CN109060198A - The double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class - Google Patents
The double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class Download PDFInfo
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
- G01L1/142—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors
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- 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
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- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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Abstract
The invention belongs to new material and sensor technical fields, disclose a kind of preparation method of double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA (polyacrylic acid) class, first using acrylic acid and acrylamide as substrate, iron ion is added and forms coordination, it forms uniform physics and is chemically crosslinked the double-deck tridimensional network, obtained hydrogel not only has tough mechanical performance, but also the characteristic closed with rapidly self-healing.In order to make full use of the characteristic of hydrogel, it is made into the capacitance pressure transducer, that both ends conductive layer is " sandwich " structure that self-healing hydrogel intermediate dielectric layer is PDMS.Preparation method of the invention is simple, and raw material sources are extensive, has good electrochemistry and mechanical performance, has broad application prospects in flexible wearable Material Field.
Description
Technical field
The invention belongs to new material and sensor technical fields, and in particular to a kind of double cross-linked network self-healing Heshuis of PAA class
The preparation method of gel capacitance pressure transducer,.
Background technique
Self-healing material is the inspiration by the Nature, and the healing of mimic biology bulk damage is mended by substance supply or energy
To mechanism, a kind of emerging biomimetic material for enabling the micro-damage of material to be able to heal automatically.Hydrogel is to absorb a large amount of water
And with three-dimensional net structure macromolecule, in recent years biomedicine, organizational project, agricultural, food, in terms of take
It must be widely applied.Hydrogel research is goed deep into people recently, the hydrogel for being able to achieve self-healing causes researcher
Very big concern.Self-healing hydrogel can start self-healing mechanism after by outer damage, to keep the complete of reticular structure
The mechanical performance of whole property and hydrogel guarantees that they can be used steadily in the long term.Self-healing material by physics, chemistry or
Original state can be completely or partially restored to after person's mechanical damage, it is most of to pass through interaction reversible between polymer backbone
Such as: hydrogen bond, covalent bond, the modes such as intermolecular force are realized.But bulk properties still cannot be satisfactory, this great beam
The development of hydrogel is tied up.
In recent years, with the development of the technologies such as Internet of Things, artificial intelligence and human-computer exchange, flexible wearable product is by more
Come more concern and approval.Flexible piezoelectric formula sensor because its sensor mechanism is simple, high sensitivity and the features such as low energy consumption by
Step becomes the hot spot of wearable electronic product research.Compared to conventional piezoelectric formula material, conductive hydrogel have high tensility,
The advantages that preparation process is simple, good biocompatibility, is gradually applied to energy storage, flexible actuator and stretchable sensor
Equal fields.Therefore high by simple and convenient method processing machinery intensity, the stable conductive hydrogel material of electrochemical performance
Material has great research significance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of good tensile property, short self-healing time, high self-healing effects
The hydrogel of rate and capacitance pressure transducer, is produced with it.
Mentality of designing of the invention is: forming chemical crosslinking network using acrylic acid (AA) and acrylamide (AM), simultaneously
Carboxyl and Fe in acrylic acid3+The tridimensional network for carrying out coordination type crosslinking in pairs, makes it have very strong stretching and self-healing
Property；By solidifying hydrogel solution in having reeded PDMS film, centre uses thin PDMS film as dielectric
The capacitance pressure transducer, of the sandwich structure formed with PDMS in conjunction with by hydrogel is made in layer, with very high sensitivity with
And big measurement range.
The technical solution of the present invention is as follows: be with acrylic acid (AA) and acrylamide (AM) first for monomer, six chloride hydrates
Iron (FeCl3·6H2It O) is metal ion network mixture, N, N '-methylene-bisacrylamide (MBAA) are crosslinking agent, Ammonium Persulfate 98.5
It (APS) is initiator, water (H2O it) is used as solvent, the double cross-linked network self-healing hydrogel self-healing hydrogels of PAA class are made；It will
Uncured PDMS mixture curing molding in reeded mold, obtains with reeded PDMS substrate, and in glass
One layer of thin PDMS of on piece spin coating obtains dielectric layer after solidification, then obtained self-healing hydrogel solution is reeded in tool
Solidify in PDMS film, hydrogel and PDMS dielectric layer that two are cured finally are subjected to the electricity that assembling forms sandwich structure
Appearance formula pressure sensor.
The double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class of the present invention the preparation method is as follows:
(1) by acrylic acid, acrylamide, ferric chloride hexahydrate (FeCl3·6H2O), N, N '-methylene-bisacrylamide
(MBAA), Ammonium Persulfate 98.5 (APS) and H2O wiring solution-forming in proportion leads to the 30 minutes gas removed in solution of nitrogen after mixing
Body occurs polymerization reaction 30 minutes at 60 DEG C, obtains self-healing hydrogel.
(2) by uncured PDMS in reeded mold curing molding, obtain with reeded PDMS substrate, and
One layer of spin coating thin PDMS (with a thickness of 0.5mm) is used as dielectric layer on the glass sheet.
(3) by the drop of self-healing hydrogel solution obtained in step (1) in PDMS groove, and make hydrogel in groove
Hydrogel and PDMS dielectric layer that two are cured are carried out assembling and form sandwich structure by curing molding.Then respectively in water
Upper conducting wire is pressed from both sides between gel and PDMS to export as electric signal, and finally device will be packaged with PDMS mixture, obtain electricity
Appearance formula pressure sensor.
Step (1) AA and H2The mass ratio of O is 1:5, the dosage of acrylamide be acrylic acid quality 0%~
25%, MBAA dosage are that 0%~0.325%, the APS dosage of acrylic acid quality is 0.5%, FeCl of acrylic acid quality3·6H2O
Dosage is the 0~1.2% of the amount of acrylic substance.When 2.5%, the MBAA dosage that the dosage of acrylamide is acrylic acid quality is
0.2%, the APS dosage of acrylic acid quality is 0.5%, FeCl of acrylic acid quality3·6H2O dosage is the amount of acrylic substance
When 0.72%, the comprehensive performance of self-healing hydrogel is optimal, self-healing capability, and elongation at break and maximum tension all go out very much
Color.
Elongation at break is restored to 200% after compound hydrogel healing 2h is made in step (1), and self-healing efficiency is
Elongation at break is restored to 1000% after 9.5%, 4h, and elongation at break is restored to after self-healing efficiency is 47.6%, 5h
1582%, elongation at break is restored to 1920% after self-healing efficiency is 75.4%, 6h, and self-healing efficiency is 90.8%.After 8h
Elongation at break is restored to 2173%, and self-healing efficiency is 100%.
PDMS substrate described in step (2) and dielectric layer make method particularly includes: (are made of PDMS liquid component
Two-component external member, density 1.04g/ml, viscosity 3500mPa.s, 184 silicon rubber of Dow corning Sylgard) according to matter
Amount ratio: 10:1 is uniformly mixed obtained mixture, deaerates 30 minutes and removes bubble.Then uncured mixture is poured into can
It is formed in the mold of 10mm × 20mm and 20mm thickness film, a hour is heated at 80 DEG C, the PDMS film being cured (is had
The groove of 1mm depth) removing.On the glass sheet by uncured mixture drop, with 300rpm spin coating 25s, one is heated at 80 DEG C
A hour, then removing obtains the PDMS film with a thickness of 0.5mm as intermediate dielectric layer.
The utility model has the advantages that compared with prior art, the present invention is mainly reflected in raw materials used at low cost, and production method is simple,
Fabrication cycle is short.The method of the present invention is assigned using chemical crosslinking polyacrylic acid with iron ion crosslinking polyacrylic acid simultaneously
Hydrogel dual network structure, enhances the tensile property and self-healing capability of hydrogel.The hydrogel that this method obtains breaks
It splits elongation and is up to 2173%；Self-healing recovery time is most 8h fastly, and self-healing efficiency is 100%.The condenser type of preparation
Pressure sensor, in the low pressure range of 0~400Pa, transducer sensitivity 3.28PF/KPa, and in 0.4~60kPa pressure
In range, sensitivity 0.34PF/kPa, and the pressure that can accurately measure 15Pa acts on the variation of lower capacitor.Compared to
The hydrogel pressure sensor of same type.The present invention makes simpler convenience, it is at low cost and have higher sensitivity with
And measurement width, and conductive layer has outstanding self-healing capability.
Detailed description of the invention
Fig. 1 is the different Fe prepared according to embodiment 13+The stress-strain curve of the hydrogel of concentration；
Fig. 2 is the stress-strain curve of the hydrogel of the different MBAA concentration prepared according to embodiment 2；
Fig. 3 is the stress-strain curve of the hydrogel of the different AM concentration prepared according to embodiment 3；
Fig. 4 is the PAA-PAM/Fe prepared according to embodiment 33+The SEM of hydrogel schemes；
Fig. 5 is the PAA-PAM/Fe prepared according to embodiment 33+The photo of hydrogel hydrogel before and after healing, (a) cutting
Hydrogel can stretch after hydrogel (c) healing after being divided into the healing of two parts (b)；
Fig. 6 is the PAA-PAM/Fe prepared according to embodiment 33+Hydrogel self-healing tensile stress-strain curve figure；
Fig. 7 is the curve graph of the capacitance pressure transducer, pressure change and capacitor that are prepared according to embodiment 4.
Specific embodiment
The present invention is described in further details below by embodiment, these embodiments are only used to illustrate the present invention, and
It does not limit the scope of the invention, illustrates embodiment in conjunction with example, the specific process is as follows:
Embodiment 1
Take 2g acrylic acid, 0.05g acrylamide, 4mg MBAA, 10mg APS is added and is relative to the amount of substance of acrylic acid
The FeCl of 0~1.2mol%3·6H2O stirs 30 minutes after mixing in the aqueous solution of 10mL, leads to nitrogen 30 minutes and removes
Gas in solution, solution is poured into the mold of polytetrafluoroethylene (PTFE), is occurred polymerization reaction 30 minutes at 60 DEG C, is obtained after cooling
To different Fe3+The hydrogel of concentration.When acrylamide content is 0g, FeCl3·6H2O content is labeled as when being 0.72mol%
PAA/Fe3+Hydrogel；When acrylamide content is 2.5wt%, FeCl3·6H2PAA-PAM is labeled as when O content is 0mol%
Hydrogel.
Embodiment 2
Embodiment 1 is changed to take 2g acrylic acid, 0.05g acrylamide, 10mg APS, 0.054g FeCl3·6H2O is added
The content of MBAA is 0~0.325wt% relative to acrylic acid quality, stirs 30 minutes and is uniformly mixed in the aqueous solution of 10mL
Afterwards, lead to the 30 minutes gas removed in solution of nitrogen, occur polymerization reaction 30 minutes at 60 DEG C, obtain the water of different MBAA concentration
Gel, remaining step and embodiment 1 are identical.
Embodiment 3
Embodiment 1 is changed to take 2g acrylic acid, 4mg MBAA, 10mg APS, 0.054g FeCl3·6H2Propylene is added in O
The content of amide is 0~25wt% relative to acrylic acid quality, and 30 minutes are stirred in the aqueous solution of 10mL after mixing, is led to
The nitrogen 30 minutes gas removed in solution, occurs polymerization reaction 30 minutes at 60 DEG C, obtains the water of different acrylamide concentrations
Gel, remaining step and embodiment 1 are identical.When acrylamide content is 2.5wt%, FeCl3·6H2O content is 0.72mol%
When be labeled as PAA-PAM/Fe3+Hydrogel.
Embodiment 4
(1) by PDMS, (the two-component external member being made of liquid component, density 1.04g/ml, viscosity are
184 silicon rubber of 3500mPa.s, Dow corning Sylgard) according to mass ratio: 10:1 is uniformly mixed obtained mixture,
It deaerates 30 minutes and removes bubble.Then uncured mixture is poured into the mold that can form 10mm × 20mm and 20mm thickness film
In, a hour is heated at 80 DEG C, then by the PDMS film being cured (groove with 1mm depth) removing.It will be uncured
Mixture drop with 300rpm spin coating 25s, and heats a hour, then removing obtains thickness on the glass sheet at 80 DEG C
For 0.5mm PDMS film as intermediate dielectric layer.
(2) by PAA-PAM/Fe obtained in embodiment 33+Hydrogel solution drips in PDMS groove, and hydrogel is made to exist
Hydrogel and PDMS dielectric layer that two are cured are carried out assembling and form sandwich structure by curing molding in groove.Then divide
Upper conducting wire is pressed from both sides not between hydrogel and PDMS to export as electric signal, and finally device will be sealed with PDMS mixture,
Obtain capacitance pressure transducer,.
Study on Mechanical Properties is carried out to hydrogel in embodiment 1,2,3 respectively using omnipotent machine on probation.Tension test uses
Sample size are as follows: 50mm × 10mm × 02mm cuboid, tensile loads rate are as follows: 10mm/min, test result be five times
The average value of test.As shown in Figure 1, 2, 3, FeCl is worked as in discovery3·6H2O is compared to the substance withdrawl syndrome of acrylic acid
0.72%, acrylamide is that 2.5%, MBAA is compared to the mass concentration of acrylic acid compared to the mass concentration of acrylic acid
0.2%, APS are 0.5% compared to the mass concentration of acrylic acid, the PAA-PAM/Fe of preparation3+The elongation at break of hydrogel reaches
To 2173%.
It is illustrated in figure 6 PAA-PAM/Fe under different time3+The stress-strain curve of hydrogel, passes through different time
Section, the elongation at break that hydrogel restores judge self-healing degree.Before 4h, self-healing efficiency reaches 47.6%, later
Self-healing slows, and the time that self-healing restores is 8h, and self-healing efficiency is 100%.
To the PAA-PAM/Fe prepared in embodiment 13+Hydrogel, after carrying out freeze-drying 12h, using scanning electron microscope
(SEM, FEI Quanta650) observes hydrogel surface appearance structure, and discovery hydrogel is porous network structure, as shown in Figure 4.
From fig. 5, it can be seen that after hydrogel is cut off (Fig. 5 a), hydrogel after two part Hydrogel contact 2h at room temperature
It realizes selfreparing, smooth (Fig. 5 b) that incision position becomes, and middle section can be stretched and do not occur to be broken (Fig. 5 c).Pass through pulling force
The elongation at break that hydrogel known to load-deformation curve restores judges self-healing degree, and hydrogel breaks in 2h after severance
It splits elongation and is restored to 200%, elongation at break is restored to 1000% after self-healing efficiency is 9.5%, 4h, and self-healing efficiency is
Elongation at break is restored to 1582% after 47.6%, 5h, and elongation at break is restored to after self-healing efficiency is 75.4%, 6h
1920%, self-healing efficiency is 90.8%, as shown in Figure 6.
To in embodiment 4 with PAA-PAM/Fe3+The capacitance pressure transducer, of hydrogel preparation carries out pressure sensitive test
Experiment.As shown in fig. 7, in the low pressure range of 0-400Pa, transducer sensitivity 3.28PF/KPa, and in 0.4~60kPa
In pressure limit, sensitivity 0.34PF/kPa, and the pressure that can accurately measure 15Pa acts on the variation of lower capacitor.This
Will be in wearable device, flexible electronic devices, field of biosensors is with very high application prospect.
Claims (6)
1. a kind of preparation method of the double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class, it is characterised in that: institute
Stating preparation method, steps are as follows:
(1) by acrylic acid (AA), acrylamide (AM), ferric chloride hexahydrate (FeCl3·6H2O), N, N '-methylene bisacrylamide acyl
Amine (MBAA), Ammonium Persulfate 98.5 (APS) and water (H2O) wiring solution-forming in proportion leads to 30 minutes removing solution of nitrogen after mixing
In gas, carry out polymerization reaction 30 minutes at 60 DEG C, obtain the double cross-linked network self-healing hydrogels of PAA class；
(2) by uncured PDMS in reeded mold curing molding, obtain with reeded PDMS substrate, and in glass
One layer of thin PDMS of glass on piece spin coating is as dielectric layer；
(3) by the drop of self-healing hydrogel solution obtained in step (1) in PDMS groove, and make hydrogel in recessed in-tank-solidification
Hydrogel and PDMS dielectric layer that two are cured are carried out assembling and form sandwich structure by molding；Then respectively in hydrogel
Upper conducting wire is pressed from both sides between PDMS to export as electric signal, and finally device will be packaged with PDMS mixture, obtain condenser type
Pressure sensor.
2. the preparation method of the double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class as described in claim 1,
It is characterized by: the sensor obtained is made of self-healing hydrogel and PDMS, wherein hydrogel is formed in conjunction with PDMS
The capacitance pressure transducer, of hydrogel-PDMS- hydrogel " sandwich " structure.
3. the preparation method of the double cross-linked network self-healing hydrogels of PAA class as described in claim 1, it is characterised in that: step
(1) AA and H2The mass ratio of O is 1:5, and the dosage of acrylamide is that 0~25%, the MBAA dosage of acrylic acid quality is third
0~0.325%, the APS dosage of olefin(e) acid quality is 0.5%, FeCl of acrylic acid quality3·6H2O dosage is acrylic substance
The 0~1.2% of amount.
4. the preparation method of the double cross-linked network self-healing hydrogels of PAA class as described in claim 1, it is characterised in that: step
(1) elongation at break is restored to 200% after the healing of hydrogel made from 2h, and self-healing efficiency is elongation at break after 9.5%, 4h
It is restored to 1000%, elongation at break is restored to 1582% after self-healing efficiency is 47.6%, 5h, and self-healing efficiency is
Elongation at break is restored to 1920% after 75.4%, 6h, and elongation at break is restored to after self-healing efficiency is 90.8%, 8h
2173%, self-healing efficiency is 100%.
5. the preparation method of the double cross-linked network self-healing hydrogels of PAA class as described in claim 1, it is characterised in that: step
(2) composition of the hydrogel for preparing capacitance pressure transducer, in mass ratio are as follows: AA and H2The mass ratio of O be 1:5, third
It is 0.2%, the APS dosage of acrylic acid quality is acrylic acid matter that the dosage of acrylamide, which is 2.5%, the MBAA dosage of acrylic acid quality,
0.5%, FeCl of amount3·6H2O dosage is the 0.72% of the amount of acrylic substance.
6. the preparation method of the double cross-linked network self-healing hydrogel capacitance pressure transducer,s of PAA class as described in claim 1,
It is characterized by: pair that PDMS described in step (2) (184 silicon rubber of Dow corning Sylgard) is made of liquid component
Component external member, density 1.04g/ml, viscosity 3500mPa.s, two components are according to mass ratio: 10:1 is uniformly mixed and obtains
Mixture deaerates 30 minutes and removes bubble；Then uncured mixture is poured into in reeded Teflon mould,
A hour is heated at 80 DEG C, can form 10mm × 20mm and 20mm thickness and has the PDMS film of 1mm deep trouth；In addition will not consolidate
The PDMS mixture of change, on the glass sheet with 300rpm spin coating 25s, is heated a hour at 80 DEG C, obtained by the method for spin coating
With a thickness of 0.5mm PDMS film as intermediate dielectric layer.
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Application publication date: 20181221 |