CN113603902A - Conductive hydrogel electrode material and application thereof - Google Patents
Conductive hydrogel electrode material and application thereof Download PDFInfo
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- CN113603902A CN113603902A CN202110824646.1A CN202110824646A CN113603902A CN 113603902 A CN113603902 A CN 113603902A CN 202110824646 A CN202110824646 A CN 202110824646A CN 113603902 A CN113603902 A CN 113603902A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/103—Detecting, measuring or recording devices for testing the shape, pattern, colour, size or movement of the body or parts thereof, for diagnostic purposes
- A61B5/11—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb
- A61B5/1113—Local tracking of patients, e.g. in a hospital or private home
- A61B5/1114—Tracking parts of the body
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/103—Detecting, measuring or recording devices for testing the shape, pattern, colour, size or movement of the body or parts thereof, for diagnostic purposes
- A61B5/11—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb
- A61B5/1126—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb using a particular sensing technique
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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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
Abstract
The invention discloses a conductive hydrogel electrode material and application thereof, which is prepared by fully mixing raw materials including acrylamide, sodium carboxymethyl cellulose, soluble metal inorganic salt, diene-containing flexible long-chain compound, initiator and water, vacuum degassing and curing. According to the invention, the two specific polymers are combined to form semi-interpenetrating or interpenetrating double-network hydrogel, and inorganic salt or conductive polymer is added for compounding, so that the prepared conductive hydrogel material has good mechanical properties and a higher strain window, can still have good sensitivity under micro-deformation, and enhances the reliability of signals.
Description
Technical Field
The invention belongs to the technical field of wearable sensing equipment for organisms or soft robots, and particularly relates to a conductive hydrogel electrode material and application thereof.
Background
With the continuous development and progress of social productivity and scientific technology, the demand of various industries on virtual reality technology (VR technology) is increasing day by day, the VR technology has the characteristics of immersion, interactivity and the like, and in order to realize the effect of human-computer interaction, wearable electronic wearable sensors which are more sensitive and more skin-close are needed. However, what is not satisfactory is that the conductor (such as metal, carbon-based material, conductive composite material, conductive polymer) widely used in various circuits at present has poor stretchability, and is not ideal for portable and wearable use. Therefore, the development of a flexible bionic thin-film device/sensor which can be deformed in a large area by pulling and pressing and has sensing capability like human skin is urgent. The flexible sensor has shown potential application value in the fields of medical care, exercise health detection, implantable devices, entertainment games, future internet of things, software robots, artificial intelligence AI and the like, and the research on the functionalization, miniaturization and modularization of the flexible sensor is more and more emphasized, so that wearable or implantable electronic products become possible.
Conductive gels have attracted attention as a new functional material in the field of manufacturing soft electronic devices. The conductive gel may be classified into an electron conductive gel and an ion conductive gel according to a difference in a conductive mechanism. An electron conducting gel generally refers to a composite conducting organogel that transports charge by adding electrons, such as nanomaterials or conducting polymers, as carriers. The composite conductive organic gel has poor interface compatibility between the added conductive material and the gel matrix, so that the inside of the material does not coordinate and irreversibly move in the deformation process, the tensile property is reduced, and the viscous deformation in the electronic conductive gel can trigger a dynamic electric response signal to show noise. Thus, although electronically conductive gels have a generally recognized high sensitivity in strain-electric sensing devices, the problem of low signal-to-noise ratio and low response reliability of most devices during application is limited.
In recent years, ionic hydrogels have been developed for flexible and stretchable sensing devices due to their high transparency, high stretchability, specific flexibility and biocompatibility. The typical preparation of ionic flexible conductors currently in the research phase is a polymer matrix loaded with dissolved inorganic salts (NaCl, LiCl, FeCl)3、ZnSO4Etc.). The conductors are mainly flexible matrixes composed of polymers, so the conductors have the essential characteristics of ductility, stability, high elasticity, resilience and the like of high polymer materials, and can maintain the volume conductivity in a reversible deformation process, so that the conductors are applied to the fields of ion skin, ion cables, ion touch control and the like. The conductive gel sensor prepared by the ionic conductor has a stable ion transmission channel, can generate reliable response signals in time under external stimulation, and has simple manufacturing process and wide application prospect. However, the chemically crosslinked polymer electrolyte network composed of a single polymer is often weak in mechanical properties, prone to fatigue, and has a small strain window, and thus the sensitivity of the conventional ion conductive gel sensor to sensing fine deformation is insufficient.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the conductive hydrogel electrode material which has the advantages of low price, simple process, time-saving and high-efficiency preparation and convenient industrialization;
the invention also aims to provide a flexible bionic sensor applying the conductive hydrogel material.
The technical scheme of the invention is as follows:
a conductive hydrogel electrode material is prepared from raw materials including acrylamide, sodium carboxymethyl cellulose, soluble metal inorganic salt, diene-containing flexible long-chain compound, initiator and water through full mixing, vacuum degassing and solidifying, wherein the soluble metal inorganic salt is NaCl, KCl, LiCl or ZnSO4、FeCl3And NaSO4At least one of the compounds, the diene-containing flexible long-chain compound is N, N-methylene bisacrylamide or polyethylene glycol diacrylate, the initiator is an oxidation initiator or a photoinitiator, the mass ratio of the acrylamide, the sodium carboxymethylcellulose, the soluble metal inorganic salt, the diene-containing flexible long-chain compound and the initiator is 1-5:0.05-5:0.1-3:0.0005-0.0025:0.008-0.04, and the amount of water is 30-70 wt%.
In a preferred embodiment of the present invention, the oxidation initiator is ammonium persulfate or potassium persulfate.
Further preferably, the oxidation initiator is used in combination with N, N' -dimethylethylenediamine.
In a preferred embodiment of the present invention, the photoinitiator is 2-hydroxy-2-methylpropiophenone or 2-hydroxy-4- (2-hydroxyethoxy) -2-methylpropiophenone.
In a preferred embodiment of the invention, the adhesive is prepared from acrylamide, sodium carboxymethylcellulose, soluble metal inorganic salt, diene-containing flexible long-chain compound, photoinitiator and water by thoroughly mixing, vacuum degassing and curing.
Further preferably, the soluble metal inorganic salt is ZnSO4·7H2O, the diene-containing flexible long-chain compound is N, N-methylene bisacrylamide, and the photoinitiator is 2-hydroxy-2-methyl propiophenone.
Still more preferably, the mass ratio of the acrylamide, the sodium carboxymethylcellulose, the soluble metal inorganic salt, the diene-containing flexible long-chain compound and the photoinitiator is 1.5-3:0.05-0.25:0.3-0.5:0.0008-0.0015: 0.012-0.024.
The other technical scheme of the invention is as follows:
a flexible bionic sensor is provided with the conductive hydrogel electrode material.
In a preferred embodiment of the present invention, a support encapsulant is also included.
Further preferably, the supporting and packaging material is 3M VHB transparent adhesive tape.
The invention has the beneficial effects that:
1. according to the invention, the two specific polymers are combined to form semi-interpenetrating or interpenetrating double-network hydrogel, and inorganic salt or conductive polymer is added for compounding, so that the prepared conductive hydrogel material has good mechanical properties (high tensile strength and capability of resisting general external impact) and a higher strain window, and still has good sensitivity under micro-deformation, and the reliability of signals is enhanced.
2. The method adopts a one-pot free radical polymerization reaction method, has simple operation and low equipment requirement, the experimental raw materials are all commonly used chemical products, no organic solvent is used, the production process is safe and reliable, the explosion risk does not exist, the price is low, and the economic benefit is high after industrialization.
3. The specific initiator of the invention replaces the traditional thermal initiation reaction to prepare the ionic conduction gel, thereby overcoming the problems of long thermal initiation reaction time and the like and reducing the water loss of the prepared hydrogel in the thermal reaction process.
4. The mechanical property of the hydrogel can be adjusted through different ion concentrations in the conductive hydrogel electrode material, so that a dynamic adjustable effect is achieved.
5. The matrix frame of the ionic-conductive hydrogel electrode material disclosed by the invention adopts the combination of semi-rigid and flexible polymers, so that the problem that single polymer gel is easy to fatigue is well solved, and the fatigue resistance of the integral sensing device is improved.
6. The flexible bionic sensor disclosed by the invention has the characteristics that different conductivity intervals are shown after being stimulated by an external environment on the premise of keeping the dimensional stability of a solid phase.
Drawings
FIG. 1 is a Fourier transform infrared spectrum of the ion-conducting gel prepared in example 3 of the present invention and the raw materials used.
FIG. 2 is a graph showing the results of the lighting experiment (including stretching, twisting, and folding) of the ion-conducting gel strip in example 3 of the present invention.
FIG. 3 is a stress-strain diagram for uniaxial tensile testing of gel strips according to examples 1 to 3 of the present invention.
Fig. 4 is a graph showing the effect of the application of the flexible strain sensor in example 2 of the present invention (fig. 4b, the highest point of the pulse is when the index finger is at 0 °, and the lowest point is at 90 °).
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
Example 1:
formula/g of mixed solution:
AM：3g；
ZnSO4·7H2O：0.3g；
CMCNa：0.15g；
solvent: water;
preparing 5 wt% CMCNa aqueous solution and 15 wt% MBA dispersion in advance, weighing 3g of 5 wt% CMCNa solution, 3g AM, and 0.3g ZnSO4·7H2O was put into a 20mL glass bottle, 2cm magnetons and 10mL water were added, and the mixture was stirred at 1000rpm for 60min to obtain a uniform mixed solution. Then, 10. mu.L of 15% MBA and 24mg of a photoinitiator 1173 were added to the mixed solution, and the mixture was again stirred at high speed for about 30 minutes, and the mixed solution was vacuum-degassed for 10 minutes and then poured into a suitable light-transmitting mold to be sealed. Placing the mold into 365nm ultraviolet curing box, placing until the illumination is finished for 30min, taking out the formed conductive gel shown in figure 3, blowing the surface of the gel with inert gas, and cutting the large gel into strip 30 × 3 × 2mm required by sensor packaging by laser cutting system3Two ends are connected with the copper sheet in an adhesion mode, and finally, two pieces of 3M VHB transparent adhesive tapes with the same size are packaged to manufacture the flexible packaging tapeA resistive stretchable ionogel strain sensor.
Example 2:
formula/g of mixed solution:
AM：3g；
ZnSO4·7H2O：0.3g；
CMCNa：0.1g；
solvent: water;
preparing 5 wt% CMCNa aqueous solution and 15 wt% MBA dispersion in advance, weighing 2g of 5 wt% CMCNa solution, 3g AM, 0.3g ZnSO4·7H2O is put into a 20mL glass bottle, 2cm magnetons and 10mL water are added, the temperature is heated to 40 ℃, and the mixture is stirred at 1000rpm for 60min to obtain a uniform mixed solution. Then 10 μ L of 15% MBA and 24mg of photoinitiator 1173 were added to the mixed solution, stirred at high speed again for about 30min, the mixed solution was vacuum degassed for 10min, and then poured into a suitable light-transmitting mold to be sealed. Placing the mold into 365nm ultraviolet curing box, placing until the illumination is finished for 30min, taking out the formed conductive gel shown in figure 3, blowing the surface of the gel with inert gas, and cutting the large gel into strip 30 × 3 × 2mm required by sensor packaging by laser cutting system3And two ends of the flexible stretchable resistance type ionic gel strain sensor are jointed with the copper sheet in an adhesion mode, and finally, the flexible stretchable resistance type ionic gel strain sensor is packaged by two 3M VHB transparent adhesive tapes with the same size.
The flexible stretchable resistance type ionic gel strain sensor is directly adhered to a human body detection joint to be detected and is adhered to a forefinger joint in a graph of fig. 4a, and a lighting experiment of bending at different angles is carried out. The strain sensor is connected with the electrochemical workstation through a lead to detect the change of the electric signal generated by the human body movement, as shown in fig. 4b, wherein the highest point of the pulse is when the index finger is at 0 degree, and the lowest point of the pulse is when the index finger is at 90 degrees.
Example 3:
formula/g of mixed solution:
AM：3g；
ZnSO4·7H2O：0.3g；
CMCNa：0.25g；
solvent: water;
5 wt% CMCNa aqueous solution and 15 wt% MBA dispersion are prepared in advance, and 5g of 5 wt% CMCNa solution, 3g AM, and 0.3g ZnSO are weighed4·7H2O is put into a 20mL glass bottle, 2cm magnetons and 10mL water are added, the temperature is heated to 40 ℃, and the mixture is stirred at 1000rpm for 60min to obtain a uniform mixed solution. Then 10 μ L of 15% MBA and 24mg of photoinitiator 1173 were added to the mixed solution, stirred at high speed again for about 30min, the mixed solution was vacuum degassed for 10min, and then poured into a suitable light-transmitting mold to be sealed. Placing the mold into 365nm ultraviolet curing box, placing until the illumination is finished for 30min, taking out the formed conductive gel shown in figures 1 and 3, blowing the surface of the gel with inert gas, and cutting the large gel into strips of 30 x 3 x 2mm required by sensor packaging by a laser cutting system3And two ends of the flexible stretchable resistance type ionic gel strain sensor are jointed with the copper sheet in an adhesion mode, and finally, the flexible stretchable resistance type ionic gel strain sensor is packaged by two 3M VHB transparent adhesive tapes with the same size.
The conductive gel obtained in this example was cut into 30X 6X 3mm3And the long strip realizes a passage by connecting the power supply, the LED lamp and the gel long strip in series. The gel was subjected to mechanical deformation such as stretching, twisting, bending, and the like under the action of a voltage of 3V, and the stability of the gel under the energized condition was verified, and the result is shown in fig. 2.
Example 4:
formula/g of mixed solution:
AM：1.5g；
ZnSO4·7H2O：0.5g；
CMCNa：0.05g；
solvent: water;
preparing 5 wt% CMCNa aqueous solution and 15 wt% MBA dispersion in advance, weighing 1g of 5 wt% CMCNa solution, 1.5g AM, 0.5g ZnSO4·7H2O is put into a 20mL glass bottle, 2cm magnetons and 5mL water are added, the temperature is heated to 40 ℃, and the mixture is stirred at 1000rpm for 60min to obtain a uniform mixed solution. Then 6. mu.L of 15% MBA and 12mg of photoinitiator 1173 are added to the mixed solution, the mixture is again stirred at high speed for about 30min, the mixed solution is degassed in vacuum for 10min, and then poured into a suitable light-transmitting mold for sealing. Placing the mold into 365nm ultraviolet curing box, placing until the illumination is finished for 30min, taking out the formed conductive gel, blowing the surface of the gel with inert gas, and cutting the large gel into strip shape of 30 × 3 × 2mm required by sensor packaging by laser cutting system3And two ends of the flexible stretchable resistance type ionic gel strain sensor are jointed with the copper sheet in an adhesion mode, and finally, the flexible stretchable resistance type ionic gel strain sensor is packaged by two 3M VHB transparent adhesive tapes with the same size.
Example 5:
formula/g of mixed solution:
AM：2.5g；
ZnSO4·7H2O：0.5g；
CMCNa：0.15g；
solvent: water;
preparing 5 wt% CMCNa aqueous solution and 15 wt% MBA dispersion in advance, weighing 3g of 5 wt% CMCNa solution, 2.5g AM, 0.5g ZnSO4·7H2O is put into a 20mL glass bottle, 2cm magnetons and 10mL water are added, the temperature is heated to 40 ℃, and the mixture is stirred at 1000rpm for 60min to obtain a uniform mixed solution. Then 10 μ L of 15% MBA and 20mg of photoinitiator 1173 were added to the mixed solution, stirred at high speed again for about 30min, the mixed solution was vacuum degassed for 10min, and then poured into a suitable light-transmitting mold to be sealed. Placing the mold into 365nm ultraviolet curing box, placing until the illumination is finished for 30min, taking out the formed conductive gel, blowing the surface of the gel with inert gas, and cutting the large gel into strip shape of 30 × 3 × 2mm required by sensor packaging by laser cutting system3And two ends of the flexible stretchable resistance type ionic gel strain sensor are jointed with the copper sheet in an adhesion mode, and finally, the flexible stretchable resistance type ionic gel strain sensor is packaged by two 3M VHB transparent adhesive tapes with the same size.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A conductive hydrogel electrode material, whichIs characterized in that: is prepared from raw materials including acrylamide, sodium carboxymethyl cellulose, soluble metal inorganic salt, diene-containing flexible long-chain compound, initiator and water through fully mixing, vacuum degassing and solidifying, wherein the soluble metal inorganic salt is NaCl, KCl, LiCl or ZnSO4、FeCl3And NaSO4At least one of the compounds, the diene-containing flexible long-chain compound is N, N-methylene bisacrylamide or polyethylene glycol diacrylate, the initiator is an oxidation initiator or a photoinitiator, the mass ratio of the acrylamide, the sodium carboxymethylcellulose, the soluble metal inorganic salt, the diene-containing flexible long-chain compound and the initiator is 1-5:0.05-5:0.1-3:0.0005-0.0025:0.008-0.04, and the amount of water is 30-70 wt%.
2. The conductive hydrogel electrode material of claim 1, wherein: the oxidation initiator is ammonium persulfate or potassium persulfate.
3. The conductive hydrogel electrode material of claim 2, wherein: the oxidation initiator is used in combination with N, N, N ', N' -dimethylethylenediamine.
4. The conductive hydrogel electrode material of claim 1, wherein: the photoinitiator is 2-hydroxy-2-methyl propiophenone or 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone.
5. The conductive hydrogel electrode material of claim 1, wherein: is prepared from acrylamide, carboxymethyl cellulose sodium, soluble metal inorganic salt, diene-containing flexible long-chain compound, photoinitiator and water through mixing, vacuum degassing and solidifying.
6. The conductive hydrogel electrode material of claim 5, wherein: the soluble metal inorganic salt is ZnSO4.7H2O, the diene-containing flexible long-chain compound is N, N-methylene bisacrylamide, andthe photoinitiator is 2-hydroxy-2-methyl propiophenone.
7. The conductive hydrogel electrode material of claim 6, wherein: the mass ratio of the acrylamide to the sodium carboxymethylcellulose to the soluble metal inorganic salt to the diene-containing flexible long-chain compound to the photoinitiator is 1.5-3:0.05-0.25:0.3-0.5:0.0008-0.0015: 0.012-0.024.
8. A flexible bionic sensor is characterized in that: an electrically conductive hydrogel electrode material as claimed in any one of claims 1 to 7.
9. A flexible biomimetic sensor as recited in claim 8, wherein: a supporting encapsulation material is also included.
10. A flexible biomimetic sensor as recited in claim 9, wherein: the supporting and packaging material is 3M VHB transparent adhesive tape.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115304323A (en) * | 2022-07-21 | 2022-11-08 | 中交四航工程研究院有限公司 | Conductive mortar and preparation method and application thereof |
| CN117126429A (en) * | 2023-10-25 | 2023-11-28 | 之江实验室 | Gel semi-dry electrode and preparation method and application thereof |
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Cited By (3)
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