CN102565146A - Resistance type humidity element and preparation method thereof - Google Patents

Resistance type humidity element and preparation method thereof Download PDF

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Publication number
CN102565146A
CN102565146A CN2011104432123A CN201110443212A CN102565146A CN 102565146 A CN102565146 A CN 102565146A CN 2011104432123 A CN2011104432123 A CN 2011104432123A CN 201110443212 A CN201110443212 A CN 201110443212A CN 102565146 A CN102565146 A CN 102565146A
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humidity
sensitive element
sensitive
preparation
resistance
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CN102565146B (en
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张小水
肜建娜
祁明锋
张利霞
王向涛
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WEISHENG ELECTRONICS TECH Co Ltd ZHENGZHOU
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WEISHENG ELECTRONICS TECH Co Ltd ZHENGZHOU
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Abstract

The invention provides a resistance type humidity element and a preparation method thereof. The humidity element comprises a humidity element substrate, a humidity element electrode arranged on the humidity element substrate, and a hydrophilic low-resistance humidity sensing film and a hydrophobic high-resistance humidity sensing film which are arranged on the humidity element electrode in turn, wherein the hydrophilic low-resistance humidity sensing film and the hydrophobic high-resistance humidity sensing film are compounded together by a thermal crosslinking process. The preparation method comprises the following steps of: preparing the humidity element electrode on the humidity element substrate; preparing a prepolymerization solution 1 and a prepolymerization solution 2; and performing dip coating on the humidity element electrode in the prepolymerization solution 1, drying the humidity element under an infrared lamp, performing dip coating on the humidity element electrode in the prepolymerization solution 2, and performing thermal crosslinking to obtain the resistance type humidity element. The humidity element has the advantages of simple structure, moderate resistance, excellent performance, high precision and high adaptability, and the preparation method has the advantages of being easy to implement, along with simple process and low cost.

Description

Electric resistance type humidity sensitive element and preparation method thereof
Technical field
The present invention relates to a kind of humidity-sensitive element, specifically, related to a kind of electric resistance type humidity sensitive element and preparation method thereof.
Background technology
Humidity sensor was risen the seventies in 20th century, in fields such as industrial and agricultural production, fresh-keeping, the weather forecast of storage, national defence, environmental protection, household electrical appliances, scientific research and space flight great demand was arranged; Existing resistance type humidity sensor because that aspects such as the wet element production technology of structural design, material selection, sense exist is not enough, in use, exists that output accuracy is not high, the problem of humidity bad adaptability.
In order to solve the problem of above existence, people are seeking a kind of desirable technical solution always.
Summary of the invention
The objective of the invention is the deficiency to prior art, thus provide a kind of simple in structure, resistance is moderate, excellent performance, high, the adaptable electric resistance type humidity sensitive element of precision, and a kind of preparation method of electric resistance type humidity sensitive element also is provided.
To achieve these goals; The technical scheme that the present invention adopted is: a kind of electric resistance type humidity sensitive element; It comprises the humidity-sensitive element substrate, is arranged on the on-chip humidity-sensitive element electrode of said humidity-sensitive element and is successively set on hydrophilic low-resistance humidity-sensitive film and the hydrophobic high resistant humidity-sensitive film on the said humidity-sensitive element electrode that said hydrophilic low-resistance humidity-sensitive film and said hydrophobic high resistant humidity-sensitive film are combined with each other through heat cross-linking technology.
A kind of preparation method of electric resistance type humidity sensitive element, it may further comprise the steps:
Step 1, on said humidity-sensitive element substrate the preparation said humidity-sensitive element electrode;
Get 1~3 milliliter of methylacryoyloxyethyl trimethyl ammonium chloride solution, join in 2~4 milliliters the absolute ethyl alcohol, stir, make pre-polymerization liquid 1;
In the closed container of anhydrous and oxygen-free, add 3-aminopropyl triethoxysilane, bromination of n-butane, absolute ethyl alcohol successively, under 40~50 ℃ temperature, the water-bath closed container, and carry out magnetic agitation; Then, the flow feeding argon gas with 60~150 ml/min reacts after 20~30 hours; Obtain Polymer Solution, more said Polymer Solution is poured in the excessive absolute ether, obtain white depositions; And, obtain white powder with the vacuum drying at room temperature of said white depositions, last; Get said white powder 1~3 gram, be dissolved in 3.5~6.5 milliliters the absolute ethyl alcohol, make pre-polymerization liquid 2;
Step 2, said humidity-sensitive element electrode lifted plated film in pre-polymerization liquid 1 after, infrared lamp baking 1~3 hour down lifts plated film again in pre-polymerization liquid 2, then, in 80~100 ℃ baking oven, carry out heat cross-linking, keeps 6~10 hours, promptly gets electric resistance type humidity sensitive element.
Based on above-mentioned, in step 1, after adopting silk-screen printing technique printed silver slurry conductiving point and interdigital carbon electrode on the said humidity-sensitive element substrate, adopt the reflow soldering process welding to go up Y type lead-in wire again, prepare said humidity-sensitive element electrode with this.
Based on above-mentioned, said humidity-sensitive element substrate is an alumina ceramic substrate.
The relative prior art of the present invention has outstanding substantive distinguishing features and marked improvement; Specifically, this electric resistance type humidity sensitive element is to be composited by two kinds of different humidity-sensitive films of resistance, arrives under the different humidity of high humidity at low humidity; The material that the hydrophilic low-resistance humidity-sensitive film of ground floor is adopted is the macromolecular materials that contain strong polar group like that such as ammonium chloride quaternary ammonium salt; Its water wettability is stronger, and resistance integral body is on the low side, and the material that the hydrophobic high resistant humidity-sensitive film of the second layer is adopted is the material that silane quaternary ammonium salt etc. contains hydrophobic group; Its hydrophobicity is stronger; Resistance integral body is higher, and these two kinds of different humidity-sensitive films of resistance are combined, and can obtain that resistance is moderate, excellent performance, high, the adaptable humidity-sensitive element of precision.The material that this preparation method will have technology and new proportioning now combines, and makes the humidity-sensitive element performance of preparation more stable, consistance is strong, its have technology simple, be easy to realization, low cost and other advantages.
Description of drawings
Fig. 1 is the structural representation of said electric resistance type humidity sensitive element.
Fig. 2 is the experimental data chart of said humidity-sensitive element 1.
Fig. 3 is the experimental data chart of said humidity-sensitive element 2.
Fig. 4 is the experimental data chart of said humidity-sensitive element 3.
Embodiment
Through embodiment, technical scheme of the present invention is done further detailed description below.
As shown in Figure 1; A kind of electric resistance type humidity sensitive element; It comprises humidity-sensitive element substrate 1, is arranged on the humidity-sensitive element electrode on the said humidity-sensitive element substrate 1 and is successively set on hydrophilic low-resistance humidity-sensitive film 5 and the hydrophobic high resistant humidity-sensitive film 6 on the said humidity-sensitive element electrode that said hydrophilic low-resistance humidity-sensitive film 5 is combined with each other through heat cross-linking technology with said hydrophobic high resistant humidity-sensitive film 6; Said humidity-sensitive element electrode includes a pair of interdigital carbon electrode 2, a pair of silver slurry conductiving point 3 and a pair of Y type lead-in wire 4, and said humidity-sensitive element substrate 1 is an alumina ceramic substrate.
A kind of preparation method of electric resistance type humidity sensitive element, it may further comprise the steps:
Step 1, on said humidity-sensitive element substrate 1 preparation said humidity-sensitive element electrode; Specifically comprise: after adopting silk-screen printing technique printing a pair of silver slurry conductiving point 3 and a pair of interdigital carbon electrode 2 on the said humidity-sensitive element substrate 1, adopt the reflow soldering process welding to go up a pair of Y type lead-in wire 4 again;
Get methylacryoyloxyethyl trimethyl ammonium chloride solution, promptly get 1~3 milliliter of DMC solution, join in 2~4 milliliters the absolute ethyl alcohol, stir, make pre-polymerization liquid 1;
In the closed container of anhydrous and oxygen-free, add 3-aminopropyl triethoxysilane, bromination of n-butane, absolute ethyl alcohol successively, under 40~50 ℃ temperature, the water-bath closed container, and carry out magnetic agitation; Then, the flow feeding argon gas with 60~150 ml/min reacts after 20~30 hours; Obtain Polymer Solution, more said Polymer Solution is poured in the excessive absolute ether, obtain white depositions; And, obtain white powder with the vacuum drying at room temperature of said white depositions, last; Get said white powder 1~3 gram, be dissolved in 3.5~6.5 milliliters the absolute ethyl alcohol, make pre-polymerization liquid 2;
Step 2, a pair of interdigital carbon electrode 2 of said humidity-sensitive element electrode lifted plated film in pre-polymerization liquid 1 after, infrared lamp baking 1~3 hour down lifts plated film again in pre-polymerization liquid 2; Then, in 80~100 ℃ baking oven, carry out heat cross-linking; Kept 6~10 hours, and promptly got electric resistance type humidity sensitive element.
Experiment test:Adopt identical test to use the humidity-sensitive element electrode, under identical condition, will test with the humidity-sensitive element electrode and in pre-polymerization liquid, lift plated film, in baking oven, carry out heat cross-linking again with humidity-sensitive element substrate and test; To test with the humidity-sensitive element electrode and in pre-polymerization liquid 1, lift plated film, heat cross-linking, obtain humidity-sensitive element 1; To test with the humidity-sensitive element electrode and in pre-polymerization liquid 2, lift plated film, heat cross-linking, obtain humidity-sensitive element 2; To test in pre-polymerization liquid 1, lift plated film with the humidity-sensitive element electrode after, infrared lamp baking 1~3 hour down lifts plated film, heat cross-linking again in pre-polymerization liquid 2, obtain humidity-sensitive element 3.
With said humidity-sensitive element 1, said humidity-sensitive element 2, said humidity-sensitive element 3, be placed on LiCl, CH respectively 3COOK, MgCl 2, K 2CO 3, NaBr, KI, NaCl, KCl, K 2In the saturated salt solution of SO4, the humidity value of this saturated salt solution is respectively 11%RH, 23%RH, 33%RH, 43%RH, 59%RH, 70%RH, 75%RH, 85%RH, 98%RH; After treating that said humidity-sensitive element 1, said humidity-sensitive element 2, said humidity-sensitive element 3 are stable; Adopt the LCR digital electric bridge; Write down respectively humidity-sensitive element by low humidity to the output resistance of high humidity with by the output resistance of high humidity to low humidity, i.e. output resistance under the sucting wet state and the output resistance under the dehumidification state.
Experiment effect:Can know that from Fig. 2, Fig. 3 and Fig. 4 under different humidity, the resistance integral body of said humidity-sensitive element 1 is less than normal, the resistance integral body of said humidity-sensitive element 2 is bigger than normal, and the resistance integral body of said humidity-sensitive element 3 is moderate, and humidity adaptability is strong, stable performance.
DMC solution contains strong polar group-NH4CI, and hydroscopicity is strong, and prepared humidity-sensitive element resistance is less; Si in the silane quaternary ammonium salt-O group has not only played crosslinked effect, and it still is a hydrophobic group simultaneously, is difficult for suction, and prepared humidity-sensitive element resistance is bigger; DMC solution and silane quaternary ammonium salt are combined prepared humidity-sensitive element, when low humidity, steam only with the silane quaternary ammonium salt effect; What show is the character of silane quaternary ammonium salt, and resistance is bigger, when high humidity; Steam gets on the DMC rete, shows the character of DMC solution, and resistance is less; During long-term the placement, DMC solution moisture absorption swelling, ion channel increases, and resistance is tending towards reducing, and the silane quaternary ammonium salt hydroscopicity is poor, and desorption is slow, and conductive ion reduces, and resistance is tending towards increasing, so with the element that two kinds of films combine, the stability of its resistance is tending towards strengthening.
Should be noted that at last: above embodiment is only in order to technical scheme of the present invention to be described but not to its restriction; Although with reference to preferred embodiment the present invention has been carried out detailed explanation, the those of ordinary skill in affiliated field is to be understood that: still can specific embodiments of the invention make amendment or the part technical characterictic is equal to replacement; And not breaking away from the spirit of technical scheme of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention asks for protection.

Claims (4)

1. electric resistance type humidity sensitive element; Comprise the humidity-sensitive element substrate and be arranged on the on-chip humidity-sensitive element electrode of said humidity-sensitive element; It is characterized in that: it also comprises hydrophilic low-resistance humidity-sensitive film and the hydrophobic high resistant humidity-sensitive film that is successively set on the said humidity-sensitive element electrode, and said hydrophilic low-resistance humidity-sensitive film and said hydrophobic high resistant humidity-sensitive film are combined with each other through heat cross-linking technology.
2. the preparation method of the described electric resistance type humidity sensitive element of claim 1 is characterized in that, it may further comprise the steps: step 1, the said humidity-sensitive element electrode of preparation on said humidity-sensitive element substrate; Get 1~3 milliliter of methylacryoyloxyethyl trimethyl ammonium chloride solution, join in 2~4 milliliters the absolute ethyl alcohol, stir, make pre-polymerization liquid 1; In the closed container of anhydrous and oxygen-free, add 3-aminopropyl triethoxysilane, bromination of n-butane, absolute ethyl alcohol successively, under 40~50 ℃ temperature, the water-bath closed container, and carry out magnetic agitation; Then, the flow feeding argon gas with 60~150 ml/min reacts after 20~30 hours; Obtain Polymer Solution, more said Polymer Solution is poured in the excessive absolute ether, obtain white depositions; And, obtain white powder with the vacuum drying at room temperature of said white depositions, last; Get said white powder 1~3 gram, be dissolved in 3.5~6.5 milliliters the absolute ethyl alcohol, make pre-polymerization liquid 2; Step 2, said humidity-sensitive element electrode lifted plated film in pre-polymerization liquid 1 after, infrared lamp baking 1~3 hour down lifts plated film again in pre-polymerization liquid 2, then, in 80~100 ℃ baking oven, carry out heat cross-linking, keeps 6~10 hours, promptly gets electric resistance type humidity sensitive element.
3. the preparation method of electric resistance type humidity sensitive element according to claim 2; It is characterized in that: in step 1; After adopting silk-screen printing technique printed silver slurry conductiving point and interdigital carbon electrode on the said humidity-sensitive element substrate; Adopt the reflow soldering process welding to go up Y type lead-in wire again, prepare said humidity-sensitive element electrode with this.
4. according to the preparation method of claim 2 or 3 described electric resistance type humidity sensitive elements, it is characterized in that: said humidity-sensitive element substrate is an alumina ceramic substrate.
CN201110443212.3A 2011-12-27 2011-12-27 Resistance type humidity element and preparation method thereof Active CN102565146B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103226119A (en) * 2012-12-28 2013-07-31 青岛润鑫伟业科贸有限公司 Humidity-sensitive element
CN105753509A (en) * 2016-02-01 2016-07-13 浙江大学 Humidity sensing ceramic, and preparation method and application thereof
CN107533027A (en) * 2015-02-17 2018-01-02 霍尼韦尔国际公司 Humidity sensor and the method for manufacturing the sensor

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CN1320817A (en) * 2000-03-31 2001-11-07 Tdk株式会社 Moisture sensor and mfg. method thereof
JP3557245B2 (en) * 1994-05-24 2004-08-25 松下電器産業株式会社 Humidity-sensitive element and method of manufacturing the same
US20040244482A1 (en) * 2003-06-03 2004-12-09 General Electric Company Humidity sensor element containing polyphenylsulfone
CN101788520A (en) * 2010-03-16 2010-07-28 浙江大学 Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof
CN202393728U (en) * 2011-12-27 2012-08-22 郑州炜盛电子科技有限公司 Resistor type humidity-sensitive element

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3557245B2 (en) * 1994-05-24 2004-08-25 松下電器産業株式会社 Humidity-sensitive element and method of manufacturing the same
CN1320817A (en) * 2000-03-31 2001-11-07 Tdk株式会社 Moisture sensor and mfg. method thereof
US20040244482A1 (en) * 2003-06-03 2004-12-09 General Electric Company Humidity sensor element containing polyphenylsulfone
CN101788520A (en) * 2010-03-16 2010-07-28 浙江大学 Polyelectrolyte surface acoustic wave resonance type humidity sensitive element containing silicon and manufacture method thereof
CN202393728U (en) * 2011-12-27 2012-08-22 郑州炜盛电子科技有限公司 Resistor type humidity-sensitive element

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103226119A (en) * 2012-12-28 2013-07-31 青岛润鑫伟业科贸有限公司 Humidity-sensitive element
CN107533027A (en) * 2015-02-17 2018-01-02 霍尼韦尔国际公司 Humidity sensor and the method for manufacturing the sensor
CN105753509A (en) * 2016-02-01 2016-07-13 浙江大学 Humidity sensing ceramic, and preparation method and application thereof
CN105753509B (en) * 2016-02-01 2018-08-31 浙江大学 A kind of humiceram and its preparation method and application

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