CN109490380A - Humidity sensor and its preparation method of application, equipment and humidity sensor - Google Patents
Humidity sensor and its preparation method of application, equipment and humidity sensor Download PDFInfo
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- CN109490380A CN109490380A CN201811614121.XA CN201811614121A CN109490380A CN 109490380 A CN109490380 A CN 109490380A CN 201811614121 A CN201811614121 A CN 201811614121A CN 109490380 A CN109490380 A CN 109490380A
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- 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
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- 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
- G01N27/125—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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Abstract
The present invention provides the preparation method of a kind of humidity sensor and its application, equipment and humidity sensor, the humidity sensor includes gel, the gel includes polymer network, the solvent that the gel is collectively formed in conjunction with the polymer network and the electrolytic salt being dissolved in the solvent, and the polymer network has for the functional group with water molecules.
Description
Technical field
The present invention relates to sensor technical fields, more particularly to a kind of humidity sensor and its application, equipment and humidity
The preparation method of sensor.
Background technique
Flexible extensible sensor can closely be attached to the curved surface with labyrinth, for example, human body, robot or
Various information are obtained on the skin of artificial limb, it is therefore, multiple in electronic skin, wearable electronics and health medical treatment etc. in recent years
Field shows wide application prospect.It is desirable to the flexible sensors for being attached to above human skin can be as the skin of people
Has the function of scalable and selfreparing.Tensility can allow the skin of flexible sensor and people to move together, and such people is just
It will not feel well.Self-healing properties can be certainly when being ruptured, scratching or go beyond the limit of deformation range by electronic device
I repairs its electricity, machinery and other performance, to extend the service life of device.Flexible extensible humidity sensor is in health medical treatment
It is widely used demand with fields such as environmental monitorings.For example, flexible humidity sensor, which is attached to above human skin, to be surveyed
The humidity of human skin is measured, to evaluate the physiological health feature of human body, the effect of metabolic condition or skin care item.By measuring wound
The humidity at place can obtain the information of wound healing.Humidity sensor can also be used to the respiratory rate of measurement human body, and detection sleep is exhaled
Inhale the diseases such as interruption.
Traditional humidity-sensitive material includes graphene, MoS2, carbon nano-sized carbon (CNTs), porous ceramics and conducting polymer etc.,
Their tensility can be poor.The flexibility reported at present/stretchable humidity sensor is all by these traditional humidity-sensitive materials
It is integrated into above flexible/stretchable substrate by structure process regulation, to realize flexible/stretchable function.But this side
Method technical process is very complicated, and cannot or can only realize very limited extensibility.The humidity sensor reported at present is most
Big elongation strain is only 60%.Therefore how by simple preparation method obtain stretchable humidity sensor be we urgently
It solves the problems, such as.
Summary of the invention
Based on this, it is necessary to provide the preparation method of a kind of humidity sensor and its application, equipment and humidity sensor.
The present invention provides a kind of humidity sensor, including gel, and the gel includes polymer network and the polymer
The electrolytic salt that network integration is collectively formed the solvent of the gel and is dissolved in the solvent.
The polymer network has functional group in one of the embodiments, for forming hydrogen with water molecules
Key.
The functional group is hydrophilic radical in one of the embodiments, and the functional group includes-NH2、SO3 -With-
At least one of OH preferably includes-NH2、SO3 -With-OH.
The solvent includes water in one of the embodiments, and including or do not include organic solvent, it is described organic molten
Agent is preferably the small molecule polyol that carbon atom number is 1~10, more preferably at least one of glycerine and ethylene glycol.
The gel is dual network gel, including first polymer network and the second polymerization in one of the embodiments,
Object network.
The first polymer network is for coating the solvent, the second polymer in one of the embodiments,
Network is used to enhance the mechanical strength of the gel, it is preferred that the first polymer network and the second polymer network
Mass ratio be 16:1~1.3:1, it is preferred that the first polymer network be polyacrylamide, the second polymer net
Network is carragheen.
The electrolytic salt includes at least one of potassium chloride, calcium chloride, sodium chloride in one of the embodiments,
Preferably calcium chloride.
The gel has the transparency in one of the embodiments, and the elongation strain of the gel is greater than 1200%.
It in one of the embodiments, further include electrode, the electrode is able to reflect the electrolytic salt for measurement and exists
The parameter of ion mobility in the gel, it is preferred that the parameter be the electrolytic salt ionic conductivity or from
The resistance of sub- resistivity or the gel.
In one of the embodiments, further include the detection device of the parameter, is electrically connected with the electrode, for passing through
Parameter described in the electrode measurement.
The present invention also provides the application of the humidity sensor described in one kind, the humidity sensor is for passing through the electrolysis
Matter salt relative humidity variations in the variation detection environment of the ion mobility in the gel.
The hydrone can pass through hydrogen bond knot with the functional group of the polymer network in one of the embodiments,
It closes.
The present invention also provides a kind of equipment, the equipment is wearable humidity sensing device, humidity electronic skin, people
Machine interface, flexible robot or Medical Devices, the equipment include the humidity sensor.
The equipment further includes flexible substrates and/or prompting device, the humidity sensor layer in one of the embodiments,
It is folded to be arranged on the flexible substrates surface, when the humidity sensor senses relative humidity above or below range of set value
The prompting device issues prompt.
The present invention also provides a kind of preparation methods of humidity sensor, include the following steps:
Monomer, crosslinking agent, initiator, second polymer, electrolytic salt and solvent are uniformly mixed in a heated condition,
Mixed solution is obtained, the monomer, the crosslinking agent and the initiator are used to form first polymer network, and described second is poly-
Gel can be formed with the solvent by closing object；
Make the monomer, the crosslinking agent and the initiator crosslink polymerization reaction in the mixed solution to be formed
The first polymer network, is then cooled into second polymer network, obtains the gel.
It further include that the gel is placed in organic solvent to soak in one of the embodiments, when the solvent is water
Bubble, the organic solvent is preferably the small molecule polyol that carbon atom number is 1~10, more preferably in glycerine and ethylene glycol
It is at least one.
Humidity sensor provided by the invention makes Water Molecular Adsorption and is dissolved in the solvent of gel using gel characteristic,
The concentration of polymer is influenced, and the variation of polymer concentration influences the migration of the zwitterion of electrolytic salt in gel, to produce
Raw electrical signal forms response of the gel to humidity.Using gel as humidity sensor, can make sensor have it is excellent can
Draftability and flexibility can be widely used in wearable device.
Detailed description of the invention
Fig. 1 a is the one pot process process schematic of dual network of embodiment of the present invention gel；
Fig. 1 b is functional group adsorbed water molecule schematic diagram in dual network of embodiment of the present invention gel；
Fig. 2 is that glycerine, ethylene glycol and calcium chloride and water molecules are illustrated in dual network of embodiment of the present invention gel
Figure；
Fig. 3 is dual network of embodiment of the present invention gel as the charge of humidity sensor and transmits schematic diagram；
Fig. 4 is the flexibility and tensile properties test chart of dual network of embodiment of the present invention gel；
Fig. 5 is the cryoprotective effects test chart after -18 DEG C of cryo-conservations of dual network of embodiment of the present invention gel；
Fig. 6 is the self-healing properties test chart of dual network of embodiment of the present invention gel；
Fig. 7 is the optical transmittance test data figure of dual network of embodiment of the present invention gel；
Fig. 8 a is for dual network of embodiment of the present invention gel as humidity sensor to humidity dynamic response curve；
Fig. 8 b is that the dual network gel of glycerine of embodiment of the present invention modification is rung as humidity sensor real-time monitoring humidity
Answer curve；
Fig. 8 c is dual network of embodiment of the present invention gel as humidity sensor and responds linear matched curve to humidity；
Fig. 8 d is that the dual network gel of glycerine of embodiment of the present invention modification is wet as humidity sensor detection human body respiration
Spend response test figure；
Fig. 8 e is test of the dual network gel of glycerine of embodiment of the present invention modification as humidity sensor a cycle
Middle response time and recovery time test curve；
Fig. 8 f is the dual network gel of glycerine of embodiment of the present invention modification as one month by a definite date people of humidity sensor
Body breathes Humidity Detection response test figure；
It in relative humidity is 65% that Fig. 9 a, which is dual network of embodiment of the present invention gel, and temperature is mass loss in 25 DEG C of environment
Versus time curve；
It in relative humidity is 55% that Fig. 9 b, which is dual network of embodiment of the present invention gel, and temperature is mass loss in 40 DEG C of environment
Versus time curve；
Fig. 9 c is dual network of embodiment of the present invention gel in relative humidity 37%, temperature be in 60 DEG C of environment mass loss with
The change curve of time；
It in relative humidity is 65% that Fig. 9 d, which is dual network of embodiment of the present invention gel, and temperature is relative resistance in 25 DEG C of environment
Versus time curve；
It in relative humidity is 55% that Fig. 9 e, which is dual network of embodiment of the present invention gel, and temperature is relative resistance in 40 DEG C of environment
Versus time curve；
Fig. 9 f is dual network of embodiment of the present invention gel in relative humidity 37%, temperature be in 60 DEG C of environment relative resistance with
The change curve of time.
Wherein, drawing reference numeral are as follows: N, N '-methylene-bisacrylamide 1, chlorination calcium ion 2, acrylamide monomer 3, OK a karaoke club
Glue 4, polyacrylamide polymers network 5, carragheen network 6, hydrogen bond 7, hydrone 8, glycerol molecule 9, glycol molecule 10,
Electrode 11.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, by the following examples, it and combines attached
Figure, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only to explain this hair
It is bright, it is not intended to limit the present invention.
The embodiment of the present invention provides a kind of humidity sensor, including gel, the gel include polymer network, with it is described
Polymer network is in conjunction with the solvent that the gel is collectively formed and the electrolytic salt being dissolved in the solvent, the polymer
Network has for the functional group with water molecules.
Humidity sensor provided in an embodiment of the present invention can make Water Molecular Adsorption and be dissolved in when humidity is larger in environment
In the solvent of gel, the concentration of diluted electrolyte salt and polymer in a solvent declines the concentration of polymer, thus to dissolution
The inhibition of the zwitterion migration of electrolytic salt in a solvent reduces, and increases Ion transfer speed, and when in environment
Humidity becomes smaller, hydrone De contamination, increases the concentration of polymer, increases the inhibition of Ion transfer, Ion transfer speed
Degree reduces, and the variation of Ion transfer speed can be reflected by the conductance or resistance of gel, to form gel to the sound of humidity
It answers.Using gel as humidity sensor, sensor can be made to have excellent tensility and flexibility, can be widely used in wearing
It wears in device.
The polymer network can have for the functional group with water molecules, keep hydrone easier described
Gel adsorption simultaneously enters in the solvent.Further, the polymer network may act as solid matrix, to limit the electrolyte
Salt ion and the solvent, instead of container required for ionic liquid or liquid metal conductor.
The functional group is hydrophilic radical, and the functional group preferably includes-NH2, SO3 -At least one of with-OH,
It more preferably include-NH2, SO3 -With-the OH ,-NH2、SO3 -With-OH hydrogen bond can be formed with water molecules.It is appreciated that wet
Whether the sensitivity and hydrone for spending sensor can comparatively fast enter the solvent when humidity increase in external environment, and outside
It is related comparatively fast to deviate from the solvent when humidity declines in portion's environment.Utilize-OH, SO3 -、-NH2Can with hydrone formed hydrogen bond from
And and water molecules, promote the quick adsorption of hydrone and enter in the solvent, and the binding force that hydrogen bond provides is relatively
Weak, the water molecule energy when relative humidity declines in external environment in solvent is desorbed rapidly, keeps humidity sensor with higher
Sensitivity.
The solvent forms zwitterion for dissolving the electrolytic salt.Preferably, the solvent includes water, described
Gel is hydrogel.The solvent may also include or not include organic solvent, in one embodiment, in order to solve in hydrogel
The problem of moisture content easily evaporates and tends to be dry, and the draftability, electric conductivity and stability of the humidity sensor is caused to decline, it is described
Solvent further includes organic solvent, and the organic solvent is preferably hygroscopicity small molecule polyol, more preferably glycerine and second two
At least one of alcohol.The organic solvent may be selected to be the alcohols solvent that can be improved gel water-retaining property, such as C atomicity is
1~10 hygroscopicity small molecule polyol solves the problems, such as that moisture is evaporable in gel, while can be improved the high temperature resistant of gel
Property, additionally it is possible to the freezing point of solvent is reduced, the frost resistance of gel is improved, enables sensor normal work in wider temperature range
Make.In one embodiment, the organic solvent is at least one of glycerine and ethylene glycol, glycerine and/or ethylene glycol with
The freezing point of the mixed solution of water can reach negative temperature, and the anti-freezing property of the gel can be improved.Further, the small molecule is polynary
Alcoholic solvent contains multiple-OH groups, can form hydrogen bond with hydrone, promote the absorption of hydrone, further increase to wet
Spend the sensitivity of detection.And the organic solvent will not reduce the mechanical deformation ability of the gel.
The gel can have the elongation strain of superelevation, and the elongation strain of the gel can be more than 1200%, real one
It applies in example, up to 1225%, draftability is best stretchable wet of the draftability reported at present for the elongation strain of the gel
Spend 20.4 times of sensor (elongation strain 60%).
The gel can have the transparency, it is preferred that the gel is more than 60% in the optical transmittance of visible light wave range.
Humidity sensor with clear gel for example may be mounted on display screen or window, form transparent humidity sensor layer.
The gel can have porosity, can be more advantageous to the absorption of hydrone.It in one embodiment, can be described solidifying
Pore former is added in the forming process of the polymer network of glue and forms uniform micro, improves the porosity of gel.
In order to enhance the mechanical strength of gel, the scalability and service life of gel are improved, it is preferred that the gel is
Dual network gel, including first polymer network and second polymer network.First polymer network and second polymer network
It can uniformly mix.
The first polymer network and the second polymer network have different physical properties.The first polymer
Network may be selected to be the polymer that gel can be formed with solvent, form gel, second polymerization for coating the solvent
Object network is evenly distributed in the gel, for enhancing the mechanical strength of the gel.The second polymer network is preferred
For polymer molecule network flexible, making the gel integrally has preferable flexible and elasticity.
The second polymer network can be the network structure being physical crosslinking by ionic bond, such as can be selected from OK a karaoke club
One of glue, chondroitin sulfate, gelatin, alginate are a variety of.
The first polymer network can be the high molecular polymer network structure being chemically crosslinked by covalent bond, described
First polymer network can be selected from one of polyacrylamide, polyaniline, polyvinylamine or a variety of.The first polymer net
Network is reacted to obtain by monomer, crosslinking agent, initiator by polymerization crosslinking.
The polymer network is sacrificial since the expansion of polymer chain, the ionomer of the second polymer network provide
Domestic animal key can be realized effective energy dissipation, increase the expansion and contraction of the gel.
The first polymer network and/or second polymer network can have the functional group, preferred real
It applies in example, the first polymer network and the second polymer network are respectively provided with different functional groups, such as distinguish
With-NH2、SO3 -With it is one or more in-OH.Due to the presence of the functional group, the first polymer network and described
Second polymer network can be combined between the two by the effect of hydrogen bond.
The electrolytic salt may include at least one of potassium chloride, calcium chloride, sodium chloride, preferably calcium chloride.Chlorination
Calcium can form hydrate with water molecules, further promote the absorption of hydrone, can improve the sensitivity of humidity sensor
The water-retaining property of humidity sensor can be improved again.
Referring to Fig. 1, as shown in Figure 1a, the first polymer network is polyacrylamide 5, described in implementing one
Second polymer network is carragheen network 6.Electrolytic salt is calcium chloride 2.Solvent is water or water and ethylene glycol and/or the third three
The combination of alcohol.The polyacrylamide 5 is being caused by monomeric acrylamide 3 and crosslinking agent N, N '-methylene-bisacrylamide 1
Cross-linked polymeric obtains under the action of agent.Acrylamide 3, N, N '-methylene-bisacrylamide 1, carragheen 4, calcium chloride 2 and initiation
Agent is evenly heated mixing in water, and first polymerization forms polyacrylamide 5, and then cooling forms carragheen network 6, with solvent, molten
Dual network gel is collectively formed in solution calcium chloride 2 in a solvent and polyacrylamide 5.The polyacrylamide 5 and the OK a karaoke club
The mass ratio of glue 4 is preferably 16:1~1.3:1, more preferably 5:1~3:1.In the embodiment, the dual network gel contains simultaneously
There is a large amount of-NH2、SO3 -With-OH functional group, can be combined to form a large amount of hydrogen bonds 7 with hydrone 8, as shown in Figure 1 b, for wet
The sensitivity for spending response is very high.
Due to the double-spiral structure of the carragheen and the polymer molecular chain of the polyacrylamide, in the drawing of gel
The sacrifice key that the expansion of polymer chain, carragheen double helix provide during stretching can be realized effective energy dissipation, make gel
With better elongation strain, it is able to bear the deformation such as a greater degree of stretch bending.The polyacrylamide and institute simultaneously
Hydrogen bond can also be formed by stating between carragheen, made to be formed between the first polymer network and the second polymer network and cooperateed with
Effect, during gel tensile deformation, hydrogen bond, which is dynamically broken and recombinates, promotes energy dissipation, further enhances described solidifying
The elongation strain of glue.
In one embodiment, when solvent be water, can be further by obtained hydrogel in organic solvent, such as ethylene glycol
And/or be soaked for a period of time in glycerine, there are concentration differences between hydrone and ethylene glycol and/or glycerine, cause molecule
Diffusion makes ethylene glycol and/or glycerine replace part water, there are three types of the water of form in hydrogel, " Free water ", " intermediate water " with
And " strong bound form water "." Free water " can freely replace not in conjunction with polymer network with ethylene glycol and/or glycerine；It is " intermediate
Water " is loosely combined by hydrogen bond with polymer network, can slowly be replaced with ethylene glycol and/or glycerine；" strong bound form water " then
It is not easy to be replaced.Referring to Fig. 2, replacing the glycerol molecule 9 of aqueous solvent and/or glycol molecule 10 that there are a large amount of-OH, it is easy to
It is combined with hydrone 8, improves the water-retaining property of gel, and make sensor that there is wider operating temperature range.
Due to foring a large amount of hydrogen bonds between the polyacrylamide and the carragheen, hydrogen bond can easily give birth to again
At, therefore can also selfreparing after gel fracture.After gel fracture, a large amount of hydrogen bonds can will be described on plane of disruption surface
Gel both ends are sticky again, and selfreparing can be realized at room temperature.It is described organic in addition to a large amount of hydrogen bonds between polymer chain
Solvent ethylene glycol and glycerol molecule can also form a large amount of hydrogen bonds with the polyacrylamide or the carragheen, therefore in solvent
It can further improve the self-reparing capability of the gel comprising ethylene glycol and/or glycerine.Further, in a heated condition,
When heating sol-gel transition temperature, the dissociation of first polymer network polymer carragheen double-spiral structure can be made to become single
Chain, the single-stranded double-spiral structure that reassembles into of the carragheen of interface repairs bursting surface after cooling, therefore in a heated condition can be more
Further increase the selfreparing effect of gel.The ability of gel selfreparing also can be improved in the addition of ionic electrolyte salt simultaneously.
The humidity sensor senses external environment by ion mobility of the electrolytic salt in the gel
In humidity.In one embodiment, the humidity sensor further includes electrode, and the electrode is able to reflect the electricity for measuring
The parameter for solving ion mobility of the matter salt in the gel, preferably measure the electrolytic salt in the gel from
The resistance of electron conductivity or ion resistivity or the gel.The electrode can be sheet metal, metallic film or conductive paste
Material, such as Copper thin film, aluminium film, silver paste, aluminium paste, carbon slurry.Two electrodes can be separately positioned on the both ends of the gel.
The humidity sensor may also include detection device, and the detection device is electrically connected with described two electrodes respectively,
For the ionic conductivity or ion resistivity by electrolytic salt described in the electrode measurement in the gel.
The embodiment of the present invention also provides a kind of application of humidity sensor, and the humidity sensor is used for by described
Humidity variation of the electrolytic salt in the variation detection environment of the ionic conductivity in the gel.Entered by hydrone or is deviate from
The concentration variation of electrolytic salt caused by solvent in gel in a solvent will affect the speed of the ionic electrolyte salt migration,
That is ionic conductivity or ion resistivity.Referring to Fig. 3, the zwitterion of electrolytic salt moves between two electrodes 11, when
When ambient humidity increases, Water Molecular Adsorption is simultaneously dissolved in hydrogel, declines the concentration of high molecular polymer, thus to ion
The inhibition of migration reduces, and increases ionic mobility, and electric current increases.When ambient humidity reduces, hydrone evaporation is detached from
Hydrogel increases the concentration of polymer, so that the inhibition to Ion transfer increases, reduces ionic mobility, electric current
Reduce.Absorption and desorption are reversible process.
Resistance R=ρ the * L/A, R, ρ, L, A of gel described in the humidity sensor are respectively the resistance of gel, resistance
Rate, length and cross-sectional area.The resistance of the gel is determined by resistivity or conductivity, when the zwitterion of the electrolytic salt
Migration rate changes in the gel, and the resistance of the gel entirety also changes therewith.Therefore, the humidity sensor
It can be changed by measuring the humidity of the gel resistance or conductance changed in detection environment.
The embodiment of the present invention also provides a kind of equipment using the humidity sensor, such as wearable humidity dress
It sets, humidity electronic skin, man-machine interface, flexible robot or Medical Devices.
The humidity sensor that the equipment may also include flexible substrates and be layered in the flexible substrates surface.It is described
Equipment may also include prompting device, when the humidity sensor senses in environment relative humidity above or below the setting value model
The prompting device issues prompt when enclosing.
The humidity sensor cannot be only used for the humidity in monitoring environment to improve the health and comfort level of living environment,
It can also be used to monitor human body respiration (breathing is human health care and movable closely related important physiological signal), human skin humidity
Humidity (the healing shape of wound of (humidity level of skin includes a large amount of valuable physiology and metabolic information) and wound circumference
Condition can be assessed by monitoring the humidity level of wound circumference) etc. various physiologic informations, monitoring the health status of human body.
The humidity sensor combines draftability, the transparency and self-repairability, has widened flexible and wearable electronic device
The application range of part.Its draftability can be such that sensor is attached on human skin, and with the smallest interference and human body one
Movement is played, such as the humidity electronic skin can be placed directly against real-time monitoring human health status or environment on human skin
Middle humidity variation is to remind.It is important that its transparency has it in consumer electronics, military affairs, display and new energy equipment
Meaning.Its self-repairability be automatically repaired electronic device can after surface scratching and mechanical damage, significantly extend
Service life.
After the gel can be mixed by the polymer that will form gel with the solvent heating for being dissolved with electrolytic salt
Cooling down obtains.Other functional components, such as first polymer net can be added into mixed system in a heated condition
Network or the raw material for being used to form first polymer network, make the component of the addition uniform during being cooled into gel
Be compounded in gel.It can also further be replaced, be changed solidifying with other solvents and original solvent after forming gel
Solvent composition in glue.Such as replaced using glycerine or ethylene glycol, obtain the dual network of glycerine or ethylene glycol modification
Gel.
For the dual network gel, the embodiment of the present invention also provides a kind of preparation method of humidity sensor, packet
Include following steps:
S10 mixes monomer, crosslinking agent, initiator, second polymer, electrolytic salt and solvent in a heated condition
Uniformly, mixed solution is obtained, the monomer, the crosslinking agent and the initiator are used to form first polymer network, described
Second polymer can form gel with the solvent；
S20 makes the monomer, the crosslinking agent and the initiator crosslink polymerization reaction in the mixed solution
Form the first polymer network, it is then cooling that the second polymer is made to form second polymer network, and with it is described molten
Dosage form is at the gel.
In step S10, the monomer for forming first polymer network forms polymerizeing for second polymer network with described
The mass ratio of object is preferably 16:1~1.3:1.It is furthermore preferred that the monomer for forming first polymer network and described forming the
The mass ratio of the polymer of dimerization polymeric network is 5:1.
In step S10, it is preferred that first make the monomer, crosslinking agent, second polymer and electrolytic salt 75 DEG C~
100 DEG C uniformly then mixing, dissolving electrolyte salt are cooled to 60 DEG C~75 DEG C, the initiator are added, in the solvent
It is even to be mixed to get the mixed solution.
In step S20, the monomer, the crosslinking agent and the initiator, can be with according to the difference of initiator type
Cross-linking polymerization occurs under illumination or heating condition and forms the first polymer network.
In one embodiment, it can be heated under air-proof condition, temperature is preferably 80 DEG C~105 DEG C.Described in formation
Solution is cooled to 0 DEG C~10 DEG C formation gels after first polymer network.
When the solvent is water, the preparation method of the humidity sensor can also include step S30, by the gel
It is placed in the organic solvent and impregnates, replace the part water in gel by organic solvent.The time of the immersion is preferably 1 small
When~12 hours.The organic solvent is preferably the small molecule polyol that carbon atom number is 1~10, more preferably glycerine and second
At least one of glycol.
Embodiment 1
S10, by 4g acrylamide powder, 0.8g carragheen powder, 0.1g calcium chloride powder and 0.003gN, N '-methylene
Bisacrylamide powder is in 50mL deionized water, and magnetic agitation is to uniform at 75 DEG C；It is cooled to 60 DEG C of addition 0.02g over cures again
Sour ammonium is uniform with magnetic agitation, obtains mixed solution；
Mixed solution is placed in baking oven sealing at 95 DEG C and reacts 1~2 hour to form polyacrylamide network by S20, then
It is placed under 4 DEG C of low temperature environments and reacts 1~2 hour to form carragheen network, it is solidifying to obtain polyacrylamide/carragheen dual network
Glue.
Embodiment 2
S10, by 4g acrylamide powder, 0.8g carragheen powder, 0.1g calcium chloride powder and 0.003gN, N '-methylene
Bisacrylamide powder is in 50mL deionized water, and magnetic agitation is to uniform at 75 DEG C；It is cooled to 60 DEG C of addition 0.02g over cures again
Sour ammonium is uniform with magnetic agitation, obtains mixed solution；
Mixed solution is placed in baking oven sealing at 95 DEG C and reacts 1~2 hour to form polyacrylamide network by S20, then
It is placed under 4 DEG C of low temperature environments and reacts 1~2 hour to form carragheen network, it is solidifying to obtain polyacrylamide/carragheen dual network
Glue；
Polyacrylamide/carragheen dual network gel is placed in 100% ethylene glycol and impregnates 1 hour by S30, obtains second
The double-network hydrogel of glycol modification.
Embodiment 3
It is essentially identical with 2 preparation method of embodiment, the difference is that, 100% ethylene glycol solution replaces in S30
100% glycerin solution.
Embodiment 4
It is essentially identical with 2 preparation method of embodiment, the difference is that, 100% ethylene glycol solution replaces in S30
20% ethylene glycol solution.
Embodiment 5
It is essentially identical with 2 preparation method of embodiment, the difference is that, 100% ethylene glycol solution replaces in S30
20% glycerin solution.
Experimental example
1, the flexibility and draftability of gel
Referring to Fig. 4, double nets of dual network gel (in Fig. 4 a shown in DN) and embodiment 2 preparation prepared by embodiment 1
Network gel (in Fig. 4 a shown in EG-DN, marking colored dyestuff) places 50 hours very in 40 DEG C, the environment that relative humidity is 55%
To the longer time, observe that apparent volume contraction occurs in dual network gel prepared by embodiment 1, and second prepared by embodiment 2
Complete (such as Fig. 4 a) is still kept behind dual network gel 50 hours of glycol modification, then modifies the ethylene glycol placed 50 hours
Dual network gel distorted, is bent, stretching experiment, and distortion is still up to 540 °, bending up to 155 ° (as shown in Figure 4 b).Embodiment
The elongation strain of the dual network gel of 2 preparations can reach for 1225% (as illustrated in fig. 4 c), illustrate dual network prepared by the present invention
Gel has excellent flexibility and elongation strain, while the water-retaining property of gel can be improved for organic solvent ethylene glycol and stretching is answered
Denaturation.
2, influence of the solvent to gel frost resistance
After keeping the temperature 1 hour in the environment of dual network gel prepared by Examples 1 to 5 is placed on -18 DEG C, as shown in figure 5,
It was found that the gel (in Fig. 5 shown in 1#) taken water as a solvent freezes completely, does not have tensility, but contain second in solvent
Gel does not freeze not only the gel (in Fig. 5 shown in 2#~5#) of glycol or glycerine under the same conditions, and can occur
500% tensile deformation and it is not broken.This shows can be by the freezing point much lower of gel comprising ethylene glycol or glycerine in solvent
To 0 DEG C hereinafter, the frost resistance of gel can be increased substantially.
3, self-repairability
The self-repairability of the gel can be assessed by serving as conducting wire come small bulbs in lighting circuit.Referring to Fig. 6,
It is cut off with the dual network gel that pocket knife prepares embodiment 2, the experimental results showed that gel is led before being cut off gel with pocket knife
After electric (as shown in Figure 6 a) becomes non-conductive (not shown), but will be cut into two sections gel after being cut into two sections docks
Heating makes to have restored electric conductivity (as shown in Figure 6 b) again after gel selfreparing, further draws the gel after selfreparing
It stretches, the gel still has biggish elongation strain (as fig. 6 c), but stretching causes resistance to become larger, and selfreparing cannot
Reach 100%.
4, transparent
Referring to Fig. 7, the optical transmittance of the double-network hydrogel visible light wave range of Examples 1 to 3 preparation all has height
Optical transmittance, it is still high-visible in the background patterns of gel overlay region " Zhongshan University " printed words.
5, Unordered system
There is the humidity sensor of bipolar electrode chemical resistance structure using the dual network gel preparation of Examples 1 to 5 preparation,
It recycles Keithley (Keithley) semiconductor test system to apply a fixed voltage on humidity sensor, passes through measurement
Relative electro-conductivity changes delta G/G under different relative humidities0(wherein Δ G is relative to its initial conductance G0Conductance variation)
To evaluate the characteristic of humidity sensor.Humidity sensor test is carried out indoors, and sensor exposure duration and purge time are
300s is purged with dry air, and response definition is Relative electro-conductivity variation.Referring to Fig. 8, double nets prepared by Examples 1 to 3
Network gel tests a series of its response to different relative humidity (from 4% to 90%) as humidity sensor.It tested herein
Sensitivity, response speed and the signal resume speed of sensor can be determined in journey, while finding sensor to the effective of humidity
Detection range, while the response magnitude of sensor can be obtained with the variation relation of humidity.Response-relative humidity curve will be carried out
Fitting, obtains corresponding relation equation.
Dynamic response curve as shown in Figure 8 a, the dual network gel of Examples 1 to 3 preparation is with indoor relative humidity
Increase increases immediately, when indoor relative humidity is 90%, ethylene glycol modification dual network gel and embodiment prepared by embodiment 2
The glycerine modification dual network gel of 3 preparations is up to 239% and 978% as humidity sensor conductance response ratio respectively, explanation
The absorption that can promote hydrone in solvent containing ethylene glycol and glycerine, improves the sensitivity of humidity sensor；
As shown in Figure 8 b, the glycerine modification dual network gel that prepared by embodiment 3 as humidity sensor, humidity down to
Remaining to detect that conductance responds when 4%, wide detection range of the relative humidity from 4% to 90% all has significant response, and with
Relative humidity increase to 90% conductance from 4% and increase 543 times or more.
As shown in Figure 8 c, have between the response of dual network gel humidity sensor and relative humidity of preparation of the embodiment of the present invention
There is good linear relationship, as the relative humidity response curve of the linear fit as shown in 8c, calculates the double of the preparation of embodiment 1
Glycerine prepared by ethylene glycol modification dual network gel and embodiment 3 prepared by network gel, embodiment 2 modifies dual network gel
It is respectively 0.24,6.2 and 10 as humidity sensor response sensitivity (slope), glycerine prepared by embodiment 3 modifies double nets
Sensitivity highest of the network gel as humidity sensor.
As shown in figure 8d, glycerine prepared by the dual network gel and embodiment 3 of the ethylene glycol modification that prepared by embodiment 2 is repaired
Decorations dual network gel has high sensitivity and being enough as humidity sensor and detects human body respiration, breathing cause exhalation gas and
The difference of humidity between environment, in exhalation process, the conductance of sensor increases suddenly, then rapid and complete in breathing process
It is complete to restore signal.
Response and recovery time are defined as reaching the time of 90% signal intensity in the entire amplitude of response factor.Such as figure
Shown in 8e, glycerine prepared by embodiment 3 modifies dual network gel humidity sensor, response time for respiration and extensive
The multiple time is only 0.27s and 0.3s, shows that sensor has fast response time and restores fast characteristic.
As illustrated in fig. 8f, dual network gel is modified as humidity sensor by glycerine prepared by embodiment 3 and monitors people
One month by a definite date breathing detection of body, it can be seen from the figure that gel prepared by embodiment 3 has well as humidity sensor
Stability, in test, response is basically stable at 49.3%, and error is only 0.98%.
It is breathed out when can detect human body respiration as humidity sensor using the dual network gel of preparation of the embodiment of the present invention
The humidity of gas changes, and responds fast, restores fast and favorable repeatability, the human body respiration experiment preferably outdoors into
Row.Human body respiration is monitored using the humidity sensor, can get important physiological signal relevant to human body, this application is very
With practicability.
6, the water-retaining property and stability of gel
Gel humidity sensor prepared by embodiment 1, embodiment 2 and embodiment 3 is exposed in varying environment and is carried out surely
Qualitative detection.
As shown in Fig. 9 a and Fig. 9 d, embodiment 1 is prepared double in ambient temperature and moisture environment (relative humidity 65%, 25 DEG C of environment)
Network gel humidity sensor only just loses most of moisture for 20 hours, loses conductive capability within 10 hours；And prepared by embodiment 2
Dual network gel humidity sensor quality and resistance are basically unchanged；Dual network gel humidity sensor quality prepared by embodiment 3
It tends towards stability after loss 30%, resistance becomes original 400% and gradually tends towards stability.
As shown in Fig. 9 b and Fig. 9 e, relative humidity 55%, in 40 DEG C of environment, dual network gel humidity prepared by embodiment 1
Sensor only just loses most of moisture in 8 hours, and loses conductive capability；Dual network gel humidity sensor prepared by embodiment 2
It tends towards stability after device mass loss 45%, resistance becomes original 150% and tends towards stability；Dual network prepared by embodiment 3 is solidifying
It tends towards stability after glue humidity sensor mass loss 30%, but resistance is significantly promoted.
As shown in Fig. 9 c and Fig. 9 f, relative humidity 37%, in 60 DEG C of high temperature drying environment, double nets of Examples 1 to 3 preparation
Weight loss increased network gel at high temperature, but after continuing 74 hours under the conditions of this exceedingly odious, embodiment 2
The rate of weight loss of the dual network gel of ethylene glycol or the glycerine modification prepared with embodiment 3 is still below the preparation of embodiment 1
Dual network gel.Humidity sensor prepared by embodiment 1 only just loses most of moisture in 8 hours, and loses conductive capability；Implement
It tends towards stability after dual network gel humidity sensor mass loss 60% prepared by example 2, resistance becomes original 12000%；It is real
It tends towards stability after applying the dual network gel humidity sensor mass loss 55% of the preparation of example 3, but resistance becomes original 8000%
And there is stable tendency.
Above-mentioned experiment shows in same humidity and temperature environment, ethylene glycol prepared by embodiment 2 and embodiment 3 or the third three
The dual network gel of alcohol modification is more preferable than the water-retaining property for the double-network hydrogel that embodiment 1 is not modified, and fights high temperature drying environment
Ability it is stronger, gel stability is more preferable, this illustrates that ethylene glycol or glycerine have hygroscopicity, can be improved the water conservation of gel
Property.The dual network gel of ethylene glycol modification simultaneously is in a mild condition than the weight loss of the dual network gel of glycerine modification
It is small, but under extreme conditions, the weight loss but than the dual network gel of glycerine modification is big, and (phase under temperate conditions
To humidity 55%, in 40 DEG C of environment), it is (as shown in figure 9b, small 40 that mass loss with the extension of exposure duration transition state occurs
When or so).This explanation, under the conditions of relatively mild, the dual network gel of ethylene glycol modification has preferable water-retaining property；And in pole
It holds under exacting terms, the dual network gel of glycerine modification has preferable water-retaining property.This may be because glycerine compares second
Glycol has lower vapour pressure, higher boiling point and higher viscosity, and glycerine is unevenly distributed in gel and causes at room temperature.
From the point of view of conductive condition, dual network gel prepared by embodiment 1 27 hours or longer time in exposed and environment
After become almost non-conductive, this is mainly due to gels to lose result caused by most water.In contrast, embodiment 2
The dual network gel of ethylene glycol or the glycerine modification prepared with embodiment 3 maintains conduction under all experiment conditions
Property, even if this further illustrates that harsh environmental conditions, spent glycol and glycerol moieties replace the water in hydrogel also can be significant
Improve the water-retaining property and stability of gel.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of humidity sensor, which is characterized in that including gel, the gel includes polymer network and the polymer
The electrolytic salt that network integration is collectively formed the solvent of the gel and is dissolved in the solvent, the polymer network tool
Have for the functional group with water molecules.
2. humidity sensor according to claim 1, which is characterized in that the functional group is hydrophilic radical, the function
Energy group includes-NH2、SO3 -At least one of with-OH ,-NH is preferably included2、SO3 -With-OH.
3. humidity sensor according to claim 1, which is characterized in that the solvent includes water, and including or do not wrap
Organic solvent is included, the organic solvent is preferably the small molecule polyol that carbon atom number is 1~10, more preferably glycerine and second
At least one of glycol.
4. humidity sensor according to claim 1, which is characterized in that the gel is dual network gel, including first
Polymer network and second polymer network.
5. humidity sensor according to claim 4, which is characterized in that first converging network is described molten for coating
Agent, the second polymer network are used to enhance the mechanical strength of the gel, it is preferred that the first polymer network and institute
The mass ratio for stating second polymer network is 16:1~1.3:1, it is preferred that the first polymer network is polyacrylamide,
The second polymer network is carragheen.
6. humidity sensor according to claim 1, which is characterized in that the electrolytic salt include potassium chloride, calcium chloride,
At least one of sodium chloride, preferably calcium chloride.
7. humidity sensor according to claim 1, which is characterized in that further include electrode, the electrode is for measuring institute
State the parameter of ion mobility of the electrolytic salt in the gel, it is preferred that the parameter be the electrolytic salt from
The resistance of electron conductivity or ion resistivity or the gel.
8. a kind of application of humidity sensor according to any one of claims 1 to 7, which is characterized in that the humidity
Sensor is used for relatively wet in the variation detection environment of the ion mobility in the gel by the electrolytic salt
Degree variation.
9. a kind of equipment, the equipment is that can wear humidity sensing device, humidity electronic skin, man-machine interface, flexible machine
People or Medical Devices, which is characterized in that the equipment includes humidity sensor according to any one of claims 1 to 7.
10. a kind of preparation method of humidity sensor, which comprises the steps of:
Monomer, crosslinking agent, initiator, second polymer, electrolytic salt and solvent are uniformly mixed in a heated condition, obtained
Mixed solution, the monomer, the crosslinking agent and the initiator are used to form first polymer network, the second polymer
Gel can be formed with the solvent；
Make the monomer, the crosslinking agent and the initiator crosslinked in the mixed solution polymerization reaction formed it is described
Then first polymer network is cooled into second polymer network, obtain the gel.
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| CN113092540A (en) * | 2021-03-24 | 2021-07-09 | 吉林大学 | Novel high-sensitivity micro-humidity sensor and preparation method thereof |
| CN113125523A (en) * | 2021-04-19 | 2021-07-16 | 苏州大学 | Humidity sensor based on PAAm flexible hydrogel and preparation method thereof |
| CN113125523B (en) * | 2021-04-19 | 2023-08-11 | 苏州大学 | Humidity sensor based on PAAm flexible hydrogel and preparation method thereof |
| CN113125520A (en) * | 2021-04-21 | 2021-07-16 | 重庆大学 | MoS2PEO humidity sensor, double-device humidity sensing device and humidity detection method |
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