CN106046244A - Nonelectrolyte macromolecule humidity-sensitive resin, preparation method thereof and conductive ink and humidity-sensitive sensor produced based on nonelectrolyte macromolecule humidity-sensitive resin - Google Patents

Nonelectrolyte macromolecule humidity-sensitive resin, preparation method thereof and conductive ink and humidity-sensitive sensor produced based on nonelectrolyte macromolecule humidity-sensitive resin Download PDF

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CN106046244A
CN106046244A CN201610372727.1A CN201610372727A CN106046244A CN 106046244 A CN106046244 A CN 106046244A CN 201610372727 A CN201610372727 A CN 201610372727A CN 106046244 A CN106046244 A CN 106046244A
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humidity
monomer
sensitive resin
solvent
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CN106046244B (en
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许赵武
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GUANGZHOU HAIGU ELECTRONIC TECHNOLOGY CO LTD
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GUANGZHOU HAIGU ELECTRONIC TECHNOLOGY CO LTD
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
    • C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/10—Esters
    • C08F222/12—Esters of phenols or saturated alcohols
    • C08F222/20—Esters containing oxygen in addition to the carboxy oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
    • C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
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    • C08F220/285—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing a polyether chain in the alcohol moiety
    • C08F220/286—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing a polyether chain in the alcohol moiety and containing polyethylene oxide in the alcohol moiety, e.g. methoxy polyethylene glycol (meth)acrylate
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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/10—Esters
    • C08F222/12—Esters of phenols or saturated alcohols
    • C08F222/20—Esters containing oxygen in addition to the carboxy oxygen
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Abstract

The invention belongs to the technical field of high polymer materials and relates to nonelectrolyte macromolecule humidity-sensitive resin, a preparation method thereof and conductive ink and a humidity-sensitive sensor produced based on the nonelectrolyte macromolecule humidity-sensitive resin. The preparation method of the nonelectrolyte macromolecule humidity-sensitive resin includes: allowing polyethylene glycol monomer and acrylic acid monomer to have first-step reaction in solvent dissolved with catalyst to obtain a hydrophilic compound; allowing the hydrophilic compound and coupling agent, acrylics monomer and/or monomer containing vinyl to have second-step reaction in solvent containing initiator to obtain the humidity-sensitive resin. The humidity-sensitive resin and conductive materials are ground and mixed to produce the conductive ink. The conductive ink is printed on a ceramic substrate containing interdigital electrodes to form a humidity-sensitive film, and accordingly the dewing sensor with extremely good stability in high-temperature and high-humidity environments is produced.

Description

Non-electrolyte family macromolecule wet sensitive resin and preparation method thereof and based on wet sensitive resin-made Standby electrically conductive ink and moisture sensor
Technical field
The present invention relates to technical field of polymer materials, particularly relate to a kind of non-electrolyte family macromolecule wet sensitive resin and Preparation method, and based on the standby electrically conductive ink formed of wet sensitive resin-made and condensation sensor.
Background technology
Humidity sensor is a kind of common tool for testing atmospheric water content, and it can be by the humidity of surveyed environment Signal is converted to the signal of telecommunication being easy to process, show, record, and is a kind of important sensor.Due to conventional humidity sensor Price is prohibitively expensive, so it is simply applied to some special dimensions, as military, meteorological etc..Development and people along with technology Growth in the living standard, present humidity sensor has application in all trades and professions and a lot of life area.Wherein utilize high score It is the most popular field that sub-humidity-sensitive material makes humidity sensor, and resistor-type high molecule humidity sensor is at mesh Front application is especially prevalent, and the substrate of humidity sensor covers one layer of humidity-sensitive film being made up of humidity sensing polymer materials, macromolecule The resistance value difference that the moisture that humidity-sensitive material absorbs under different humidity environment is different and causes, thus utilize this characteristic to examine Survey the moisture in air.
Humidity sensing polymer materials for resistance type humidity sensor generally contains some high scores such as quaternary ammonium salt, sulfonate Sub-electrolyte, its technique is simple, be prone to batch production, cheap, thus is widely applied, but, due to these salt things Matter ran off in hot and humid lower easy decomposition, caused its stability the highest, so, it is applied to resistance with these polyelectrolytes Type humidity sensor can only use in the environment of some are less demanding, it is impossible to meet at hot and humid (70%RH ~ 100% RH)--apply under conditions of dew point.Therefore, it is necessary to prior art is improved.
Summary of the invention
In view of this, it is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of at hot and humid lower environment Under there is the non-electrolyte family macromolecule wet sensitive resin of excellent stability, and based on the standby electrically conductive ink of this wet sensitive resin-made and Condensation sensor.
In order to solve above-mentioned technical problem, the present invention uses following scheme to realize:
The preparation method of a kind of non-electrolyte family macromolecule wet sensitive resin, comprises the steps:
S1: polyethylene glycols monomer and acrylic monomer are carried out esterification in dissolved with the solvent of catalyst, obtains hydrophilic Compound；
The hydrophilic compounds of S2: step S1 and coupling agent, acrylic ester monomer and/or containing vinyl-based monomer containing drawing Send out in the solvent of agent and carry out copolyreaction, obtain wet sensitive resin.
Utilize humidity sensor prepared by electrolytes humidity sensing polymer materials, due to electrolytes humidity sensing polymer materials Conduction ion to be formed, in the environment of hot and humid, be therefore easily caused the loss of ion and the decomposition of material.Therefore originally Invention uses polyethylene glycols monomer and acrylic monomer to carry out esterification so that product is double with reactive carbon carbon Key, then follow the acrylic ester monomer with other specific function and/or carry out copolymerization prepare non-electrical containing vinyl monomer Solve matter wet sensitive resin, in conjunction with conductive material, it is to avoid the problem that ion runs off so that utilize its prepared humidity sensor to exist There is under high humidity environment superior stability and sensitivity.
In step S1:
Described polyethylene glycols monomer is methoxy poly (ethylene glycol) 400, methoxy poly (ethylene glycol) 600, methoxy poly (ethylene glycol) 2000, one or more in PEG400, Macrogol 600, Macrogol 2000；These of present invention selection are The methoxy poly (ethylene glycol) of row and the molecular weight of Polyethylene Glycol are more suitable for reacting with other component so that the resin of preparation Modest viscosity, it is simple to mixing homogeneously and follow-up printing of subsequent conductive material.
Described acrylic monomer is one or both in acrylic acid, methacrylic acid；
In step S1, described solvent is the one in toluene, oxolane, dimethylformamide, dimethyl sulfoxide, dichloroethanes Or it is several；
Described catalyst is one or more in phosphoric acid, concentrated sulphuric acid, p-methyl benzenesulfonic acid.
In step S2:
Described coupling agent is aminopropyl triethoxysilane, glycydoxy trimethoxy silane, methacryl Epoxide propyl trimethoxy silicane, VTES, mercaptopropyl trimethoxysilane, ethylenediamine propyl triethoxy Silane, ethylenediamine hydroxypropyl methyl dimethoxysilane one or more.
The coupling agent that the present invention selects can improve the interface performance with inorganic filler, especially with methacryloxy Propyl trimethoxy silicane, VTES, VTES coordinate other component as coupling agent, Polymer and the caking property of conductive material and breathability can be significantly improved, accelerate resin water suction and dehydration, thus improve condensation The response speed of sensor.
Described acrylic ester monomer be acrylic acid methyl ester., ethyl acrylate, butyl acrylate, Isobutyl 2-propenoate, third Olefin(e) acid n-octyl, Isooctyl acrylate monomer, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate, methyl methacrylate, methacrylic acid second Ester, isopropyl methacrylate, butyl methacrylate, isobutyl methacrylate, 2-Propenoic acid, 2-methyl-, isooctyl ester, metering system Acid hydroxyl ethyl ester, Hydroxypropyl methacrylate, glycidyl methacrylate, allyl glycidyl ether, methacrylic acid are different One or more in norbornene ester；Described is one or both in styrene, vinylacetate containing vinyl monomer.
Methyl methacrylate, ethyl methacrylate, styrene can as hard monomer, give polymer wearability and Thermostability；Butyl acrylate, n-octyl, Isooctyl acrylate monomer, 2-Propenoic acid, 2-methyl-, isooctyl ester are as soft monomer, Ke Yiju Compound improves tolerance to cold；With with the 2-(Acryloyloxy)ethanol of hydroxyl, Hydroxypropyl acrylate, metering system hydroxyl ethyl ester, metering system Acid hydroxypropyl acrylate as function monomer, the sensitivity to water and the adhesive force to base material of polymer can be improved；Use methyl-prop Olefin(e) acid ethylene oxidic ester, allyl glycidyl ether, as internal crosslinker, can improve the thermostability of polymer, resistance to water and resistance to Chemicals.
In step S2, described solvent be methanol, ethanol, isopropanol, n-butyl alcohol, isobutanol, ethyl acetate, butyl acetate, Acetone, butanone, toluene, dimethylbenzene, ethylene glycol monomethyl ether, butyl glycol ether, ethylene glycol phenyl ether, propylene glycol monomethyl ether, propandiol butyl ether, One or more in dimethyl sulfoxide.
Described initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, peroxy dicarbonate diisopropyl One or more in ester, cyclohexanone peroxide, lauroyl peroxide.
Further, in step S1, described polyethylene glycols monomer, acrylic monomer, solvent and catalyst are by weight Part meter is respectively 35 ~ 50 parts, 10 ~ 35 parts, 25 ~ 50 parts, 0.1 ~ 2 part；In step S2, described hydrophilic compounds, coupling agent, propylene Esters of gallic acid monomer and/or containing vinyl monomer, solvent, initiator by weight be respectively 25 ~ 45 parts, 1 ~ 5 part, 15 ~ 25 Part, 25 ~ 50 parts, 0.1 ~ 2 part.
Further, 5 ~ 15h is reacted at step S1 reaction condition is temperature 80 ~ 150 DEG C；Step S2 reaction condition is temperature 5 ~ 25h is reacted at spending 55 ~ 85 DEG C.
Inventor, by substantial amounts of test, is examined or check by different materials, different amounts and different process, finally makes The wet sensitive resin of preparation is applied to during humidity sensor possess superior performance.
A kind of electrically conductive ink, each component mixed grinding including following weight portion forms: the wet sensitive prepared by said method Resin 20 ~ 50 parts, solvent 30 ~ 80 parts and conductive material 10 ~ 20 parts.
Preparing the solvent in electrically conductive ink is methanol, ethanol, isopropanol, n-butyl alcohol, isobutanol, ethyl acetate, acetic acid fourth Ester, acetone, butanone, toluene, dimethylbenzene, ethylene glycol monomethyl ether, butyl glycol ether, ethylene glycol phenyl ether, propylene glycol monomethyl ether, propylene glycol fourth One or more in ether, dimethyl sulfoxide.
Described conductive material is one or more in bronze, argentum powder, copper powder, graphite, white carbon black, carbon fibre, nikel powder.
A kind of condensation sensor, including ceramic substrate, interdigital electrode and humidity-sensitive film, described interdigital electrode is arranged on ceramic base On sheet, described humidity-sensitive film is arranged on the ceramic substrate containing interdigital electrode, and it is formed by above-mentioned electrically conductive ink printing.
Described condensation sensor is prepared via a method which: above-mentioned electrically conductive ink is printed on the pottery with interdigital electrode On substrate, at temperature 120 ~ 150 DEG C, toast 5 ~ 25min form.
Electrically conductive ink is printed on ceramic substrate and forms the humidity sensing film that breathability is strong, and mode of printing can use silk-screen side Formula, thus prepares humidity sensor.Owing to prepared humidity sensor out has well under the conditions of hot and humid Stability, uses under dew point environment mainly for high humidity, therefore referred to as condensation sensor.Condensation prepared by the present invention passes Sensor strengthens along with the rising of air humidity, water absorption, and resistance can become big, and traditional electrolytes humidity sensing polymer materials system Standby moisture sensor, along with the rising of air humidity, water absorption strengthens, and resistance can diminish.Under high humidity, resistance becomes big, resistance The order of magnitude can be bigger, make the change of data become apparent from, it is easier to measure, therefore, the condensation sensor of the present invention is at high humidity The rh value of lower test is more accurate.
Compared with prior art, there is advantages that
1, each component mentioned by the present invention obtains easily, cheap, and the manufacturing process of wet sensitive resin is simple, is suitable for batch raw Produce；
2, the condensation sensor prepared by the present invention, under conditions of high humidity (70%RH ~ 100%RH), have the highest sensitivity, relatively Little humidity hysteresis (less than 1%RH) and quickly response (moisture absorption and dehumidification are all in 20s)；
3, the wet sensitive resin prepared by the present invention is a kind of non-electrolyte family macromolecule, and ion will not occur in the environment of high humidity Run off and the phenomenon of material decomposition so that the condensation sensor of preparation has higher stability under high humidity environment.
Detailed description of the invention
In order to allow those skilled in the art be more fully understood that technical scheme, below the present invention is made further Illustrate.
Embodiment 1
1, the preparation of wet sensitive resin
S1: by mass parts: by polyethylene glycols monomer 35 parts, acrylic monomer 10 parts, solvent 25 parts, catalyst 0.1 part, add Entering in the flask equipped with thermometer, agitator, condenser and water knockout drum, be warming up to 80 DEG C of reaction 5h, reaction distills out after terminating Solvent, the monomer of excess and the moisture of generation, obtain hydrophilic compounds；
Described polyethylene glycols monomer is methoxy poly (ethylene glycol) 400；
Described acrylic monomer is methacrylic acid；
Described solvent is dichloroethanes；
Described catalyst is p-methyl benzenesulfonic acid.
S2: by mass parts: by hydrophilic compounds 25 parts, acrylic ester monomer 15 parts, solvent 25 parts, coupling agent 1 part, draw Send out agent 0.1 part, be equipped with in the flask of thermometer, agitator, condenser and nitrogen protection device, react under the conditions of 55 DEG C 5h, obtains the macromolecule wet sensitive resin of non-electrolyte class, and nitrogen protection can make chemical reaction not by the oxygen in air and moisture Disturbed.；
Described acrylic ester monomer is acrylic acid methyl ester.；
Described solvent is methanol；
Described coupling agent is aminopropyl triethoxysilane；
Described initiator is 2,2'-Azobis(2,4-dimethylvaleronitrile).
2, the preparation of electrically conductive ink:
Above-mentioned wet sensitive resin 10 parts, solvent 30 parts, 10 parts of mix and blends of conductive material are ground；
Described solvent is methanol；
Described conductive material copper powder.
3, the preparation of condensation sensor:
Above-mentioned electrically conductive ink is printed on the ceramic substrate with interdigital electrode by the way of silk-screen, at the drying tunnel of 120 DEG C In, toast 5min, it is thus achieved that the humidity-sensitive film being attached in interdigital electrode, prepare condensation sensor.
4, after tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 0.9%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 9.89S, dehumidification 11.36S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 2
1, the preparation of wet sensitive resin
S1: by mass parts: by polyethylene glycols monomer 50 parts, acrylic monomer 35 parts, solvent 50 parts, catalyst 2 parts, adds In flask equipped with thermometer, agitator, condenser and water knockout drum, being warming up to 150 DEG C of reaction 15h, reaction distills out after terminating Solvent, the monomer of excess and the moisture of generation, obtain hydrophilic compounds；
Described polyethylene glycols monomer is PEG400；
Described acrylic monomer is acrylic acid；
Described solvent is dimethylformamide；
Described catalyst is concentrated sulphuric acid.
S2: by mass parts: by hydrophilic compounds 45 parts, acrylic ester monomer 25 parts, solvent 50 parts, coupling agent 5 parts, draw Send out agent 2 parts, be equipped with in the flask of thermometer, agitator, condenser and nitrogen protection device, react under the conditions of 85 DEG C 25h, obtains the macromolecule wet sensitive resin of non-electrolyte class；
Described acrylic ester monomer is methyl methacrylate；
Described solvent is acetone；
Described coupling agent is methacryloxypropyl trimethoxy silane；
Described initiator is benzoyl peroxide.
2, the preparation of electrically conductive ink:
Above-mentioned wet sensitive resin 50 parts, solvent 80 parts, 20 parts of mix and blends of conductive material are ground；
Described solvent is acetone；
Described conductive material carbon fibre.
3, the preparation of condensation sensor:
Above-mentioned electrically conductive ink is printed on the ceramic substrate with interdigital electrode by the way of silk-screen, at the drying tunnel of 150 DEG C In, toast 25min, it is thus achieved that the humidity-sensitive film being attached in interdigital electrode, prepare condensation sensor.
4, after tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 0.9%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 8.21S, dehumidification 9.45S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 3
1, the preparation of wet sensitive resin
S1: by mass parts: by polyethylene glycols monomer 35 parts, acrylic monomer 10 parts, solvent 25 parts, catalyst 0.1 part, add Entering in the flask equipped with thermometer, agitator, condenser and water knockout drum, be warming up to 110 DEG C of reaction 10h, reaction is distilled after terminating Go out solvent, the monomer of excess and the moisture of generation, obtain hydrophilic compounds；
Described polyethylene glycols monomer is methoxy poly (ethylene glycol) 600, methoxy poly (ethylene glycol) 2000 and Macrogol 600 Mixing, the weight portion of three is respectively 10 parts, 15 parts, 10 parts；
Described acrylic monomer is the mixing of acrylic acid and methacrylic acid, and both weight portions are respectively 3 parts, 7 parts；
Described solvent is dimethylformamide, toluene and oxolane mixing, and the weight portion of three is respectively 10 parts, 8 parts, 7 parts；
Described catalyst is phosphoric acid.
S2: by mass parts: by hydrophilic compounds 25 parts, acrylic ester monomer 15 parts, solvent 25 parts, coupling agent 1 part, draw Send out agent 0.1 part, be equipped with in the flask of thermometer, agitator, condenser and nitrogen protection device, react under the conditions of 70 DEG C 15h, obtains the macromolecule wet sensitive resin of non-electrolyte class；
Described acrylic ester monomer is 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate, glycidyl methacrylate three The mixing of person, the weight portion of three is respectively 3 parts, 7 parts, 5 parts；
Described solvent is the mixing of ethyl acetate, toluene and ethylene glycol monomethyl ether, and the weight portion of three is respectively 15 parts, 5 parts, 5 parts；
Described coupling agent is glycydoxy trimethoxy silane, dredges propyl trimethoxy silicane and ethylenediamine propyl group The mixing of triethoxysilane, the weight portion of three is respectively 0.5 part, 0.2 part, 0.3 part；
Described initiator is azodiisobutyronitrile.
2, the preparation of electrically conductive ink:
Above-mentioned wet sensitive resin 10 parts, solvent 30 parts, 10 parts of mix and blends of conductive material are ground；
Described solvent is the mixing of ethyl acetate, toluene and ethylene glycol monomethyl ether, the weight portion of three be respectively 15 parts, 10 parts, 5 Part；
Described conductive material is the mixing of bronze, graphite and nikel powder, and the weight portion of three is respectively 2 parts, 4 parts, 4 parts.
3, the preparation of condensation sensor:
Above-mentioned electrically conductive ink is printed on the ceramic substrate with interdigital electrode by the way of silk-screen, at the drying tunnel of 135 DEG C In, toast 15min, it is thus achieved that the humidity-sensitive film being attached in interdigital electrode, prepare condensation sensor.
4, after tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 0.8%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 8.58S, dehumidification 9.75S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 4
1, the preparation of wet sensitive resin
S1: by mass parts: by polyethylene glycols monomer 50 parts, acrylic monomer 35 parts, solvent 50 parts, catalyst 2 parts, adds In flask equipped with thermometer, agitator, condenser and water knockout drum, being warming up to 150 DEG C of reaction 15h, reaction distills out after terminating Solvent, the monomer of excess and the moisture of generation, obtain hydrophilic compounds；
Described polyethylene glycols monomer is Macrogol 2000 and the mixing of methoxy poly (ethylene glycol) 600, and both weight portions divide It it is not 30 parts, 20 parts；
Described acrylic monomer is the mixing of acrylic acid and methacrylic acid, and both weight portions are respectively 10 parts, 25 parts；
Described solvent is the mixing of dimethylformamide and dimethyl sulfoxide, and the weight portion of three is respectively 30 parts, 20 parts；
Described catalyst is the mixing of phosphoric acid and p-methyl benzenesulfonic acid, and both weight portions are respectively 1 part, 1 part.
S2: by mass parts: by hydrophilic compounds 45 parts, acrylic ester monomer and containing vinyl monomer 25 parts, solvent 50 parts, coupling agent 5 parts, initiator 2 parts, be equipped with in the flask of thermometer, agitator, condenser and nitrogen protection device, Under the conditions of 85 DEG C, react 25h, obtain the macromolecule wet sensitive resin of non-electrolyte class；
Described acrylic ester monomer and containing vinyl monomer be allyl glycidyl ether, isobornyl methacrylate, Cinnamic mixing, the weight portion of three is respectively 10 parts, 5 parts, 10 parts；
Described solvent is the mixing of ethylene glycol phenyl ether, propandiol butyl ether and dimethyl sulfoxide, the weight portion of three be respectively 15 parts, 20 parts, 15 parts；
Described coupling agent is VTES, the mixing of ethylenediamine hydroxypropyl methyl dimethoxysilane, both weights Amount part is respectively 2 parts, 3 parts；
Described initiator is the mixing of azodiisobutyronitrile, di-isopropyl peroxydicarbonate, and both weight ratios are respectively It it is 0.8 part, 1.2 parts.
2, the preparation of electrically conductive ink:
Above-mentioned wet sensitive resin 50 parts, solvent 80 parts, 20 parts of mix and blends of conductive material are ground；
Described solvent is the mixing of ethylene glycol phenyl ether, propandiol butyl ether and dimethyl sulfoxide, the weight portion of three be respectively 20 parts, 35 parts, 25 parts；
Described conductive material argentum powder and the mixing of white carbon black, both weight portions are respectively 10 parts, 10 parts.
3, the preparation of condensation sensor:
Above-mentioned electrically conductive ink is printed on the ceramic substrate with interdigital electrode by the way of silk-screen, at the drying tunnel of 150 DEG C In, toast 25min, it is thus achieved that the humidity-sensitive film being attached in interdigital electrode, prepare condensation sensor.
4, after tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 0.9%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 9.54S, dehumidification 9.99S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 5
1, the preparation of wet sensitive resin
S1: by mass parts: by polyethylene glycols monomer 40 parts, acrylic monomer 20 parts, solvent 40 parts, catalyst 1 part, adds In flask equipped with thermometer, agitator, condenser and water knockout drum, being warming up to 120 DEG C of reaction 10h, reaction distills out after terminating Solvent, the monomer of excess and the moisture of generation, obtain hydrophilic compounds；
Described polyethylene glycols monomer is methoxy poly (ethylene glycol) 2000；
Described acrylic monomer is methacrylic acid；
Described solvent is the mixing of toluene, dimethylformamide and dichloroethanes, the weight portion of three be respectively 10 parts, 15 parts, 15 parts；
Described catalyst is the mixing of p-methyl benzenesulfonic acid and concentrated sulphuric acid, and both weight portions are respectively 0.4 part, 0.6 part.
S2: by mass parts: by hydrophilic compounds 35 parts, acrylic ester monomer and containing vinyl monomer 20 parts, solvent 40 parts, coupling agent 3 parts, initiator 1 part, be equipped with in the flask of thermometer, agitator, condenser and nitrogen protection device, Under the conditions of 70 DEG C, react 15h, obtain the macromolecule wet sensitive resin of non-electrolyte class；
Described acrylic ester monomer and containing vinyl monomer be Isooctyl acrylate monomer, butyl methacrylate and vinyl acetate The mixing of ester, the weight portion of three is respectively 6 parts, 8 parts, 6 parts；
Described solvent is the mixing of butyl glycol ether, propylene glycol monomethyl ether and butyl acetate, the weight portion of three be respectively 10 parts, 15 Part, 15 parts；
Described coupling agent is ethylenediamine hydroxypropyl methyl dimethoxysilane；
Described initiator is the mixing of lauroyl peroxide and cyclohexanone peroxide, both weight portions be respectively 0.3 part, 0.7 Part.
2, the preparation of electrically conductive ink:
Above-mentioned wet sensitive resin 30 parts, solvent 55 parts, 15 parts of mix and blends of conductive material are ground；
Described solvent is butyl glycol ether, propylene glycol monomethyl ether and the mixing of butyl acetate, the weight portion of three be respectively 15 parts, 25 parts, 15 parts；
Described conductive material argentum powder and the mixing of white carbon black, both weight portions are respectively 5 parts, 10 parts.
3, the preparation of condensation sensor:
Above-mentioned electrically conductive ink is printed on the ceramic substrate with interdigital electrode by the way of silk-screen, at the drying tunnel of 150 DEG C In, toast 25min, it is thus achieved that the humidity-sensitive film being attached in interdigital electrode, prepare condensation sensor.
4, after tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.2%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 10.31S, dehumidification 12.54S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 6
The present embodiment is similar to Example 1, and difference is, polyethylene glycols monomer is methoxy poly (ethylene glycol) 800.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.0%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 10.11S, dehumidification 11.89S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Embodiment 7
The present embodiment is similar to Example 4, and difference is, polyethylene glycols monomer is methoxy poly (ethylene glycol) 1000 and poly-second two The mixing of alcohol 800, both weight portions are respectively 30 parts, 20 parts.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.0%RH；
Temperature coefficient: < 0.3%RH/ DEG C；
Response speed: moisture absorption 9.99S, dehumidification 10.85S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Comparative example 1
This comparative example is similar to Example 1, and difference is, in the preparation process of wet sensitive resin, the reaction condition of step S1 is temperature Reacting 3h at spending 75 DEG C, the reaction condition of step S2 is reaction 3h under temperature 50 C.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.9%RH；
Temperature coefficient: 0.5%RH/ DEG C；
Response speed: moisture absorption 15.96S, dehumidification 18.69S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance substantially diminishes.
Comparative example 2
This comparative example is similar with embodiment 2, and difference is, in the preparation process of wet sensitive resin, the reaction condition of step S1 is Reacting 18h at 160 DEG C, the reaction condition of step S2 is reaction 30h at temperature 95 DEG C.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.3%RH；
Temperature coefficient: 0.5%RH/ DEG C；
Response speed: moisture absorption 12.54S, dehumidification 14.11S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Comparative example 3
This comparative example is similar to Example 3, and difference is, in the preparation process of wet sensitive resin, and the polyethylene glycols list of step S1 Body 35 parts, acrylic monomer 5 parts, solvent 25 parts, catalyst 0.1 part.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 2.0%RH；
Temperature coefficient: 0.5%RH/ DEG C；
Response speed: moisture absorption 18.15S, dehumidification 21.36S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Comparative example 4
This comparative example is similar to Example 4, and difference is, in the preparation process of wet sensitive resin, and the hydrophilic compounds 50 of step S2 Part, acrylic ester monomer and containing vinyl monomer 30 parts, solvent 50 parts, coupling agent 10 parts, initiator 2 parts.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.5%RH；
Temperature coefficient: 0.4%RH/ DEG C；
Response speed: moisture absorption 14.56S, dehumidification 16.89S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance diminishes.
Comparative example 5
This comparative example is similar to Example 5, and difference is, in the preparation process of wet sensitive resin, and the polyethylene glycols list of step S1 Body 35 parts, acrylic monomer 10 parts, solvent 65 parts, catalyst 0.1 part.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.5%RH；
Temperature coefficient: 0.3%RH/ DEG C；
Response speed: moisture absorption 13.11S, dehumidification 14.98S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.
Comparative example 6
This comparative example is similar to Example 1, and difference is, during wet sensitive resin-made is standby, the hydrophilic compounds of step S2 65 parts, Acrylic ester monomer 20 parts, solvent 50 parts, coupling agent 10 parts, initiator 2 parts.
After tested, the performance of condensation sensor is as follows:
Response interval: 70-100%RH, when humidity is less than 70%RH, resistance is had no significant effect by humidity change；
Impedance variation is interval: 103-106Ω；
Humidity hysteresis: 1.3%RH；
Temperature coefficient: 0.3%RH/ DEG C；
Response speed: moisture absorption 10.98S, dehumidification 12.65S；
Accelerated ageing is tested: after placing 96 hours in the environment of 95%RH/40 DEG C, resistance is without significant change.

Claims (10)

1. the preparation method of a non-electrolyte family macromolecule wet sensitive resin, it is characterised in that comprise the steps:
S1: polyethylene glycols monomer and acrylic monomer are carried out esterification in dissolved with the solvent of catalyst, obtains hydrophilic Compound；
S2: by the hydrophilic compounds of step S1 and coupling agent, acrylic ester monomer and/or containing vinyl monomer containing drawing Send out in the solvent of agent and carry out copolyreaction, obtain wet sensitive resin.
The preparation method of non-electrolyte family macromolecule wet sensitive resin the most according to claim 1, it is characterised in that step S1 In,
Described polyethylene glycols monomer is methoxy poly (ethylene glycol) 400, methoxy poly (ethylene glycol) 600, methoxy poly (ethylene glycol) 2000, one or more in PEG400, Macrogol 600, Macrogol 2000；
Described acrylic monomer is one or both in acrylic acid, methacrylic acid；
Described solvent is one or more in toluene, oxolane, dimethylformamide, dimethyl sulfoxide, dichloroethanes；
Described catalyst is one or more in phosphoric acid, concentrated sulphuric acid, p-methyl benzenesulfonic acid.
The preparation method of non-electrolyte family macromolecule wet sensitive resin the most according to claim 2, it is characterised in that step S2 In,
Described coupling agent is aminopropyl triethoxysilane, glycydoxy trimethoxy silane, methacryl Epoxide propyl trimethoxy silicane, VTES, mercaptopropyl trimethoxysilane, ethylenediamine propyl triethoxy Silane, ethylenediamine hydroxypropyl methyl dimethoxysilane one or more；
Described acrylic ester monomer is acrylic acid methyl ester., ethyl acrylate, butyl acrylate, Isobutyl 2-propenoate, acrylic acid N-octyl, Isooctyl acrylate monomer, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate, methyl methacrylate, ethyl methacrylate, Isopropyl methacrylate, butyl methacrylate, isobutyl methacrylate, 2-Propenoic acid, 2-methyl-, isooctyl ester, methacrylic acid The different ice of hydroxyl ethyl ester, Hydroxypropyl methacrylate, glycidyl methacrylate, allyl glycidyl ether, methacrylic acid One or more in sheet ester；
Described is one or both in styrene, vinylacetate containing vinyl monomer；
Described solvent is methanol, ethanol, isopropanol, n-butyl alcohol, isobutanol, ethyl acetate, butyl acetate, acetone, butanone, first In benzene, dimethylbenzene, ethylene glycol monomethyl ether, butyl glycol ether, ethylene glycol phenyl ether, propylene glycol monomethyl ether, propandiol butyl ether, dimethyl sulfoxide One or more；
Described initiator be azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, di-isopropyl peroxydicarbonate, One or more in cyclohexanone peroxide, lauroyl peroxide.
The preparation method of non-electrolyte family macromolecule wet sensitive resin the most according to claim 3, it is characterised in that step S1 In, described polyethylene glycols monomer, acrylic monomer, solvent and catalyst by weight be respectively 35 ~ 50 parts, 10 ~ 35 Part, 25 ~ 50 parts, 0.1 ~ 2 part；In step S2, described hydrophilic compounds, coupling agent, acrylic ester monomer and/or containing vinyl Class monomer, solvent, initiator are respectively 25 ~ 45 parts, 1 ~ 5 part, 15 ~ 25 parts, 25 ~ 50 parts, 0.1 ~ 2 part by weight.
5., according to the preparation method of the non-electrolyte family macromolecule wet sensitive resin described in any one of Claims 1-4, its feature exists In, step S1 reaction condition is reaction 5 ~ 15h at temperature 80 ~ 150 DEG C；Step S2 reaction condition is to react 5 at temperature 55 ~ 85 DEG C ~25h。
6. the wet sensitive resin using method described in any one of claim 1 to 5 to prepare.
7. an electrically conductive ink, it is characterised in that include that each component mixed grinding of following weight portion forms: claim 1 to 5 Wet sensitive resin prepared by method described in any one 10 ~ 50 parts, solvent 30 ~ 80 parts and conductive material 10 ~ 20 parts.
Electrically conductive ink the most according to claim 7, it is characterised in that described solvent is methanol, ethanol, isopropanol, positive fourth Alcohol, isobutanol, ethyl acetate, butyl acetate, acetone, butanone, toluene, dimethylbenzene, ethylene glycol monomethyl ether, butyl glycol ether, second two One or more in alcohol phenylate, propylene glycol monomethyl ether, propandiol butyl ether, dimethyl sulfoxide.
Electrically conductive ink the most according to claim 7, it is characterised in that described conductive material is bronze, argentum powder, copper powder, stone One or more in ink, white carbon black, carbon fibre, nikel powder.
10. a condensation sensor, it is characterised in that include that ceramic substrate, interdigital electrode and humidity-sensitive film, described interdigital electrode set Putting on a ceramic substrate, described humidity-sensitive film is arranged on the ceramic substrate containing interdigital electrode, and it is arbitrary by claim 7 to 9 Electrically conductive ink printing described in Xiang forms.
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