14 | 黄德欢 | Resistance-type film humidity-sensitive element containing silicon copolymer |
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