CN111396273A - Photo-thermal stimulation intelligent response actuator film, preparation method and application thereof - Google Patents
Photo-thermal stimulation intelligent response actuator film, preparation method and application thereof Download PDFInfo
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- CN111396273A CN111396273A CN202010168994.3A CN202010168994A CN111396273A CN 111396273 A CN111396273 A CN 111396273A CN 202010168994 A CN202010168994 A CN 202010168994A CN 111396273 A CN111396273 A CN 111396273A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F03—MACHINES OR ENGINES FOR LIQUIDS; WIND, SPRING, OR WEIGHT MOTORS; PRODUCING MECHANICAL POWER OR A REACTIVE PROPULSIVE THRUST, NOT OTHERWISE PROVIDED FOR
- F03G—SPRING, WEIGHT, INERTIA OR LIKE MOTORS; MECHANICAL-POWER PRODUCING DEVICES OR MECHANISMS, NOT OTHERWISE PROVIDED FOR OR USING ENERGY SOURCES NOT OTHERWISE PROVIDED FOR
- F03G7/00—Mechanical-power-producing mechanisms, not otherwise provided for or using energy sources not otherwise provided for
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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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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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The invention discloses a photo-thermal stimulation intelligent response actuator film, a preparation method and application thereof, and belongs to the technical field of polymer compounding. The photothermal stimulation intelligent response actuator film is formed by three films which are sequentially stacked from top to bottom, wherein the first layer is a carbon nano composite film layer of poly (N-isopropyl acrylamide), the second layer is a carbon nano composite film layer, and the third layer is a carbon nano composite film layer of poly (N-isopropyl acrylamide-co-acrylamide). The invention also discloses a preparation method and application of the photo-thermal stimulation intelligent response actuator film. The photo-thermal stimulation intelligent response actuator film can generate large deformation in a wider temperature range in stages, has reversibility in temperature stimulation response, and is particularly suitable for photo-thermal response actuators of soft robots, drug delivery, motors, artificial muscles and the like.
Description
Technical Field
The invention relates to a photo-thermal stimulation intelligent response actuator film, a preparation method and application thereof, belonging to the technical field of polymer compounding.
Background
The intelligent actuator can respond to environmental stimuli (such as pH value, temperature, electricity, chemical energy, solvent, humidity and light), provides well controllable and reversible shape change, and has huge application potential in the fields of wearable computers, artificial muscles, electronic skins, intelligent micro-robots and the like. Accordingly, many researchers have been working on rational design and construction of intelligent drives based on various material systems. Currently, actuators under development or application include shape memory alloys or polymers, stimuli-responsive gels, liquid crystal polymers, and conjugated polymers, among others.
Using light as an external field to stimulate the actuator to obtain a response is an important way. The light responsive material provides programmable and reversible mechanical functions in opto-mechanical actuators with advantages such as contactless actuation, local and remote control, omission of the use of connecting wires or electrodes, etc. As a branch of light-responsive materials, near-infrared (NIR) responsive polymeric nanocomposites are of interest because of their minimal invasiveness and high transparency in "bio-windows". They are generally composed of near-infrared absorbing nanomaterials (e.g., anisotropic metal nanostructures, carbon nanotubes, and graphene) with various soft matrices that can be stimuli-responsive. The carbon material shows high photo-thermal conversion efficiency in a near infrared band; when incorporated into a polymer matrix, it converts the absorbed near infrared light into thermal energy, thereby increasing the temperature of the nanocomposite, and the change in temperature causes a phase change to occur, ultimately causing a stimulus response mechanism to occur. The carbon nano tube and the graphene can be used as photo-thermal conversion medium materials of photo-thermal response actuators, and the high-molecular nano composite material actuators are endowed with excellent comprehensive performance.
Poly (N-isopropylacrylamide) (PNIPAM), as a temperature-sensitive high molecular polymer, has a special response mode to temperature, namely poly (N-isopropylacrylamide) has a low critical solution temperature (L CST), and at the temperature of 30-35 ℃, poly (N-isopropylacrylamide) generates reversible conformational change between hydrophilic and hydrophobic, so that phase separation occurs, poly (N-isopropylacrylamide) contains amide and isopropyl groups in the molecule, if the temperature is below the low critical solution temperature, poly (N-isopropylacrylamide) can be stably existed in water through hydrogen bonds of the amide groups and water, water molecules surround the hydrophobic groups, so that poly (N-isopropylacrylamide) has hydrophilicity and is in a stretching state in an aqueous solution, the temperature is gradually increased, the hydration of poly (N-isopropylacrylamide) and water is weakened, the mutual attraction among the isopropyl groups in the molecule is enhanced, if the temperature is above the low critical solution temperature, the hydrogen bonds are completely broken, the internal structure is stretched by the hydrogen bonds, the hydrogen bonds are converted into a spherical structure, the hydrophobic structure is changed into a spherical structure, the hydrophobic structure is changed into a temperature-controlled, the temperature-controlled composite material is recovered to be used for the development of a low temperature-controlled nano tube, and the temperature is recovered.
In view of the above, it is desirable to provide a novel photo-thermal stimulation smart response actuator film and a method for manufacturing the same, so as to solve the deficiencies of the prior art.
Disclosure of Invention
One of the objectives of the present invention is to provide a photo-thermal stimulation smart response actuator membrane. The photo-thermal stimulation intelligent response actuator film can generate large deformation in stages in a wider temperature range, has reversibility in temperature stimulation response, and is particularly suitable for photo-thermal response actuators of soft robots, drug delivery, motors, artificial muscles and the like.
The technical scheme for solving the technical problems is as follows: the photothermal stimulation intelligent response actuator film is composed of three films which are sequentially stacked from top to bottom, wherein the first layer is a carbon nano composite film layer of poly (N-isopropylacrylamide), the second layer is a carbon nano composite film layer, and the third layer is a carbon nano composite film layer of poly (N-isopropylacrylamide-co-acrylamide).
The principle of the photo-thermal stimulation intelligent response actuator film is as follows:
Poly-N-isopropylacrylamide (PNIPAM) has excellent temperature-sensitive characteristic and generates phase change at a certain temperature (32 ℃) to generate temperature response. The phase change of poly (N-isopropylacrylamide-co-acrylamide) occurs at higher temperature, corresponding temperature response is generated, and the temperature of the response is adjusted according to the number of acrylic acid units. Therefore, the three-layer structure can be utilized to endow the film with large deformation in stages in a wider temperature range, and the temperature stimulus response is reversible.
In the invention, the carbon nano material film is used as a substrate film, and a carbon nano composite film layer of poly N-isopropyl acrylamide and a carbon nano composite film layer of poly (N-isopropyl acrylamide-co-acrylamide) are respectively coated on two surfaces of the substrate film to obtain the three-layer film. Under the irradiation of Near-infrared light (NIR), the three-layer film absorbs heat, firstly makes a first response in a temperature response interval (relatively low temperature) of poly (N-isopropylacrylamide) to generate a first bending deformation, then stimulates poly (N-isopropylacrylamide-co-acrylamide) in a higher temperature interval generated after heat absorption, and makes a second response to generate a second bending deformation; the temperature is lowered and the deformation proceeds in the reverse direction. Compared with single poly-N-isopropylacrylamide stimulus response, poly-N-isopropylacrylamide and poly (N-isopropylacrylamide-co-acrylamide) have synergistic effect in the composite structure of the three-layer membrane of the invention, generate twice deformation, increase deformation amount and expand temperature range, have preliminary program response characteristics, and have great application prospect in the fields of artificial muscles and other artificial intelligent materials.
The photo-thermal stimulation intelligent response actuator film has the beneficial effects that:
1. the photo-thermal stimulation intelligent response actuator film can generate large deformation in stages in a wider temperature range, has reversibility in temperature stimulation response, and is particularly suitable for photo-thermal response actuators of soft robots, drug delivery, motors, artificial muscles and the like.
2. The photo-thermal stimulation intelligent response actuator film can adjust the low critical solution temperature of the second stage according to the actual application requirement, and can perform repeated and cyclic reversible bending in two different temperature response intervals.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the carbon nano composite film layer of the poly (N-isopropylacrylamide-co-acrylamide) is formed by compounding the poly (N-isopropylacrylamide-co-acrylamide) and a carbon nano material; the poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 35-90 ℃, the weight-average molecular weight is 1-100 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is a final product which is prepared by heating N-isopropylacrylamide and acrylamide in a water bath at 40 ℃ for 12 hours in a nitrogen atmosphere according to the mass ratio of (90-65): 10-35, washing and drying.
The adoption of the further beneficial effects is as follows: the poly-N-isopropyl acrylamide has a hydrophilic chain segment and a hydrophobic chain segment, so that the poly-N-isopropyl acrylamide has good processability, temperature sensitivity and mechanical properties. The hydrophilic and hydrophobic groups on the polymer chain are regularly distributed, so that the hydrophilic-hydrophobic conversion is carried out under specific conditions. The inventors of the present application have studied and found that the response temperature of poly (N-isopropylacrylamide-co-acrylamide) increases with the increase in the amide group content (i.e., the proportion of acrylamide) in the copolymer. The acrylamide of the hydrophilic group and the poly-N-isopropylacrylamide are subjected to copolymerization reaction according to a certain mass ratio, so that the response temperature of the poly (N-isopropylacrylamide-co-acrylamide) can be changed. Therefore, the finished photo-thermal stimulation intelligent response actuator film can adjust the low critical solution temperature of the second stage according to the practical application requirement, and can perform repeated and cyclic reversible bending in two different temperature response intervals.
Further, the thickness of the carbon nano composite film layer of the poly N-isopropyl acrylamide is 0.02mm-0.03 mm; the thickness of the carbon nano material film layer is 0.02mm-0.03 mm; the thickness of the carbon nano composite film layer of the poly (N-isopropyl acrylamide-co-acrylamide) is 0.02mm-0.04 mm.
The second objective of the present invention is to provide a method for preparing the above-mentioned photo-thermal stimulation smart response actuator film. The preparation method of the photo-thermal stimulation intelligent response actuator film has the advantages of simple process, convenient operation, wide raw material source, low cost, high production efficiency, environmental protection and energy conservation, and can realize industrial batch production.
The technical scheme for solving the technical problems is as follows: a preparation method of a photo-thermal stimulation intelligent response actuator film comprises the following steps:
step 1: taking a carbon material, dispersing the carbon material in a solvent, wherein the mass volume ratio of the carbon material to the solvent is (3-8) mg, (1-5) ml, and forming a film after uniformly stirring to obtain a carbon nano material film layer;
step 2: dissolving or dispersing poly-N-isopropylacrylamide and the carbon material which is the same as the carbon material in the step 1 into a solvent, wherein the proportion of the poly-N-isopropylacrylamide to the carbon material to the solvent is (5-35) mg, (5-10) ml, and stirring uniformly to obtain a mixed solution A;
and step 3: coating the mixed solution A obtained in the step (2) on the carbon nano material film layer obtained in the step (1) to form a film, so as to obtain a double-layer film of the carbon nano composite material film layer (1) with the carbon nano material film layer and the poly N-isopropylacrylamide;
and 4, step 4: dissolving or dispersing poly (N-isopropylacrylamide-co-acrylamide) and the carbon material which is the same as the carbon material in the step 1 into a solvent, wherein the proportion of the poly (N-isopropylacrylamide-co-acrylamide), the carbon material and the solvent is (5-35) mg, (5-10) ml, and uniformly stirring to obtain a mixed solution B;
and 5: and (3) coating the mixed solution B obtained in the step (4) on one surface, close to the carbon nano-material film layer, of the double-layer film obtained in the step (3) to form a film, so as to obtain a three-layer film, namely the photo-thermal stimulation intelligent response actuator film, of the carbon nano-composite film layer with poly (N-isopropylacrylamide), the carbon nano-material film layer and the carbon nano-composite film layer with poly (N-isopropylacrylamide-co-acrylamide).
The preparation method of the photo-thermal stimulation intelligent response actuator film has the beneficial effects that:
1. the preparation method of the photo-thermal stimulation intelligent response actuator film has the advantages of simple process, convenient operation, wide raw material source, low cost, high production efficiency, environmental protection and energy conservation, and can realize industrial batch production.
2. The photo-thermal stimulation intelligent response actuator film obtained by the invention can generate large deformation in stages in a wider temperature range, and the temperature stimulation response has reversibility, so that the photo-thermal stimulation intelligent response actuator film is particularly suitable for photo-thermal response actuators of soft robots, drug delivery, motors, artificial muscles and the like.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in step 1, the carbon material is any one of graphene oxide, a single-walled carbon nanotube and a multi-walled carbon nanotube.
The adoption of the further beneficial effects is as follows: the above materials are carbon materials suitable for preparing the three-layer thin film of the present invention. The graphene oxide is a product of graphite powder after chemical oxidation and delamination, is a soft material with a non-traditional form, and has the characteristics of a polymer, a colloid and a film. In addition, the graphene oxide has a high specific surface area, and the surface of the graphene oxide has abundant functional groups.
The carbon nano tube is a tubular object formed by curling a graphite hexagonal network, and has a unique nano hollow structure, a closed topological configuration and a spiral structure, so that the carbon nano tube has a large number of special excellent properties, such as high strength, high elasticity, high specific surface area, heat resistance, corrosion resistance, heat conduction, electric conductivity and the like. Carbon nanotubes can be classified into single-walled carbon nanotubes (SWCNTs) and multi-walled carbon nanotubes (MWCNTs) according to the number of carbon atoms forming the wall of the tube.
Further, in the step 1, the thickness of the carbon nano material film layer is 0.02mm-0.03 mm.
Further, in step 2, the poly-N-isopropylacrylamide has a weight average molecular weight of 3 to 20 ten thousand.
The adoption of the further beneficial effects is as follows: the molecular weight can affect the structure and performance of the polymer, and the polymer has better film-forming and mechanical properties at the molecular weight.
Further, in the step 3, the thickness of the carbon nano composite film layer of the poly N-isopropyl acrylamide is 0.02mm-0.03 mm.
Further, in the step 4, the poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 35-90 ℃, the weight-average molecular weight is 1-100 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is a final product obtained by heating N-isopropylacrylamide and acrylamide in a water bath at 40 ℃ for 12 hours in a nitrogen atmosphere according to the mass ratio of (90-65) - (10-35), washing and drying.
The adoption of the further beneficial effects is as follows: the poly-N-isopropyl acrylamide has a hydrophilic chain segment and a hydrophobic chain segment, so that the poly-N-isopropyl acrylamide has good processability, temperature sensitivity and mechanical properties. The hydrophilic and hydrophobic groups on the polymer chain are regularly distributed, so that the hydrophilic-hydrophobic conversion is carried out under specific conditions. The inventors of the present application have studied and found that the response temperature of poly (N-isopropylacrylamide-co-acrylamide) increases with the increase in the amide group content (i.e., the proportion of acrylamide) in the copolymer. The acrylamide of the hydrophilic group and the poly-N-isopropylacrylamide are subjected to copolymerization reaction according to a certain mass ratio, so that the response temperature of the poly (N-isopropylacrylamide-co-acrylamide) can be changed. Therefore, the finished photo-thermal stimulation intelligent response actuator film can adjust the low critical solution temperature of the second stage according to the practical application requirement, and can perform repeated and cyclic reversible bending in two different temperature response intervals.
Further, in the step 4, the concentration of the mixed solution B is 1mg/ml-10 mg/ml.
The adoption of the further beneficial effects is as follows: the two monomers are copolymerized in different proportions to obtain higher low critical solution temperature so as to improve the response temperature of the material to adapt to practical situations.
Further, in step 5, the thickness of the carbon nanocomposite film layer of poly (N-isopropylacrylamide-co-acrylamide) is 0.02mm to 0.04 mm.
Further, in the step 1, the step 2 and the step 4, the solvent is any one of water, N-dimethylformamide and ethanol.
The adoption of the further beneficial effects is as follows: the above solvents can disperse the carbon material, dissolve or disperse poly-N-isopropylacrylamide, and dissolve or disperse poly (N-isopropylacrylamide-co-acrylamide) well.
Further, in the step 1, the step 2 and the step 4, the stirring mode is magnetic stirring, the rotating speed is 90-150 r/min, and the time is 24-72 h.
The adoption of the further beneficial effects is as follows: with the above parameters, the stirring is more uniform and rapid.
Further, in the step 1, the step 3 and the step 5, the film forming mode is any one of suction filtration, air drying and drying.
The adoption of the further beneficial effects is as follows: film formation can be achieved in the above-mentioned several ways.
Furthermore, the flow rate of the suction filtration is 0.1ml/s-1ml/s, and the time is 10s-30 s.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the suction filtration is more thorough.
Furthermore, the air drying temperature is 15-25 ℃, and the time is 8-12 h.
The further beneficial effects of the adoption are as follows: by adopting the parameters, the air drying effect is better.
Furthermore, the drying temperature is 45-55 ℃, and the drying time is 2-3 h.
The further beneficial effects of the adoption are as follows: by adopting the parameters, the drying effect is better.
It is a further object of the present invention to provide a photo-thermal responsive actuator. The photo-thermal response actuator of the present invention. The photo-thermal response actuator has the advantages of temperature programming control, high sensitivity, long service life and the like due to the adoption of the photo-thermal stimulation intelligent response actuator film.
The technical scheme for solving the technical problems is as follows: a photo-thermal response actuator comprises the photo-thermal stimulation intelligent response actuator film.
The photo-thermal response actuator has the beneficial effects that:
the photo-thermal response actuator has the advantages of temperature program control, high sensitivity, long service life and the like due to the adoption of the photo-thermal stimulation intelligent response actuator film.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the photo-thermal responsive actuator includes any one of a soft robot, a drug delivery, a motor, and an artificial muscle.
The adoption of the further beneficial effects is as follows: the soft robot, the drug delivery, the motor and the artificial muscle belong to the field of photo-thermal response actuators, and the photo-thermal stimulation intelligent response actuator film can be used.
Drawings
Fig. 1 is a schematic structural diagram of a double-layer film of a carbon nanocomposite film layer (1) having a carbon nanomaterial film layer (2) and poly N-isopropylacrylamide obtained in step 3 in the method for manufacturing a thermal stimulation smart response actuator film of the present invention.
Fig. 2 is a schematic structural diagram of a three-layer film having a carbon nanomaterial film layer (2), a carbon nanocomposite film layer (1) of poly N-isopropylacrylamide and a carbon nanocomposite film layer (3) of poly (N-isopropylacrylamide-co-acrylamide) obtained in step 5 in the method for preparing a thermal stimulation intelligent response actuator film of the present invention.
In the drawings, the reference numerals have the following meanings:
1. a carbon nano composite film layer of poly N-isopropyl acrylamide, a carbon nano composite film layer 2, a carbon nano composite film layer 3, and a carbon nano composite film layer of poly (N-isopropyl acrylamide-co-acrylamide).
FIG. 3 is a schematic diagram of a photothermal stimulation smart response actuator membrane of the present invention performing a secondary bending response.
Detailed Description
The principles and features of this invention are described below in conjunction with the following detailed drawings, which are given by way of illustration only and are not intended to limit the scope of the invention.
Example 1
The preparation method of the photo-thermal stimulation intelligent response actuator film comprises the following steps:
step 1: and (3) dispersing 3mg of graphene oxide in 1ml of deionized water, magnetically stirring for 72 hours at the rotating speed of 90 revolutions per minute, uniformly stirring, performing suction filtration for 20 seconds at the flow speed of 0.5ml per second, and forming a film to obtain the carbon nano material film layer 2 with the thickness of 0.02 mm.
Step 2: dissolving 5mg of poly-N-isopropylacrylamide (weight average molecular weight is 3 thousand) and 5mg of graphene oxide in 10ml of deionized water, magnetically stirring for 72 hours at the rotation speed of 90 revolutions per minute, and uniformly stirring to obtain a mixed solution A. Wherein the particle size of the graphene oxide is 0.2-10 μm.
And step 3: and (3) coating the mixed solution A obtained in the step (2) on the carbon nano material film layer 2 obtained in the step (1), and performing suction filtration for 20s at the flow rate of 0.5ml/s to form a film to obtain the double-layer film of the carbon nano composite material film layer 1 with the carbon nano material film layer 2 and the poly N-isopropylacrylamide, wherein the thickness of the carbon nano composite material film layer 1 of the poly N-isopropylacrylamide is 0.02mm, and is specifically shown in figure 1.
And 4, step 4: dissolving 5mg of poly (N-isopropylacrylamide-co-acrylamide) and 5mg of graphene oxide in 10ml of deionized water, magnetically stirring for 72 hours at the rotation speed of 90 revolutions per minute, and uniformly stirring to obtain a mixed solution B.
The poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 35 ℃, the weight-average molecular weight is 1 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is prepared by the following method:
in a three-neck round-bottom flask, 8.5g of deionized water was added, 1.28g of N-isopropylacrylamide and 0.22g of acrylamide (in a mass ratio of 85:15) were added, respectively, and after stirring, the mixture was heated at 40 ℃ for 20min to remove oxygen, thereby obtaining an aqueous solution of the mixture.
Two constant-pressure separating funnels are placed above the three-neck round-bottom flask, 0.75 mol% of potassium persulfate and 1ml of deionized water are added into one constant-pressure separating funnel, 0.75 mol% of sodium sulfite and 1ml of deionized water are added into the other constant-pressure separating funnel, the dropping speed of the two constant-pressure separating funnels is controlled to be 10 s/drop, and the two constant-pressure separating funnels are dropped into the lower three-neck round-bottom flask.
The aqueous solution of the mixture was stirred at 40 ℃ for 12h under nitrogen.
Dissolving the obtained product in a mixed solution of acetone and ethanol (volume ratio of 1:1), precipitating in excess ether, and vacuum drying at 40 deg.C (1 × 10)-1Pa) for 8h to obtain the poly (N-isopropyl acrylamide-co-acrylamide).
And 5: and (3) coating the mixed solution B obtained in the step (4) on one surface, close to the carbon nano-material film layer 2, of the double-layer film obtained in the step (3), performing suction filtration for 20s at a flow rate of 0.5ml/s to form a film, and thus obtaining the three-layer film, namely the photo-thermal stimulation intelligent response actuator film, of the carbon nano-composite film layer 1 with poly (N-isopropylacrylamide), the carbon nano-material film layer 2 and the carbon nano-composite film layer 3 with poly (N-isopropylacrylamide-co-acrylamide). Wherein the thickness of the carbon nanocomposite film layer 3 of poly (N-isopropylacrylamide-co-acrylamide) is 0.02mm, as shown in FIG. 2.
The photo-thermal stimulation intelligent response actuator film prepared in the embodiment is irradiated for 5min under near infrared light to perform first bending response. The irradiation was continued for another 8min for a second bend response. After the light irradiation is stopped, the photo-thermal stimulation intelligent response actuator film is restored to the initial state within 3 min. The reversible bending can be performed in more than 100 repeated cycles according to the above-described operation, as shown in fig. 3.
Example 2
The preparation method of the photo-thermal stimulation intelligent response actuator film comprises the following steps:
step 1: and (3) dispersing 6mg of single-walled carbon nanotubes in 3ml of N, N-dimethylformamide, magnetically stirring for 48 hours at the rotating speed of 120 revolutions per minute, uniformly stirring, drying for 2 hours at 55 ℃, and forming a film to obtain the carbon nanomaterial film layer 2 with the thickness of 0.03 mm. Wherein the grain diameter of the single-wall carbon nano tube is 1nm-2 nm.
Step 2: dissolving 25mg of poly-N-isopropylacrylamide (with a weight-average molecular weight of 7 ten thousand) and 25mg of graphene oxide in 10ml of deionized water, magnetically stirring for 48 hours at a rotation speed of 120 revolutions per minute, and uniformly stirring to obtain a mixed solution A.
And step 3: and (3) coating the mixed solution A obtained in the step (2) on the carbon nano material film layer 2 obtained in the step (1), drying for 2h at 55 ℃ to form a film, and obtaining the double-layer film of the carbon nano composite material film layer 1 with the carbon nano material film layer 2 and the poly N-isopropylacrylamide, wherein the thickness of the carbon nano composite material film layer 1 of the poly N-isopropylacrylamide is 0.03mm, and is specifically shown in figure 1.
And 4, step 4: dissolving 25mg of poly (N-isopropylacrylamide-co-acrylamide) and 25mg of single-walled carbon nanotubes in 10ml of deionized water, magnetically stirring for 48 hours at the rotating speed of 120 revolutions per minute, and uniformly stirring to obtain a mixed solution B.
The poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, has a response temperature of 60 ℃ and a weight-average molecular weight of 50 ten thousand, and is prepared by the following method:
in a three-neck round-bottom flask, 8.5g of deionized water was added, 1.13g of N-isopropylacrylamide and 0.37g of acrylamide (in a mass ratio of 75:25) were added, respectively, and after stirring, the mixture was heated at 40 ℃ for 20min to remove oxygen, thereby obtaining an aqueous solution of the mixture.
Two constant-pressure separating funnels are placed above the three-neck round-bottom flask, 0.75 mol% of potassium persulfate and 1ml of deionized water are added into one constant-pressure separating funnel, 0.75 mol% of sodium sulfite and 1ml of deionized water are added into the other constant-pressure separating funnel, the dropping speed of the two constant-pressure separating funnels is controlled to be 10 s/drop, and the two constant-pressure separating funnels are dropped into the lower three-neck round-bottom flask.
The aqueous solution of the mixture was stirred at 40 ℃ for 12h under nitrogen.
Dissolving the obtained product in a mixed solution of acetone and ethanol (volume ratio of 1:1), precipitating in excess ether, and vacuum drying at 40 deg.C (1 × 10)-1Pa) for 8h to obtain the poly (N-isopropyl acrylamide-co-acrylamide).
And 5: and (3) coating the mixed solution B obtained in the step (4) on one surface, close to the carbon nano-material film layer 2, of the double-layer film obtained in the step (3), drying at 55 ℃ for 2h, and forming a film to obtain a three-layer film, namely a photo-thermal stimulation intelligent response actuator film, of the carbon nano-composite film layer 1 with poly (N-isopropylacrylamide), the carbon nano-material film layer 2 and the carbon nano-composite film layer 3 with poly (N-isopropylacrylamide-co-acrylamide). Wherein the thickness of the carbon nanocomposite film layer 3 of poly (N-isopropylacrylamide-co-acrylamide) is 0.03mm, as shown in FIG. 2.
The photo-thermal stimulation intelligent response actuator film prepared in the embodiment is irradiated for 2min under near infrared light to perform first bending response. The irradiation was continued for 4min again for a second bend response. After the illumination is stopped, the photo-thermal stimulation intelligent response actuator film is restored to the initial state within 2 min. The reversible bending can be performed in more than 800 cycles as described above, as shown in fig. 3.
Example 3
The preparation method of the photo-thermal stimulation intelligent response actuator film comprises the following steps:
step 1: and (2) dispersing 8mg of multi-wall carbon nano tubes in 5ml of ethanol, magnetically stirring for 24 hours at the rotating speed of 150 revolutions per minute, uniformly stirring, and air-drying for 10 hours at 20 ℃ to form a film, thus obtaining the carbon nano material film layer 2 with the thickness of 0.02 mm. Wherein the particle size of the multi-wall carbon nano-tube is 20nm-40 nm.
Step 2: dissolving 35mg of poly-N-isopropylacrylamide (with the weight-average molecular weight of 20 ten thousand) and 15mg of multi-walled carbon nanotubes in 5ml of N, N-dimethylformamide, magnetically stirring for 24 hours at the rotation speed of 150 revolutions per minute, and uniformly stirring to obtain a mixed solution A.
And step 3: and (3) coating the mixed solution A obtained in the step (2) on the carbon nano material film layer 2 obtained in the step (1), air-drying for 10 hours at 20 ℃, and forming a film to obtain the double-layer film of the carbon nano composite material film layer 1 with the carbon nano material film layer 2 and the poly N-isopropylacrylamide, wherein the thickness of the carbon nano composite material film layer 1 of the poly N-isopropylacrylamide is 0.02mm, and is specifically shown in figure 1.
And 4, step 4: dissolving 35mg of poly (N-isopropylacrylamide-co-acrylamide) and 15mg of single-walled carbon nanotube into 5ml of N, N-dimethylformamide, magnetically stirring for 24 hours at the rotation speed of 150 revolutions per minute, and uniformly stirring to obtain a mixed solution B.
The poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 90 ℃, the weight-average molecular weight is 100 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is prepared by the following method:
in a three-neck round-bottom flask, 8.5g of deionized water was added, 0.98g of N-isopropylacrylamide and 0.52g of acrylamide (in a mass ratio of 65:35) were added, respectively, and after stirring, the mixture was heated at 40 ℃ for 20min to remove oxygen, thereby obtaining an aqueous solution of the mixture.
Two constant-pressure separating funnels are placed above the three-neck round-bottom flask, 0.75 mol% of potassium persulfate and 1ml of deionized water are added into one constant-pressure separating funnel, 0.75 mol% of sodium sulfite and 1ml of deionized water are added into the other constant-pressure separating funnel, the dropping speed of the two constant-pressure separating funnels is controlled to be 10 s/drop, and the two constant-pressure separating funnels are dropped into the lower three-neck round-bottom flask.
The aqueous solution of the mixture was stirred at 40 ℃ for 12h under nitrogen.
Dissolving the obtained product in a mixed solution of acetone and ethanol (volume ratio of 1:1), precipitating in excess ether, and vacuum drying at 40 deg.C (1 × 10)-1Pa) for 8h to obtain the poly (N-isopropyl acrylamide-co-acrylamide).
And 5: and (3) coating the mixed solution B obtained in the step (4) on one surface, close to the carbon nano-material film layer 2, of the double-layer film obtained in the step (3), air-drying at 20 ℃ for 10 hours to form a film, and thus obtaining a three-layer film, namely a photo-thermal stimulation intelligent response actuator film, of the carbon nano-composite film layer 1 with poly (N-isopropylacrylamide), the carbon nano-material film layer 2 and the carbon nano-composite film layer 3 with poly (N-isopropylacrylamide-co-acrylamide). Wherein the thickness of the carbon nanocomposite film layer 3 of poly (N-isopropylacrylamide-co-acrylamide) is 0.04mm, as shown in FIG. 2.
The photo-thermal stimulation intelligent response actuator film prepared in the embodiment is irradiated for 3min under near infrared light to perform first bending response. And continuing for 7min again, and performing second bending response. After the light irradiation is stopped, the photo-thermal stimulation intelligent response actuator film is restored to the initial state within 4 min. The reversible bending can be performed in more than 400 repeated cycles according to the above-described operation, as shown in fig. 3.
Experimental example 1
The influence of the carbon nano-material film layer on the photo-thermal stimulation intelligent response actuator film is examined by comparing whether the carbon nano-material film layer exists or not.
The two-layer film of comparative example 1 is different from example 1 in that no carbon nanomaterial film layer is provided and other parameters are the same, and the specific preparation method comprises the following steps:
step 1: dissolving 5mg of poly-N-isopropylacrylamide (weight average molecular weight is 3 thousand) and 5mg of graphene oxide in 10ml of deionized water, magnetically stirring for 72 hours at the rotation speed of 90 revolutions per minute, and uniformly stirring to obtain a mixed solution A. And (3) performing suction filtration for 20s at the flow rate of 0.5ml/s to form a film, thus obtaining the poly-N-isopropylacrylamide carbon nano composite film layer with the thickness of 0.02 mm.
Step 2: dissolving 5mg of poly (N-isopropylacrylamide-co-acrylamide) (the weight average molecular weight is 1 ten thousand) and 5mg of graphene oxide in 10ml of deionized water, magnetically stirring for 72 hours at the rotation speed of 90 revolutions per minute, and uniformly stirring to obtain a mixed solution B. Wherein the poly (N-isopropyl acrylamide-co-acrylamide) is prepared from N-isopropyl acrylamide and acrylamide according to a mass ratio of 85:15 by polymerization.
And step 3: and (3) coating the mixed solution B obtained in the step (2) on the carbon nano composite film layer of the poly (N-isopropylacrylamide) obtained in the step (1), and performing suction filtration for 20s at the flow rate of 0.5ml/s to form a film, so as to obtain a double-layer film comprising the carbon nano composite film layer of the poly (N-isopropylacrylamide) and the carbon nano composite film layer of the poly (N-isopropylacrylamide-co-acrylamide), wherein the thickness of the carbon nano composite film layer 1 of the poly (N-isopropylacrylamide-co-acrylamide) is 0.02 mm.
The three-layer film obtained in example 1 and the two-layer film obtained in comparative example 1 were compared in photo-thermal drive response capabilities. The film obtained in comparative example 1 could not be bent under irradiation of near infrared light. When the temperature of the oven reaches 35 ℃, the first deformation is quickly generated, and when the temperature of the oven reaches 40-95 ℃, the second deformation is quickly generated. Returning to the original state at room temperature.
And (4) conclusion: the two-layer film of comparative example 1, which has no base carbon film layer, cannot perform energy conversion between photo and heat under illumination, and thus cannot induce a phase change of a polymer. Temperature response is possible after sufficient heat absorption in the oven. Therefore, the substrate carbon film layer is an energy conversion supporter of the photo-thermal stimulation intelligent response actuator film.
Experimental example 2
The influence of the carbon nanocomposite film layer of poly (N-isopropylacrylamide-co-acrylamide) on the photo-thermal stimulation intelligent response actuator film of the invention is examined by comparing whether the carbon nanocomposite film layer of poly (N-isopropylacrylamide-co-acrylamide) exists or not.
The two-layer film of comparative example 2, different from example 1, was prepared without the carbon nanocomposite film layer of poly (N-isopropylacrylamide-co-acrylamide) and with the same other parameters by the following specific method:
step 1: and (3) dispersing 3mg of graphene oxide in 1ml of deionized water, magnetically stirring for 72 hours at the rotating speed of 90 revolutions per minute, uniformly stirring, performing suction filtration for 20 seconds at the flow speed of 0.5ml per second, and forming a film to obtain the carbon nano material film layer 2 with the thickness of 0.02 mm.
Step 2: dissolving 5mg of poly-N-isopropylacrylamide (weight average molecular weight is 3 thousand) and 5mg of graphene oxide in 10ml of deionized water, magnetically stirring for 72 hours at the rotation speed of 90 revolutions per minute, and uniformly stirring to obtain a mixed solution A.
And step 3: and (3) coating the mixed solution A obtained in the step (2) on the carbon nano material film layer 2 obtained in the step (1), and performing suction filtration for 20s at the flow rate of 0.5ml/s to form a film, so as to obtain the double-layer film of the carbon nano composite material film layer 1 with the carbon nano material film layer 2 and the poly N-isopropylacrylamide. Wherein the thickness of the carbon nano composite material film layer 1 of the poly N-isopropyl acrylamide is 0.02 mm.
The three-layer film obtained in example 1 and the two-layer film obtained in comparative example 2 were compared in photo-thermal drive response capabilities. The film obtained in comparative example 2 was irradiated with near infrared light for 5min to perform a first bending response. Irradiation was continued for another 4min without a second bend response.
And (4) conclusion: the double-layered film of comparative example 2 can perform bending response only at a relatively low temperature, and has a limited degree of bending, and cannot achieve high-temperature high-level bending response. Therefore, the carbon nano composite material film layer of poly (N-isopropyl acrylamide-co-acrylamide) is the key of the finished product photo-thermal stimulation intelligent response brake film whether to realize repeated and cyclic reversible bending in two different temperature response intervals.
Experimental example 3
Poly (N-isopropylacrylamide-co-acrylamide) is prepared by respectively adopting N-isopropylacrylamide and acrylamide with different mass ratios, and the influence of the N-isopropylacrylamide and the acrylamide with different mass ratios on the poly (N-isopropylacrylamide-co-acrylamide) is examined by examining the low Critical Solution Temperature (L power Critical Solution Temperature, L CST value for short) of a poly (N-isopropylacrylamide-co-acrylamide) film.
Adding 8.5g of deionized water into a three-neck round-bottom flask, then respectively adding N-isopropylacrylamide and acrylamide (the mass ratio of the N-isopropylacrylamide to the acrylamide is 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 100:0), uniformly stirring, and then heating at 40 ℃ for deoxygenation for 20min to obtain an aqueous solution of a mixture.
Two constant-pressure separating funnels are placed above the three-neck round-bottom flask, 0.75 mol% of potassium persulfate and 1ml of deionized water are added into one constant-pressure separating funnel, 0.75 mol% of sodium sulfite and 1ml of deionized water are added into the other constant-pressure separating funnel, the dropping speed of the two constant-pressure separating funnels is controlled to be 10 s/drop, and the two constant-pressure separating funnels are dropped into the lower three-neck round-bottom flask.
The aqueous solution of the mixture was stirred at 40 ℃ for 12h under nitrogen.
Dissolving the obtained product in a mixed solution of acetone and ethanol (volume ratio of 1:1), precipitating in excess ether, and vacuum drying at 40 deg.C (1 × 10)-1Pa) for 8h to obtain the poly (N-isopropylacrylamide-co-acrylamide) with different monomer feed ratios. The chemical reaction formula is as follows:
respectively taking 50mg of poly (N-isopropylacrylamide-co-acrylamide) with different monomer feed ratios, dissolving the poly (N-isopropylacrylamide-co-acrylamide) in 10ml of deionized water, dripping the solution on a polytetrafluoroethylene plate to form a film, drying the film in vacuum at 50 ℃ to obtain a poly (N-isopropylacrylamide-co-acrylamide) film, and respectively observing the low critical solution temperature of the poly (N-isopropylacrylamide-co-acrylamide) film. The results are shown in Table 1.
TABLE 1L CST values for poly (N-isopropylacrylamide-co-acrylamide) films
And (4) conclusion:
the poly-N-isopropyl acrylamide has a hydrophilic chain segment and a hydrophobic chain segment, so that the poly-N-isopropyl acrylamide has good processability, temperature sensitivity and mechanical properties. The hydrophilic and hydrophobic groups on the polymer chain are regularly distributed, so that the hydrophilic-hydrophobic conversion is carried out under specific conditions. The content of amide groups in the copolymer is increased by introducing acrylamide with hydrophilic groups, so that the hydrophilicity of the poly (N-isopropylacrylamide-co-acrylamide) and water is higher, more heat is required to be absorbed to reach higher temperature to destroy intermolecular hydrogen bonds, and the lower critical solution temperature is increased. The inventors of the present application have studied and found that the response temperature of poly (N-isopropylacrylamide-co-acrylamide) increases with the increase in the amide group content (i.e., the proportion of acrylamide) in the copolymer. Therefore, the finished photo-thermal stimulation intelligent response actuator film can adjust the low critical solution temperature of the second stage according to the practical application requirement, and can perform repeated and cyclic reversible bending in two different temperature response intervals.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The photo-thermal stimulation intelligent response actuator film is characterized by being formed by three films which are sequentially stacked from top to bottom, wherein the first layer is a carbon nano composite film layer (1) of poly (N-isopropylacrylamide), the second layer is a carbon nano composite film layer (2), and the third layer is a carbon nano composite film layer (3) of poly (N-isopropylacrylamide-co-acrylamide).
2. The photothermal stimulation smart response actuator membrane according to claim 1, wherein the carbon nanocomposite membrane layer (3) of poly (N-isopropylacrylamide-co-acrylamide) is compounded of poly (N-isopropylacrylamide-co-acrylamide) and carbon nanomaterial; the poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 35-90 ℃, the weight-average molecular weight is 1-100 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is a final product which is prepared by heating N-isopropylacrylamide and acrylamide in a water bath at 40 ℃ for 12 hours in a nitrogen atmosphere according to the mass ratio of (90-65): 10-35, washing and drying.
3. The photo-thermal stimulation smart response actuator membrane as claimed in claim 1, wherein the thickness of the carbon nanocomposite membrane layer (1) of poly-N-isopropylacrylamide is 0.02mm-0.03 mm; the thickness of the carbon nano material film layer (2) is 0.02mm-0.03 mm; the thickness of the carbon nano composite material film layer (3) of the poly (N-isopropyl acrylamide-co-acrylamide) is 0.02mm-0.04 mm.
4. A preparation method of a photo-thermal stimulation intelligent response actuator film is characterized by comprising the following steps:
step 1: taking a carbon material, dispersing the carbon material in a solvent, wherein the mass volume ratio of the carbon material to the solvent is (3-8) mg, (1-5) ml, and forming a film after uniformly stirring to obtain a carbon nano material film layer (2);
step 2: dissolving or dispersing poly-N-isopropylacrylamide and the carbon material which is the same as the carbon material in the step 1 into a solvent, wherein the proportion of the poly-N-isopropylacrylamide to the carbon material to the solvent is (5-35) mg, (5-10) ml, and stirring uniformly to obtain a mixed solution A;
and step 3: coating the mixed solution A obtained in the step (2) on the carbon nano material film layer (2) obtained in the step (1) to form a film, so as to obtain a double-layer film of the carbon nano composite material film layer (1) with the carbon nano material film layer (2) and the poly N-isopropylacrylamide;
and 4, step 4: dissolving or dispersing poly (N-isopropylacrylamide-co-acrylamide) and the carbon material which is the same as the carbon material in the step 1 into a solvent, wherein the proportion of the poly (N-isopropylacrylamide-co-acrylamide), the carbon material and the solvent is (5-35) mg, (5-10) ml, and uniformly stirring to obtain a mixed solution B;
and 5: and (3) coating the mixed solution B obtained in the step (4) on one surface, close to the carbon nano material film layer (2), of the double-layer film obtained in the step (3) to form a film, so as to obtain a three-layer film, namely a photo-thermal stimulation intelligent response actuator film, of the carbon nano composite material film layer (1) with poly (N-isopropylacrylamide), the carbon nano material film layer (2) and the carbon nano composite material film layer (3) with poly (N-isopropylacrylamide-co-acrylamide).
5. The method for preparing a photothermal stimulation smart response actuator membrane according to claim 4, wherein in step 1, the carbon material is any one of graphene oxide, single-walled carbon nanotubes, and multi-walled carbon nanotubes; the thickness of the carbon nano material film layer (2) is 0.02mm-0.03 mm; in the step 2, the weight average molecular weight of the poly-N-isopropylacrylamide is 3 thousand to 20 ten thousand; in the step 3, the thickness of the carbon nano composite material film layer (1) of the poly N-isopropyl acrylamide is 0.02mm-0.03 mm.
6. The method for preparing a photothermal stimulation smart response actuator film according to claim 4, wherein in step 4, the poly (N-isopropylacrylamide-co-acrylamide) is an alternating copolymer or a random copolymer, the response temperature is 35 ℃ to 90 ℃, the weight average molecular weight is 1 ten thousand to 100 ten thousand, and the poly (N-isopropylacrylamide-co-acrylamide) is a final product obtained by heating N-isopropylacrylamide and acrylamide in a water bath at 40 ℃ in a nitrogen atmosphere according to a mass ratio of (90-65): (10-35) for 12 hours, washing and drying; the concentration of the mixed solution B is 1mg/ml-10 mg/ml; in the step 5, the thickness of the carbon nano composite film layer (3) of the poly (N-isopropylacrylamide-co-acrylamide) is 0.02mm-0.04 mm.
7. The method for manufacturing a photo-thermal stimulation smart response actuator membrane as claimed in claim 4, wherein in the steps 1, 2 and 4, the solvent is any one of water, N-dimethylformamide and ethanol; the stirring mode is magnetic stirring, the rotating speed is 90-150 r/min, and the time is 24-72 h.
8. The method for manufacturing a photothermal stimulation smart response actuator film according to any one of claims 4 to 7, wherein in step 1, step 3, and step 5, the film is formed by any one of suction filtration, air drying, and baking.
9. A photo-thermal responsive actuator comprising the photo-thermal stimulation smart responsive actuator film of claims 1-3.
10. The photo-thermally responsive actuator of claim 9, wherein the photo-thermally responsive actuator comprises any one of a soft robot, a drug delivery, a motor, and an artificial muscle.
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