CN112391831A - Preparation method of electrothermal driving artificial muscle with large strain and rapid response - Google Patents
Preparation method of electrothermal driving artificial muscle with large strain and rapid response Download PDFInfo
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Abstract
The invention belongs to the technical field of material science and soft robot driving, and particularly relates to a preparation method of an electrothermal driving carbon nanotube fiber artificial muscle with large strain and rapid response. The invention provides a method for preparing fiber artificial muscle by mixing a variable hydrophilic-hydrophobic polymer and carbon nanotube fiber, and the method is applied to the field of intelligent robots. Preparing a spinnable carbon nanotube fiber, and compounding the carbon nanotube fiber with a variable hydrophilic and hydrophobic polymer by a composite doping method to prepare a quick-response composite carbon nanotube fiber artificial muscle; the expansion and contraction of the strain control device is controlled in an electric heating driving mode, water mist is led into the strain control device, and the purpose of large-strain quick response is achieved.
Description
Technical Field
The invention belongs to the technical field of material science and soft robot driving, and particularly relates to a preparation method of an electrothermal driving carbon nanotube fiber artificial muscle with large strain and rapid response.
Background
With the continuous and deep development of soft robots and the strong demand for intelligent mechanical systems, people are making efforts to develop various flexible driving devices. Compared with the traditional rigid driver, the flexible driver has the advantages of high safety, high degree of freedom of movement, strong adaptability and the like. An artificial muscle is a flexible driver that can be deformed under the excitation of external signals (light, electricity, heat, etc.). The main materials for manufacturing the artificial muscle include dielectric elastomers, shape memory alloys, nylon wires, graphene fibers, carbon nanotube fibers and the like. Among them, carbon nanotube fibers are one of various macroscopic assemblies of Carbon Nanotubes (CNTs), and inherit the excellent electrical conductivity, thermal conductivity, mechanical strength, light weight, and the like of carbon nanotubes. The carbon nanotube fiber has good structural flexibility and has great application prospect in the fields of artificial muscles, soft robots, flexible mechanical technology and the like.
The driving modes of the artificial muscle based on the carbon nano tube fiber mainly comprise electric heating driving, solvent adsorption and desorption, electrochemical driving and the like. The solvent desorption is greatly influenced by the external environment, and has the defects of low output response rate, low output energy for external work and the like. Although the electrochemical driving has high energy conversion efficiency and large driving strain, the electrolyte is required to be used, the overall mass of the artificial muscle is increased, and the actual use and operation are inconvenient. The electrothermal driving fiber artificial muscle is easy to operate and high in controllability, and is often used in experimental research and industrial application. However, the electrothermal driving carbon nanotube fiber artificial muscle has the problems of slow response speed and the like due to slow heat dissipation process. Research shows that the heat dissipation speed of the artificial muscle can be increased by reducing the cross section of the artificial muscle, but the mass and the output energy of the artificial muscle are reduced.
The invention aims to overcome the defects of slow response and large heat dissipation of the conventional electric heating driven artificial muscle, improve the output strain, response rate and other performances of the fiber artificial muscle, provides a method for preparing the fiber artificial muscle by mixing a variable hydrophilic and hydrophobic polymer and carbon nanotube fibers, and applies the method to the field of intelligent robots. The method specifically comprises the steps of preparing a spinnable carbon nanotube fiber, and compounding the carbon nanotube fiber with a variable hydrophilic and hydrophobic polymer by a composite doping method to prepare the quick-response composite carbon nanotube fiber artificial muscle; and then the mechanical and electrical properties of the fiber artificial muscle and the capacity of doing work externally are researched.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a large-strain quick-response electrothermal driving carbon nanotube fiber artificial muscle.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing electrothermal-driven carbon nanotube fiber artificial muscle with large strain and fast response is characterized in that a carbon nanotube film prepared by carbon nanotube vertical array spinning is adopted, and the film is twisted and then naturally untwisted. In order to remove impurities in the fibers and enhance the tensile strength of the fibers, the twisted fibers are subjected to vacuum high-temperature treatment (heating for 2min at 2000 ℃) and then slightly acidized to improve the hydrophilic performance of the fibers. And then uniformly spraying a material with hydrophilic and hydrophobic properties capable of being changed by temperature change into the treated carbon nanotube fibers, controlling the expansion and contraction of the carbon nanotube fibers in an electric heating driving mode, and introducing water mist to the carbon nanotube fibers. The working principle is as follows: when the temperature of the artificial muscle is room temperature, the surface of the muscle has hydrophilic property. After the power is switched on, the muscles contract, and simultaneously absorb water mist to promote the expansion of the muscles, so that the contraction rate is increased; when the temperature exceeds a certain temperature, the muscle skin polymer exhibits hydrophobicity. The water droplet can not stop on the muscle surface, so water smoke can constantly take away the heat of muscle, accelerates its cooling, has shortened recovery time. Thereby achieving the purpose of quick response to large strain.
The material with the hydrophile-lyophile property which can be changed by temperature change is polystyrene/poly N-isopropyl acrylamide (PS/PNIPAM).
The spinnable carbon nanotube array may be prepared by Chemical Vapor Deposition (CVD) in the prior art. First, methane is used as a carbon source, and ferrocene and thiophene vapor are respectively used as a catalyst and a growth promoter. Helium is used as carrier gas to introduce the gaseous raw materials into the reactor. The synthesis of carbon nanotubes is carried out at high temperatures (above 700 ℃). And the reaction is carried out in a hydrogen atmosphere. Thereby obtaining the multi-wall carbon nano-tube array.
The carbon nanotube film can be directly and continuously drawn out from the carbon nanotube vertical array.
The quick-response electric heating driving artificial muscle can be prepared by the following detailed steps:
the method comprises the following steps: the carbon nanotube film is continuously twisted into a helical fiber. One end of a carbon nano tube film is fixed with the output shaft of the motor, and a weight of 10g is hung at the other end of the carbon nano tube film. The motor twisted the film at 100rpm, and the film formed a helical carbon nanotube fiber. The specific operation steps are shown in the attached figure 1. The hanging weight related to the first step can not rotate along with the motor, so as to prevent the untwisting of the fibers in the twisting process. The spring index k of the spring-like fiber can be controlled to be D/D by hanging weights with different weights and controlling the total number of turns of the motor.
Wherein k is the spring index, D is the diameter of the helical structure, and D is the diameter of the twisted carbon nanotube fiber.
Step two: and (3) freely untwisting the twisted fibers and carrying out vacuum high-temperature annealing treatment. Two ends of the freely untwisted fiber are connected with a power supply, the upper end of the freely untwisted fiber is fixed, and a heavy object is hung at the lower end of the freely untwisted fiber. The weight size is 20% of the breaking tensile strength of the carbon nanotube fiber. The voltage was again slowly increased to bring the temperature to 2000 ℃. The vacuum high-temperature annealing time of the fiber is 2 min.
Step three: and (4) performing hydrophilization treatment on the fiber annealed in the second step. Since the original carbon nanotube fiber has hydrophobic characteristics, it is necessary to perform a hydrophilization treatment so that it rapidly absorbs water molecules and increases strain and response rate. There are generally two types of treatment methods for changing the hydrophilic and hydrophobic properties of materials. Firstly, surface microstructure treatment is carried out, and the Wenzel model shows that: the fine rough structure can increase the hydrophilic and hydrophobic properties of the material; secondly, the material is chemically modified, usually some hydrophilic groups are introduced as follows: hydroxyl, carboxyl, sulfonic acid, phosphoric acid, and the like.
Furthermore, the fiber is soaked in a mixed solution of concentrated sulfuric acid and concentrated nitric acid (the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 3: 1) for hydrophilization treatment, and the soaking time is 1 h. As a result, the fiber surface soaked by strong acid has a plurality of fold structures, and the quantity of adsorbed water molecules is increased. In addition, hydrophilic groups such as hydroxyl and carboxyl can be introduced in the process, so that the hydrophilicity of the fiber is improved. Meanwhile, the strong acid treatment of the fiber can destroy the structure of the fiber and reduce the mechanical property of the fiber. Therefore, the soaking time is controlled within a small time.
Step four: a material (PS/PNIPAM mixed solution) with hydrophilic and hydrophobic characteristics capable of changing along with temperature is uniformly coated on the surfaces of carbon nanotube fibers fixed and tensioned at two ends. Dried at room temperature for one hour. The operation method is shown in figure 2.
Further, the hydrophilic and hydrophobic properties of the film prepared by coating the PS/PNIPAM mixed solution on the carbon nanotube fibers in the fourth step can be changed along with the temperature. When the temperature is room temperature (25 ℃), it appears hydrophilic. When the temperature is raised to 45 ℃, it appears hydrophobic. (Kanidi M, Papagiannopoulos A, Matei A, Dinescu M, Pispas S, Kandyla M.applied Surface science.2020; 527:146841.)
Further, the specific preparation method of the solution is as follows: PS1448 and PNIPAM265 were measured at 1: 1 was mixed and dissolved in Tetrahydrofuran (THF) to constitute a polymer solution having a mass percentage concentration of 5 wt%.
Step five: the large-stroke quick-response carbon nanotube fiber artificial muscle driving device is shown in figure 3. The device specifically comprises a direct-current power supply, a non-contact displacement sensor, a three-way glass tube, fiber artificial muscles and a heavy object. The top end of the artificial muscle is fixed on the iron support device and is positioned in the three-way glass tube, a certain weight is hung at the bottom of the artificial muscle, and the non-contact displacement sensor below the weight is guaranteed to be hung in a centering mode. The two ends of the artificial muscle are connected with the direct-current power supply, the extension and contraction of the artificial muscle are realized by controlling the switch of the power supply, and water mist is continuously introduced into the glass tube in the driving process. The specific process is as follows: the power switch is closed, and the generated joule heat causes the artificial muscle fiber to expand radially and shorten axially. And at this time, the polymer on the surface of the fiber is hydrophilic, and water molecules in the mist are adsorbed. Water molecules enter the outer layer of the carbon nanotube fiber to cause macroscopic expansion of the fiber, and the contraction stroke is increased. When the power is turned off, heat is dissipated and the fibers stretch. At the moment, the polymer at high temperature is changed into hydrophobic property, water molecules can not stay on the fibers, and water drops flowing down continuously can take away heat, so that the speed of a return stroke is increased. During the work of the artificial muscle, the non-contact displacement sensor records the length change in the contraction and return stroke, and the work load of the muscle fiber is the weight of the suspended heavy object.
The preparation method of the large-strain quick-response carbon nanotube fiber artificial muscle provided by the invention is simple to operate, creatively adopts water mist to increase strain and accelerate reaction speed, and has the characteristics of economy and environmental protection.
Drawings
FIG. 1 is a carbon nanotube fiber twisting apparatus;
wherein, 1, a motor; 2. carbon nanotube fibers.
FIG. 2 is a schematic diagram of a fiber spray PS/PNIPAM hybrid polymer;
wherein, 3, PS/PNIPAM mixed solution.
FIG. 3 is a schematic diagram of the working principle of electrothermal driving carbon nanotube fiber artificial muscle.
4, a three-way glass tube; 5. artificial muscle made of carbon nanotube fiber; 6. a weight; 7. a non-contact displacement sensor; 8. a direct current power supply.
FIG. 4 is a schematic diagram of the results of the artificial muscle test prepared by the method of the present invention.
The invention aims to overcome the defects of slow response and large heat dissipation of the existing electrothermal driving artificial muscle, and improve the performances of output strain, response speed and the like of fiber muscle so as to overcome the problems in the prior art. The invention adopts a method for preparing fiber artificial muscle by mixing a variable hydrophilic-hydrophobic polymer and carbon nanotube fiber, and applies the method to the field of intelligent robots. The method specifically comprises the steps of preparing a spinnable carbon nanotube fiber, and compounding the carbon nanotube fiber with a variable hydrophilic and hydrophobic polymer by a composite doping method to prepare the quick-response composite carbon nanotube fiber artificial muscle; and then the mechanical and electrical properties of the fiber artificial muscle are researched.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
1. referring to fig. 1, a method for preparing a large-strain rapid-response electrothermal-driven carbon nanotube fiber artificial muscle is characterized in that a carbon nanotube film prepared by carbon nanotube vertical array spinning is twisted and naturally untwisted, high-temperature treatment (heating for 2min at 2000 ℃) is performed on the carbon nanotube film for removing impurities in the fiber and enhancing the tensile property of the fiber, and finally slight acidification treatment is performed to improve the hydrophilic property of the carbon nanotube film. And then uniformly spraying a material with hydrophilic and hydrophobic properties capable of being changed by temperature change into the treated carbon nanotube fibers, controlling the expansion and contraction of the carbon nanotube fibers in an electric heating driving mode, and introducing water mist to the carbon nanotube fibers. The working principle is as follows: when the temperature of the artificial muscle is room temperature, the surface of the muscle has hydrophilic property. After the power is switched on, the muscles contract, and simultaneously absorb water mist to promote the expansion of the muscles, so that the contraction rate is increased; when the temperature exceeds 45 ℃, the muscle surface layer polymer shows hydrophobicity. The water droplet can not stop on the muscle surface, so water smoke can constantly take away the heat of muscle, accelerates its cooling, has shortened recovery time. Thereby achieving the purpose of quick response to large strain.
The material with the hydrophile-lyophile property which can be changed by temperature change is polystyrene/poly N-isopropyl acrylamide (PS/PNIPAM).
The spinnable carbon nanotube array may be prepared by Chemical Vapor Deposition (CVD). First, methane is used as a carbon source, and ferrocene and thiophene vapor are respectively used as a catalyst and a growth promoter. Helium is used as carrier gas to introduce the gaseous raw materials into the reactor. The synthesis of carbon nanotubes is carried out at high temperatures (above 700 ℃). And the reaction is carried out in a hydrogen atmosphere. Thereby obtaining the multi-wall carbon nano-tube array.
The carbon nanotube film can be directly and continuously drawn out from the vertical array of the probe nanotubes.
2. The quick-response electric heating driving artificial muscle can be prepared by the following detailed steps:
the method comprises the following steps: the carbon nanotube film is continuously twisted into a helical fiber. One end of a carbon nano tube film is fixed with the output shaft of the motor, and a weight of 10g is hung at the other end of the carbon nano tube film. The motor twisted the film at 100rpm, and the film formed a helical carbon nanotube fiber. The specific operation steps are shown in the attached figure 1. Step one involves hanging weights to prevent untwisting of the fibers during twisting. The spring index k of the spring-like fiber can be controlled by controlling the total number of turns of the motor, namely D/D.
Wherein k is the spring index, D is the diameter of the artificial muscle, and D is the diameter of the twisted carbon nanotube fiber. The prepared fiber driver with the spiral structure has a spring coefficient larger than 1.5.
Step two: and (3) freely untwisting the twisted fibers and carrying out vacuum high-temperature annealing treatment. Two ends of the freely untwisted fiber are connected with a power supply, the upper end of the freely untwisted fiber is fixed, and a heavy object is hung at the lower end of the freely untwisted fiber. The weight size is 20% of the breaking tensile strength of the carbon nanotube fiber. The voltage was again slowly increased to bring the temperature to 2000 ℃. The vacuum high-temperature annealing time of the fiber is 2 min.
Step three: and (4) performing hydrophilization treatment on the fiber annealed in the second step. Since the original carbon nanotube fiber has hydrophobic characteristics, it is necessary to perform a hydrophilization treatment so that it can absorb water molecules to increase strain. There are generally two types of treatment methods for imparting hydrophilic and hydrophobic properties to a material. Firstly, surface microstructure treatment is carried out, and the Wenzel model shows that: the fine rough structure can increase the hydrophilic and hydrophobic properties of the material; secondly, the material is chemically modified, usually some hydrophilic groups are introduced as follows: hydroxyl, carboxyl, sulfonic acid, phosphoric acid, and the like.
The invention adopts a method of soaking fibers by concentrated sulfuric acid and concentrated nitric acid. The fibers are soaked in concentrated sulfuric acid and concentrated nitric acid for 1 hour. It can be found that the fiber surface soaked by strong acid has a plurality of fold structures, and the quantity of adsorbed water molecules is increased. In addition, hydrophilic groups such as hydroxyl carboxyl and the like are introduced in the process, so that the hydrophilicity of the fiber is improved. Meanwhile, the strong acid treatment of the fiber can destroy the structure of the fiber and reduce the mechanical property of the fiber. Therefore, the soaking time is controlled within a small time.
Step four: a material (PS/PNIPAM mixed solution) with hydrophilic and hydrophobic characteristics capable of changing with temperature is uniformly coated on the carbon nano tube fiber. Dried at room temperature for one hour and the fiber relaxed after drying to a film. The operation method is shown in figure 2.
The hydrophilic and hydrophobic properties of the film prepared from the PS/PNIPAM mixed solution in the fourth step can be changed along with the temperature. When the temperature is room temperature (25 ℃), it appears hydrophilic. When the temperature is raised to 45 ℃, it appears hydrophobic. (Kanidi M, Papagiannopoulos A, Matei A, Dinescu M, Pispas S, Kandyla M.applied Surface science.2020; 527:146841.)
The specific preparation method of the solution is as follows:
PS1448 and PNIPAM265 were measured at 1: 1 was mixed and dissolved in THF to make up a 5 wt% polymer solution.
3. The testing method for electrothermal driving carbon nanotube fiber artificial muscle with large stroke and quick response is explained in detail
The device specifically comprises a direct current power supply, a non-contact displacement sensor, a three-way glass tube and a power supply lead. The two ends of the artificial muscle are connected with the power supply, the extension and contraction of the artificial muscle are realized by controlling the power supply to be switched on and switched off, and water mist is continuously introduced into the glass tube in the process. The top end of the artificial muscle is fixed on the iron support device, and a certain weight is hung at the bottom of the artificial muscle, so that the weight and the sensor are hung in a centering manner. The two ends of the artificial muscle are connected with the power supply, the extension and contraction of the artificial muscle are realized by controlling the switch of the power supply, and water mist is continuously introduced into the glass tube in the driving process. The specific process is as follows: the power switch is closed, and the generated joule heat causes the artificial muscle fiber to expand radially and shorten axially. And at this time, the polymer on the surface of the fiber is hydrophilic, and water molecules in the mist are adsorbed. Water molecules enter the outer layer of the carbon nanotube fiber to cause macroscopic expansion of the fiber, and the contraction stroke is increased. When the power is turned off, heat is dissipated and the fibers stretch. At the moment, the polymer at high temperature is changed into hydrophobic property, water molecules can not stay on the fibers, and water drops flowing down continuously can take away heat, so that the speed of a return stroke is increased. During the work of the artificial muscle, the non-contact displacement sensor records the length change in the contraction and return stroke, and the work load of the muscle fiber is the weight of the suspended heavy object. The test results are shown in fig. 4. The strain of the artificial muscle prepared by the method reaches 9.2 percent under the square wave voltage of 1 Hz and 10V/cm.
Claims (7)
1. A preparation method of electrothermal driving artificial muscle with large strain and quick response is characterized in that a carbon nano tube film prepared by carbon nano tube vertical array spinning is adopted, and the carbon nano tube film is twisted and then naturally untwisted; in order to remove impurities in the fibers and enhance the tensile strength of the fibers, the twisted fibers are subjected to vacuum high-temperature treatment, and then the fibers subjected to the vacuum high-temperature treatment are subjected to slight acidification treatment to improve the hydrophilic performance of the fibers; uniformly spraying a material with hydrophilic and hydrophobic properties capable of being changed by temperature change into the carbon nano tube fiber subjected to slight acidification treatment, controlling the expansion and contraction of the carbon nano tube fiber in an electric heating driving mode, and introducing water mist to the carbon nano tube fiber; when the temperature of the artificial muscle is room temperature, the surface of the muscle is hydrophilic, the muscle contracts after being electrified, and meanwhile, the muscle absorbs water mist to promote the expansion of the muscle and increase the contraction rate; when the temperature exceeds a certain temperature, the polymer on the surface layer of the muscle is hydrophobic, and water drops can not stay on the surface of the muscle, so that the water mist can continuously take away the heat of the muscle, the temperature reduction of the muscle is accelerated, and the recovery time is shortened; thereby achieving the purpose of quick response to large strain.
2. The method for preparing an electrothermal driving artificial muscle with large strain and fast response according to claim 1, wherein the step of twisting the carbon nanotube film to form the helical fiber comprises: one end of a carbon nano tube film is fixed with an output shaft of a motor, a weight of 10g is hung at the other end of the carbon nano tube film, the motor twists the film at the speed of 100rpm, and then the film forms a spiral carbon nano tube fiber.
3. The method for preparing an electrothermal driving artificial muscle with high strain and rapid response according to claim 2, wherein the suspended weight cannot rotate with the motor to prevent untwisting of the fibers during twisting; the spring index k of the spring-like fiber can be controlled to be D/D by hanging weights with different weights and controlling the total number of turns of the motor; wherein k is the spring index, D is the diameter of the helical structure, and D is the diameter of the twisted carbon nanotube fiber.
4. The method for preparing an electrothermal driving artificial muscle with large strain and quick response according to claim 1, wherein the step of performing vacuum high-temperature treatment on the twisted fiber comprises the following steps: connecting two ends of the freely untwisted fiber with a power supply, fixing the upper end of the freely untwisted fiber, and hanging a heavy object at the lower end of the freely untwisted fiber; the weight is 20% of the breaking tensile strength of the carbon nanotube fiber, the voltage is slowly increased to make the temperature reach 2000 ℃, and the fiber vacuum high-temperature annealing time is 2 min.
5. The method for preparing an electrothermal driving artificial muscle with large strain and fast response as claimed in claim 1, wherein the step of slightly acidifying the fiber after vacuum and high temperature treatment to improve its hydrophilic property comprises: soaking the fiber in a mixed solution of concentrated sulfuric acid and concentrated nitric acid for hydrophilization treatment, wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 3: 1, soaking time is 1 h.
6. The method for preparing an electrothermal driving artificial muscle with large strain and rapid response according to claim 1, wherein the material whose hydrophilicity and hydrophobicity can be changed by temperature change is polystyrene/poly-N-isopropylacrylamide (PS/PNIPAM); PS1448 and PNIPAM265 were measured at 1: 1, and dissolving the mixture in tetrahydrofuran to form a polymer solution with the mass percentage concentration of 5 wt%; uniformly coating the polymer solution on the surfaces of carbon nanotube fibers with two fixed and tensioned ends, drying for one hour at room temperature, and loosening the fibers after drying to form a film; the hydrophilic and hydrophobic properties of the film prepared by coating the polymer solution on the carbon nanotube fiber can be changed along with the temperature, when the temperature is 25 ℃, the film is represented as hydrophilic, and when the temperature is increased to 45 ℃, the film is represented as hydrophobic.
7. The method for preparing an electrothermal driving artificial muscle with large strain and quick response according to claim 1, wherein the expansion and contraction of the artificial muscle are controlled in an electrothermal driving mode, and the step of introducing water mist to the artificial muscle comprises the following steps: the top end of the artificial muscle is fixed on the iron support table device and is positioned in the three-way glass tube, a certain weight is hung at the bottom of the artificial muscle, and the weight and the non-contact displacement sensor below the weight are guaranteed to be hung in a centering manner; the two ends of the artificial muscle are connected with a direct current power supply, the extension and contraction of the artificial muscle are realized by controlling the switch of the power supply, and water mist is continuously introduced into the glass tube in the driving process; the specific process is as follows: the power switch is closed, the generated Joule heat enables the artificial muscle fiber to expand radially and shorten axially, and the polymer on the surface of the fiber is hydrophilic at the moment, so that water molecules in mist can be adsorbed, and enter the outer layer of the carbon nano tube fiber to cause the fiber to expand macroscopically, thereby increasing the contraction stroke; when the power supply is disconnected, heat is dissipated, the fiber is elongated, the polymer at high temperature is changed into hydrophobic property, water molecules cannot stay on the fiber, and water drops flowing down continuously take away the heat, so that the speed of a return stroke is increased; during the work of the artificial muscle, the non-contact displacement sensor records the length change in the contraction and return stroke, and the work load of the muscle fiber is the weight of the suspended heavy object.
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