CN112080019B - Conductive self-repairing hydrogel material capable of being printed in 3D mode and preparation method and application thereof - Google Patents
Conductive self-repairing hydrogel material capable of being printed in 3D mode and preparation method and application thereof Download PDFInfo
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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- 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
- C08J2433/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
Abstract
The invention provides a conductive self-repairing hydrogel material capable of being printed in a 3D mode, and a preparation method and application thereof, wherein the preparation method comprises the following steps: step 1, dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, fully stirring, performing ultrasonic dispersion, and centrifuging to obtain a dispersion liquid A; step 2, adding calcium chloride and polyacrylic acid into the dispersion liquid A, and stirring to obtain a carbon nano tube dispersion liquid B in which the calcium chloride and the polyacrylic acid are dissolved; step 3, dissolving sodium alginate in a sodium hydroxide solution, and stirring to obtain an alkaline mixed solution C of the sodium alginate; and 4, slowly dropwise adding the mixed solution C with the same volume into the dispersion liquid B under the condition of rapid stirring, and continuously stirring for a period of time to obtain the calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel which has 3D printability, stimulation responsiveness and self-repairing capability. The method has the advantages of simple process, convenient operation and low energy consumption in the synthesis process, and is suitable for industrialization.
Description
Technical Field
The invention belongs to the technical field of conductive self-repairing hydrogel, and particularly relates to a conductive self-repairing hydrogel material for 3D printing, a bionic preparation method and application of the conductive self-repairing hydrogel material.
Technical Field
When picking mussels seashore it has been found that it is difficult to peel them from the rock without the use of suitable tools. This is because mussels secrete a cohesive elastic protein silk fluid similar to hydrogels, which allows mussels to adhere to virtually any hard solid surface, such as reef, metal, stakes, plastic, and even other biological surfaces. In addition, the protein secreted by the mussel is rich in the amino acid L-Dopa, so that the mussel has viscosity and self-repairing capability and is endowed with the conductive property.
Hydrogels have a structure similar to that of biological tissues and a high water content, and thus have played an important role in biomedical and bioengineering fields such as drug delivery, soft actuators, electrochemical devices, and artificial muscles. The conductive hydrogel combines the electrochemical performance of conductive macromolecules and the soft characteristic of the hydrogel, has large specific surface area and excellent electron transmission and ion transmission capabilities, and is an ideal material for constructing flexible intelligent equipment.
In recent years, many biomimetic conductive hydrogel materials have been developed. For example, the Small journal (Small 2017,13,1601916) reports that Graphene Oxide (GO) is partially reduced into conductive graphene by utilizing Polydopamine (PDA), and a conductive hydrogel capable of stretching, self-adhesion and self-repairing is designed. Advanced functional materials (adv. funct. mater.2017,27,1703852) reported a self-adhesive self-healing conductive composite hydrogel inspired by mussels, which could monitor the micro-movements of the human body in real time. The Nano Kuaiji (Nano Lett.2019,19,8343) also reports a conductive self-adhesive hydrogel with anisotropy, which can be combined with high-flux electrical stimulation to regulate the proliferation and oriented growth of myoblasts and is expected to be applied to the bionic field of simulating biological tissues and the like. However, none of these conductive hydrogels have both 3D printability and stimulus responsiveness, which severely limits their application in the field of bionics.
Therefore, the prepared conductive hydrogel with 3D printability, stimulation responsiveness and self-repairing capability is a hotspot and difficulty in the field of bionic hydrogels, and has important significance in the aspects of practical application, such as human body wearable intelligent equipment, software robots and the like.
Disclosure of Invention
The present invention is made to solve the above problems, and an object of the present invention is to provide a conductive hydrogel material having 3D printability, stimulation responsiveness and self-repairing capability, a biomimetic preparation method thereof, and a piezoresistive strain sensor capable of responding to external pressure stimulation in real time.
In order to achieve the purpose, the invention adopts the following scheme:
< preparation method >
The invention provides a preparation method of a conductive self-repairing hydrogel material capable of being printed in a 3D mode, which is characterized by comprising the following steps of: step 1, dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, fully stirring, performing ultrasonic dispersion, and centrifuging to obtain a dispersion liquid A; step 2, adding a certain amount of calcium chloride and polyacrylic acid into the dispersion liquid A, and stirring to obtain a carbon nano tube dispersion liquid B in which the calcium chloride and the polyacrylic acid are dissolved; step 3, dissolving a certain amount of sodium alginate in a sodium hydroxide solution with a certain concentration, and stirring to obtain an alkaline mixed solution C of the sodium alginate; and 4, slowly dropwise adding the mixed solution C with the same volume into the dispersion liquid B under the condition of rapid stirring, and continuously stirring for a period of time to obtain the calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel.
Preferably, the preparation method of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention can further have the following characteristics: in the dispersion liquid A, the concentrations of the sodium dodecyl benzene sulfonate and the carbon nano tube are respectively 0.05 to 0.15 weight percent and 0.05 to 0.25 weight percent.
Preferably, the preparation method of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention can further have the following characteristics: in the step 1, the stirring time is 10-20 min, the ultrasonic dispersion time is 30min, the rotating speed is 9000rpm, and the centrifugation time is 20 min.
Preferably, the preparation method of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention can further have the following characteristics: in the step 2, the molar concentrations of the calcium chloride and the polyacrylic acid are 0.1-0.2M and 0.1-0.3M respectively, and the average molecular weight of the polyacrylic acid is 10-25 ten thousand.
Preferably, the preparation method of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention can further have the following characteristics: in the step 3, the molar concentration of the sodium hydroxide is 0.1-0.2M, and the concentration of the sodium alginate is 0.06-0.12 wt%.
Preferably, the preparation method of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention can further have the following characteristics: the stirring time in the steps 2 and 3 is 10-20 min, and the stirring time in the step 4 is about 30 min.
< conductive self-healing hydrogel Material >
Further, the invention also provides a conductive self-repairing hydrogel material which can be 3D printed and is prepared by adopting the method described in the preparation method.
< application >
Furthermore, the invention also provides application of the conductive self-repairing hydrogel material capable of being printed in 3D as 3D printing ink. Specifically, various three-dimensional digital models can be designed by adopting Cellink HeartWare software and converted into an STL file format, and then a conductive self-repairing hydrogel material is used as 3D printing ink, and a biological 3D printer is used for printing out a designed hydrogel pattern.
Preferably, the application of the conductive self-repairing hydrogel material capable of being 3D printed provided by the invention as a 3D printing ink can further have the following characteristics: the conductive self-repairing hydrogel material is subjected to 3D printing in an air pump type extrusion printing mode.
Furthermore, the invention also provides application of the conductive self-repairing hydrogel material capable of being printed in a 3D mode as the flexible piezoresistive sensor. Specifically, two pieces of insulating elastomers VHB can be used to sandwich the printed hydrogel pattern and connect with copper electrodes to form a piezoresistive strain sensor.
Action and Effect of the invention
A large number of carbon nanotubes are uniformly distributed in the calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel prepared by the method; in the range of 0.1 to 100s-1The viscosity can be gradually reduced to below 43Pa · s by the increasing process of the shear rate of (1); after the stretched 1000 percent of length is recovered to the original length, the self-healing capability of the composite material is achievedTo more than 78%; when applied to a strain sensor, the sensor can respond to pressure stimulation caused by the bending of an index finger by 40% relative resistance change. The calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive self-repairing hydrogel prepared by the invention has the advantages of simple process, convenient operation, low energy consumption in the synthesis process and suitability for industrialization.
Drawings
FIG. 1 is a transmission scan of a calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel prepared in example one;
FIG. 2 is a graph of viscosity-shear rate of the calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel prepared in example two;
FIG. 3 is a scanning graph of the elastic modulus-strain of the calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel prepared in example two;
fig. 4 is a graph of the relative resistance change versus time in response to the stimulation of the bending pressure of the index finger of the calcium ion/polyacrylic acid/carbon nanotube/sodium alginate strain sensor prepared in example two.
Detailed Description
Specific embodiments of the conductive self-repairing hydrogel material capable of being 3D printed, the preparation method and the application thereof according to the present invention are described in detail below with reference to the accompanying drawings.
< example one >
The preparation method comprises the following steps:
(1) dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, wherein the concentration of the mixture is 0.1 wt%, stirring for 15min, then performing ultrasonic dispersion for 30min, and then centrifuging for 20min at 9000rpm to obtain a uniform carbon nano tube dispersion liquid;
(2) adding a certain amount of calcium chloride and polyacrylic acid into the carbon nano tube dispersion liquid, and stirring for 15min to obtain the carbon nano tube dispersion liquid with the molar concentrations of 0.2M calcium chloride and 0.15M polyacrylic acid;
(3) dissolving a certain amount of sodium alginate in 0.1M sodium hydroxide solution, and stirring for 15min to obtain 0.1M sodium hydroxide solution containing 0.08 wt% of sodium alginate;
(4) slowly dripping alkaline solution of sodium alginate with the same volume in carbon nano tube dispersion liquid of calcium chloride and polyacrylic acid under the condition of rapid stirring, and continuously stirring for 30min to obtain calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel;
(5) designing a grid three-dimensional digital model by using Cellink HeartWare software, converting the grid three-dimensional digital model into an STL file format, and then printing a hydrogel grid structure by using a biological 3D printer;
(6) two pieces of insulating elastomers VHB are used for clamping the hydrogel with the grid structure in the middle to form a sandwich structure, and copper electrodes are used for connecting to form the piezoresistive strain sensor.
And (3) performance characterization:
in the first embodiment, as shown in fig. 1, a large number of carbon nanotubes are uniformly distributed in the prepared calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel. In the range of 0.1 to 100s-1The viscosity decreased from 225 pas to 43 pas at the shear rate of (2). Its self-healing capacity is 85%. When applied to a strain sensor, the sensor can respond to pressure stimulation caused by the bending of an index finger by a relative resistance change of 30 percent.
< example two >
The preparation method comprises the following steps:
(1) dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, wherein the concentration of the mixture is 0.1 wt%, stirring for 15min, then performing ultrasonic dispersion for 30min, and then centrifuging for 20min at 9000rpm to obtain a uniform carbon nano tube dispersion liquid;
(2) adding a certain amount of calcium chloride and polyacrylic acid into the carbon nano tube dispersion liquid, and stirring for 15min to obtain the carbon nano tube dispersion liquid with the molar concentrations of 0.2M calcium chloride and 0.2M polyacrylic acid;
(3) dissolving a certain amount of sodium alginate in 0.1M sodium hydroxide solution, and stirring for 15min to obtain 0.1M sodium hydroxide solution containing 0.08 wt% of sodium alginate;
(4) slowly dripping alkaline solution of sodium alginate with the same volume in carbon nano tube dispersion liquid of calcium chloride and polyacrylic acid under the condition of rapid stirring, and continuously stirring for 30min to obtain calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel;
(5) designing a grid three-dimensional digital model by using Cellink HeartWare software, converting the grid three-dimensional digital model into an STL file format, and then printing a hydrogel grid structure by using a biological 3D printer;
(6) two pieces of insulating elastomers VHB are used for clamping the hydrogel with the grid structure in the middle to form a sandwich structure, and copper electrodes are used for connecting to form the piezoresistive strain sensor.
And (3) performance characterization:
in the second embodiment, a large number of carbon nanotubes are uniformly distributed in the prepared calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel. As shown in FIG. 2, in the range of 0.1 to 100s-1The viscosity decreased from 120 pas to 20 pas at the shear rate of (2). As shown in fig. 3, the self-healing capacity was 87%. As shown in fig. 4, when applied to a strain sensor, the strain sensor is able to respond to a pressure stimulus from index finger bending with a relative resistance change of 40%.
< example three >
The preparation method comprises the following steps:
(1) dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, wherein the concentration of the mixture is 0.1 wt%, stirring for 15min, then performing ultrasonic dispersion for 30min, and then centrifuging for 20min at 9000rpm to obtain a uniform carbon nano tube dispersion liquid;
(2) adding a certain amount of calcium chloride and polyacrylic acid into the carbon nano tube dispersion liquid, and stirring for 15min to obtain the carbon nano tube dispersion liquid with the molar concentrations of 0.2M calcium chloride and 0.25M polyacrylic acid;
(3) dissolving a certain amount of sodium alginate in 0.1M sodium hydroxide solution, and stirring for 15min to obtain 0.1M sodium hydroxide solution containing 0.08 wt% of sodium alginate;
(4) slowly dripping alkaline solution of sodium alginate with the same volume in carbon nano tube dispersion liquid of calcium chloride and polyacrylic acid under the condition of rapid stirring, and continuously stirring for 30min to obtain calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel;
(5) designing a grid three-dimensional digital model by using Cellink HeartWare software, converting the grid three-dimensional digital model into an STL file format, and then printing a hydrogel grid structure by using a biological 3D printer;
(6) two pieces of insulating elastomers VHB are used for clamping the hydrogel with the grid structure in the middle to form a sandwich structure, and copper electrodes are used for connecting to form the piezoresistive strain sensor.
And (3) performance characterization:
in the third embodiment, a large number of carbon nanotubes are uniformly distributed in the prepared calcium ion/polyacrylic acid/carbon nanotube/sodium alginate conductive hydrogel. In the range of 0.1 to 100s-1The viscosity decreased from 80 pas to 8 pas at the shear rate of (2). Its self-healing capacity is 78%. When applied to a strain sensor, the sensor can respond to pressure stimulation caused by the bending of an index finger by 40% relative resistance change.
The above embodiments are merely illustrative of the technical solutions of the present invention. The 3D printable electrically conductive self-repairing hydrogel material, its preparation method and application are not limited to those described in the above embodiments, but are subject to the scope defined by the claims. Any modification or supplement or equivalent replacement made by a person skilled in the art on the basis of this embodiment is within the scope of the invention as claimed in the claims.
Claims (6)
1. A preparation method of 3D printing ink is characterized by comprising the following steps:
step 1, dissolving a mixture of sodium dodecyl benzene sulfonate and carbon nano tubes in deionized water, fully stirring, performing ultrasonic dispersion, and centrifuging to obtain a dispersion liquid A;
step 2, adding a certain amount of calcium chloride and polyacrylic acid into the dispersion liquid A, and stirring to obtain a carbon nano tube dispersion liquid B in which the calcium chloride and the polyacrylic acid are dissolved;
step 3, dissolving a certain amount of sodium alginate in a sodium hydroxide solution with a certain concentration, and stirring to obtain an alkaline mixed solution C of the sodium alginate;
step 4, slowly dripping the mixed solution C with the same volume into the dispersion liquid B under the condition of rapid stirring, and obtaining the calcium ion/polyacrylic acid/carbon nano tube/sodium alginate conductive self-repairing hydrogel as 3D printing ink after continuously stirring for a period of time,
wherein, in the step 2, the molar concentrations of the calcium chloride and the polyacrylic acid are 0.1-0.2M and 0.1-0.3M respectively, and the average molecular weight of the polyacrylic acid is 10-25 ten thousand;
in the step 3, the molar concentration of the sodium hydroxide is 0.1-0.2M, and the concentration of the sodium alginate is 0.06-0.12 wt%.
2. The method of preparing a 3D printing ink according to claim 1, wherein:
wherein, in the dispersion liquid A, the concentrations of the sodium dodecyl benzene sulfonate and the carbon nano tube are respectively 0.05 to 0.15 weight percent and 0.05 to 0.25 weight percent.
3. The method of preparing a 3D printing ink according to claim 1, wherein:
in the step 1, the stirring time is 10-20 min, the ultrasonic dispersion time is 30min, the rotating speed is 9000rpm, and the centrifugation time is 20 min.
4. The method of preparing a 3D printing ink according to claim 1, wherein:
wherein the stirring time in the steps 2 and 3 is 10-20 min, and the stirring time in the step 4 is 30 min.
5. A 3D printing ink, characterized in that:
the preparation method of any one of claims 1 to 4.
6. The preparation method of the piezoresistive strain sensor is characterized by comprising the following steps:
printing a designed hydrogel grid structure by using the 3D printing ink of claim 5 and a biological 3D printer in an air pump type extrusion printing mode;
and (3) clamping the printed hydrogel by using two insulating elastomers VHB to form a sandwich structure, and connecting the sandwich structure by using copper electrodes to form the piezoresistive strain sensor.
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