CN112625281B - Janus structural color film for visual sensing and preparation method thereof - Google Patents
Janus structural color film for visual sensing and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Janus structural color film for visual sensing and a preparation method thereof, wherein the method is based on a gas-liquid interface self-assembly strategy to generate a carbon nano tube film which can be transferred to various substrates, and the carbon nano tube film is integrated into a flexible polymer substrate to prepare a stretchable flexible carbon nano tube conductor; and (3) performing polydopamine coating treatment on the flexible polymer side of the flexible carbon nanotube conductor, and further depositing a two-dimensional colloidal crystal array, so as to prepare the Janus structural color film for visual sensing. The Janus structural color film prepared by the invention is in a layered structure, has the dual characteristics of electricity and optics, and can be fixed on human skin to display photoelectric dual sensing response along with limb movement, so that the human movement condition can be sensed truly and reliably, the cost is low, the process is simple and convenient, and the film can be reused.
Description
Technical Field
The invention belongs to the field of biological materials, and particularly relates to a Janus structural color film for visual sensing and a preparation method thereof.
Background
Flexible stretchable conductors are widely used in flexible robots, electronic skins, and wearable devices due to their good flexibility, sensitivity, and high ductility. Flexible sensors can maintain good electronic performance under mechanical deformations such as bending, torsion and stretching. The common flexible electronic material can be prepared by integrating the conductive agent into the flexible supporting material through methods of deposition, phase separation, etching, ink-jet printing, direct mixing and the like, and the obtained flexible electronic material has good conductivity and flexibility. However, the conventional flexible sensor performs the related sensing response only by using a single electrical sensing index, and with the development of the flexible electronic technology, the single electrical sensing index and the sensing instability under extreme environments have been difficult to meet the requirements of practical applications, and the flexible electronic sensor with multiple sensing functions has yet to be developed.
Colloidal crystals are structures with periodic structures and photonic band gap effects that can be used to make photovoltaic devices. In addition, the colloidal crystal can be used for printing, forgery prevention, biomedical sensors, strain sensors, and the like due to its excellent structural color and responsiveness. The two-dimensional colloidal crystal is a two-dimensional compact colloidal crystal array with an ordered period, and has the characteristics of simple structure, convenient preparation, anisotropy and the like. The colloidal crystal particles can self-assemble on a gas-liquid interface to form a two-dimensional colloidal crystal array, and then deposit and transfer the two-dimensional colloidal crystal array onto other substrates so as to endow the substrates with special structural colors.
Therefore, based on the structural color responsiveness of the two-dimensional colloidal crystal array, the invention respectively deposits and integrates the carbon nano tube and the two-dimensional colloidal crystal array on the flexible supporting layer through the polydopamine coating and the multi-stage self-assembly strategy, develops the Janus structural color film for visual sensing based on interface self-assembly, and has important significance for real-time visual monitoring of human body movement.
Disclosure of Invention
Aiming at the defects of the existing flexible electronic materials, the invention provides a Janus structural color film for visual sensing and a preparation method thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of a Janus structural color film for visual sensing comprises the following steps:
(1) Dispersing the carbon nano tube solution on the water surface at a constant speed, forming a film on a gas-liquid interface by means of the Marangoni effect, and compressing the film by utilizing the siphon acting force of the porous sponge to form a carbon nano tube film with a compact structure; transferring the carbon nano tube film to a substrate by a lifting method, and obtaining a multi-layer carbon nano tube film through multiple transfers and tween infiltration; dropwise adding a polymer solution into the multilayer carbon nano tube film and curing to obtain a flexible carbon nano tube conductor;
(2) Performing polydopamine coating treatment on the flexible polymer side of the flexible carbon nanotube conductor prepared in the step (1); dispersing a colloid particle solution on a gas-liquid interface by a tip diversion method, performing self-assembly to generate a two-dimensional colloid crystal array, and depositing and transferring the two-dimensional colloid crystal array to a flexible polymer side to prepare the Janus structural color film for visual sensing.
In the step (1), the polymer solution is selected from one or more of polydimethylsiloxane, polyurethane, polyester, polyvinyl alcohol, polyimide or polyethylene naphthalate solution.
In the step (1), the polymer solution is prepared by using a volatilizable solvent, and the concentration of the polymer solution is 10% -20% m/v.
In the step (1), the tween-infiltrating refers to infiltrating the carbon nanotube film with tween 20 solution with the volume fraction of 0.25%, and then washing the surface of the carbon nanotube film with pure water.
In the step (1), the carbon nanotube layer of the flexible carbon nanotube conductor is coated in a flexible polymer to form a carbon nanotube/flexible polymer composite layer, and the thickness is 2-20 mu m.
In the step (2), the colloidal particle solution is selected from a silica nanoparticle/n-butanol ethanol solution or a polystyrene nanoparticle/acetone ethanol solution.
In the step (2), the Janus structural color film has a thickness of 50-200 mu m and is in a three-layer structure and is divided into a carbon nano tube conductive layer, a flexible polymer supporting layer and a two-dimensional colloid crystal structural color layer.
The invention also provides the Janus structural color film for visual sensing, which is prepared by adopting the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1) The Janus structural color film for visual sensing is prepared based on the polydopamine coating and the multi-stage self-assembly strategy, has photoelectric dual sensing indexes, is low in cost, simple and convenient in process and can be recycled;
2) The Janus structural color film for visual sensing has the advantages of both a flexible carbon nanotube conductor and a two-dimensional colloidal crystal, wherein the two-dimensional colloidal crystal is deposited on the surface of the flexible carbon nanotube conductor by means of a polydopamine coating to provide visual structural color for the flexible carbon nanotube conductor, and the photonic band gap characteristic and the anisotropy of the two-dimensional colloidal crystal enable the structural color to have angle dependence, so that an optical sensing index is provided for the prepared Janus structural color film; the flexible carbon nanotube conductor provides good electrical properties and flexibility for the obtained Janus structural color film;
3) The Janus structural color film for visual sensing prepared by the invention can be used for double sensing of human body movement, wherein the good electrical property of the carbon nano tube can be used as an electrical sensing index to feed back real-time resistance change in human body movement, and the two-dimensional colloidal crystal array can be used as an optical sensing index to perform visual color sensing in human body movement due to anisotropy and structural color responsiveness of the two-dimensional colloidal crystal array.
Drawings
Fig. 1 is a flow chart of a preparation process of a Janus structural color film for visual sensing, (a) is a schematic diagram of a preparation flow of a flexible carbon nanotube conductor, and (b) is a schematic diagram of a flow of a flexible carbon nanotube conductor integrated two-dimensional colloidal crystal array.
FIG. 2 is a physical view of the angle-dependent structural color of example 2, wherein the viewing angles of FIGS. a-d are 90, 60, 30 and 15, respectively.
Fig. 3 is a graph of real-time photoelectric sensing results of example 2 at joints of a human body, wherein graph a is a graph of a relative resistance change curve and a corresponding structural color change image when the bending angle of the joints of the finger is-10 °,45 ° and 90 °, graph b is a graph of a relative resistance change curve and a corresponding structural color change image when the wrist is bent toward the palm side and bent toward the back side, and graph c and graph d are a graph of a relative resistance change curve and a corresponding structural color change image when bending movements are performed on the knee and neck, respectively.
Wherein the reference numerals are as follows: the device comprises a 1-water body, a 2-carbon nano tube film, a 3-flexible carbon nano tube conductor, a 4-polydopamine coating and a 5-two-dimensional colloidal crystal array.
Detailed Description
In order to better understand the technical solutions of the present invention for those skilled in the art, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
The experimental methods used in the examples below, unless otherwise indicated, are conventional methods, and the reagents, methods and apparatus used, unless otherwise indicated, are conventional in the art.
The invention provides a preparation method of a Janus structural color film for visual sensing, which comprises the following steps:
(1) Preparing a flexible carbon nanotube conductor 3: dispersing 1mg/ml of carbon nano tube ethanol solution after ultrasonic dispersion onto a water surface 1 at a constant speed, forming a film on a gas-liquid interface by the carbon nano tube by means of the Marangoni effect, and compressing the film by utilizing the siphon acting force of the porous sponge to form a compact structure; the carbon nanotube film 2 formed on the gas-liquid interface can be transferred onto a substrate by a lifting method, a multi-layer carbon nanotube film can be obtained by means of multiple transfer and tween infiltration, then a polymer solution is dripped, and after the polymer solution is solidified, the polymer solution is carefully peeled off from the substrate, so that the flexible carbon nanotube conductor 3 is obtained.
(2) Preparing a Janus structural color film integrating a two-dimensional colloidal crystal array: placing the flexible carbon nanotube conductor 3 prepared in the step (1) on a hydrophobic substrate in a manner that the carbon nanotube side faces downwards, dropwise adding a dopamine buffer solution to process a polydopamine coating 4, flushing the surface with ultrapure water, placing the surface in a two-dimensional colloidal crystal generating device, dispersing a colloidal particle solution on a gas-liquid interface through a tip flow guiding method, firmly depositing and transferring a two-dimensional colloidal crystal array 5 generated by self-assembly on the surface of the flexible carbon nanotube conductor 3 by means of the polydopamine coating, and drying at room temperature to prepare the Janus structural color film integrating the two-dimensional colloidal crystal array.
In the step (1), the polymer solution is selected from one or more of polydimethylsiloxane, polyurethane, polyester, polyvinyl alcohol, polyimide and polyethylene naphthalate solution, and is prepared by using a volatilizable solvent, and the concentration of the polymer solution is 10% -20% m/v.
In the step (1), the tween-infiltrating refers to that after the carbon nanotube film is infiltrated by using tween 20 solution with the volume fraction of 0.25%, pure water is used for washing the surface of the film.
In the step (1), the carbon nanotube layer of the flexible carbon nanotube conductor 3 is coated in a flexible polymer to form a carbon nanotube/flexible polymer composite layer with a thickness of 2-20 μm.
In the step (2), the colloidal particle solution is selected from a silica nanoparticle/n-butanol ethanol solution or a polystyrene nanoparticle/acetone ethanol solution.
In the step (2), the Janus structural color film has a thickness of 50-200 mu m and is in a three-layer structure and is divided into a carbon nano tube conductive layer, a flexible polymer supporting layer and a two-dimensional colloid crystal structural color layer.
The following are examples:
example 1
A Janus structural color film for visual sensing based on single-layer carbon nano tube/Polydimethylsiloxane (PDMS), the preparation flow is shown in figure 1, and the method comprises the following steps:
preparation of flexible carbon nanotube conductor
The 1mg/ml carbon nanotube ethanol solution dispersed under intense ultrasound was slowly dispersed on the water surface with a syringe, and then the porous sponge was carefully stretched below the water surface along the container rim to compress the carbon nanotube film until the film was no longer small. As shown in fig. 1 (a), a carbon nanotube film was transferred onto a round Polystyrene (PS) substrate having a diameter of 35mm to obtain a single-layered carbon nanotube film, which was dried at room temperature, then 500 μl of 15% (m/v) Polydimethylsiloxane (PDMS) n-hexane mixed solution was added dropwise, and after standing in a fume hood for a period of time to volatilize n-hexane, it was cured at 75 ℃ for 2 hours, and carefully peeled off to obtain a flexible carbon nanotube conductor.
Process for integrating two-dimensional colloidal crystal arrays by flexible carbon nanotube conductors
And (3) placing the flexible carbon nanotube conductor prepared in the last step on a hydrophobic substrate in a manner that the carbon tube side is downward, dripping 2mg/ml dopamine Tris buffer solution into the hydrophobic substrate for soaking for 3 hours to perform polydopamine coating treatment, and placing the flexible carbon nanotube conductor in a two-dimensional colloidal crystal generating device after flushing the surface with ultrapure water. Silica particles with a characteristic peak of 650nm are dissolved in n-butanol solution at a concentration of 20% (m/v), and then 1/2 volume of ethanol solution is added into the silica n-butanol solution, and the mixture is uniformly mixed to prepare a colloidal particle solution with a two-dimensional colloidal crystal structure. As shown in fig. 1 (b), a proper amount of colloidal particle solution is taken by an injector, silica particles are uniformly dispersed on a gas-liquid interface of a two-dimensional colloidal crystal generating device by means of a tip flow guiding method to form a two-dimensional colloidal crystal array through self assembly, a valve of the generating device is opened, water is slowly discharged, the two-dimensional silica colloidal crystal array is deposited and transferred onto the surface of a flexible polymer, and finally, a composite film is taken out and dried under the room temperature condition, so that the Janus structural color film for visual sensing is prepared.
Example 2
A Janus structured color film for visual sensing based on 5 layers of carbon nanotubes/Polydimethylsiloxane (PDMS), comprising the steps of:
preparation of flexible carbon nanotube conductor
1mg/ml (m/v) of the carbon nanotube ethanol solution dispersed under intense ultrasound was slowly dispersed on the water surface with a syringe, and then the porous sponge was carefully stretched along the container rim below the water surface to compress the carbon nanotube film until the film was no longer diminished. As shown in fig. 1 (a), a carbon nanotube film was transferred onto a round Polystyrene (PS) substrate having a diameter of 35mm to obtain a carbon nanotube film, dried at room temperature, then wet and rinsed with a tween 20 solution having a volume ratio of 0.25% and purified water, and the above steps were repeated 4 times to obtain a 5-layer carbon nanotube film, and then 500 μl of a 15% (m/v) Polydimethylsiloxane (PDMS) n-hexane mixed solution was added dropwise, and after standing in a fume hood for a period of time to volatilize n-hexane, cured at 75 ℃ for 2 hours, and carefully peeled off to obtain a flexible carbon nanotube conductor.
Process for integrating two-dimensional colloidal crystals by flexible carbon nanotube conductors
And (3) placing the flexible carbon nanotube conductor prepared in the last step on a hydrophobic substrate in a manner that the carbon tube side is downward, dripping 2mg/ml dopamine Tris buffer solution into the hydrophobic substrate for soaking for 3 hours to perform polydopamine coating treatment, and placing the flexible carbon nanotube conductor in a two-dimensional colloidal crystal generating device after flushing the surface with ultrapure water. Silica particles with a characteristic peak of 650nm are dissolved in n-butanol solution at a concentration of 20% (m/v), and then 1/2 volume of ethanol solution is added into the silica n-butanol solution, and the mixture is uniformly mixed to prepare a colloidal particle solution with a two-dimensional colloidal crystal structure. As shown in fig. 1 (b), a proper amount of colloidal particle solution is taken by an injector, silica particles are uniformly dispersed on a gas-liquid interface of a two-dimensional colloidal crystal generating device by means of a tip flow guiding method to form a two-dimensional colloidal crystal array through self assembly, a valve of the generating device is opened, water is slowly discharged, the two-dimensional silica colloidal crystal array is deposited and transferred onto the surface of a flexible polymer, and finally, a composite film is taken out and dried under the room temperature condition, so that the Janus structural color film for visual sensing is prepared.
Example 3
A Janus structural color film for visual sensing based on 5-layer carbon nanotubes/Polyurethane (PU), comprising the steps of:
preparation of flexible carbon nanotube conductor
1mg/ml (m/v) of the carbon nanotube ethanol solution dispersed under intense ultrasound was slowly dispersed on the water surface with a syringe, and then the porous sponge was carefully stretched below the water surface along the container rim to compress the carbon nanotube film until the film was no longer small. As shown in fig. 1 (a), a carbon nanotube film was transferred onto a round Polystyrene (PS) substrate having a diameter of 35mm to obtain a single-layered carbon nanotube film, which was dried at room temperature, then wetted with a tween 20 solution having a volume ratio of 0.25% and rinsed with pure water, and the above steps were repeated 4 times to obtain a 5-layered carbon nanotube film, and then 500 μl of a 20% (m/v) Polyurethane (PU) N, N-dimethylformamide mixed solution was added dropwise, and after standing in a fume hood for a period of time to volatilize N-hexane, cured at 70 ℃ for 2 hours, and carefully peeled off to obtain a flexible carbon nanotube conductor.
Process for integrating two-dimensional colloidal crystals by flexible carbon nanotube conductors
And (3) placing the flexible carbon nanotube conductor prepared in the last step on a hydrophobic substrate in a manner that the carbon tube side is downward, dripping 2mg/ml dopamine Tris buffer solution into the hydrophobic substrate for soaking for 3 hours to perform polydopamine coating treatment, and placing the flexible carbon nanotube conductor in a two-dimensional colloidal crystal generating device after flushing the surface with ultrapure water. Silica particles with a characteristic peak of 650nm are dissolved in n-butanol solution at a concentration of 20% (m/v), and then 1/2 volume of ethanol solution is added into the silica n-butanol solution, and the mixture is uniformly mixed to prepare a colloidal particle solution with a two-dimensional colloidal crystal structure. As shown in fig. 1 (b), a proper amount of colloidal particle solution is taken by an injector, silica particles are uniformly dispersed on a gas-liquid interface of a two-dimensional colloidal crystal generating device by means of a tip flow guiding method to form a two-dimensional colloidal crystal array through self assembly, a valve of the generating device is opened, water is slowly discharged, the two-dimensional silica colloidal crystal array is deposited and transferred onto the surface of a flexible polymer, and finally, a composite film is taken out and dried under the room temperature condition, so that the Janus structural color film for visual sensing is prepared.
Example 4
The structural color characterization and photoelectric dual sensing index response human body movement characteristics of the Janus structural color film for visual sensing are prepared by the preparation method.
Taking the Janus structural color film for visual sensing based on the 5-layer carbon nano tube/Polydimethylsiloxane (PDMS) prepared in the embodiment 2 as an example, the angle-dependent structural color characterization of the Janus structural color film is determined as follows:
angular dependent structural color characterization: the Janus structural color film for visual sensing of the 5 layers of carbon nano tubes/PDMS is placed on a plane, and the change of structural color under different observation angles is recorded, as shown in figure 2, along with the reduction of the observation angles, the structural color of the Janus structural color film is subjected to blue shift due to the anisotropy of the two-dimensional photonic crystal array, so that an optical sensing index can be provided for the Janus structural color film.
Taking the Janus structural color film for visual sensing based on the 5-layer carbon nano tube/Polydimethylsiloxane (PDMS) prepared in the embodiment 2 as an example, the photoelectric dual sensing index response human body movement characteristics of the Janus structural color film are measured, and the method is specifically as follows:
the Janus structural color film for visual sensing of the 5-layer carbon nano tube/PDMS is fixed on fingers, wrists, knees and necks to monitor the motion state of a human body in real time. As can be seen from fig. 3a, under finger movement, as the bending angle gradually increases, the structural color of the Janus structural color film changes from red to green, and the relative resistance (real-time resistance/original resistance) amplitude becomes large; under the same bending angle, the relative resistance change amplitude is relatively stable, and the photoelectric sensing stability and sensitivity of the film under the condition of finger movement are shown. In addition, a 5-layer carbon nanotube/PDMS Janus structural color film for visual sensing was fixed on the wrist, knee and neck, and the structural color and relative resistance of the Janus structural color film were rapidly and stably changed with bending movement of the joint. These results demonstrate that the Janus structural color film for visual sensing has good photoelectric dual sensing response under mechanical deformation and can be used for visually monitoring the human motion condition.
In conclusion, the Janus structural color film for visual sensing is prepared based on the polydopamine coating and the multi-stage self-assembly strategy, so that the cost is low, the process is simple and convenient, and the Janus structural color film can be recycled; the Janus structural color film for visual sensing prepared by the invention has good conductivity (endowed by the carbon nano tube layer), obvious structural color response (structural color with angle dependence caused by anisotropy of the two-dimensional photonic crystal array), and simultaneously double signals can be used for sensing the mechanical motion condition of a human body, so that the reliability and the accuracy of the sensing result of the flexible wearable device are enhanced while the motion condition is visually sensed.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the invention without departing from the principles thereof are intended to be within the scope of the invention as set forth in the following claims.
Claims (7)
1. The preparation method of the Janus structural color film for visual sensing is characterized by comprising the following steps of:
(1) Dispersing the carbon nano tube solution on the water surface at a constant speed, forming a film on a gas-liquid interface by means of the Marangoni effect, and compressing the film by utilizing the siphon acting force of the porous sponge to form a carbon nano tube film with a compact structure; transferring the carbon nano tube film to a substrate by a lifting method, and obtaining a multi-layer carbon nano tube film through multiple transfers and tween infiltration; dropwise adding a polymer solution into the multilayer carbon nano tube film and curing to obtain a flexible carbon nano tube conductor;
(2) Performing polydopamine coating treatment on the flexible polymer side of the flexible carbon nanotube conductor prepared in the step (1); dispersing a colloid particle solution on a gas-liquid interface by a tip diversion method, performing self-assembly to generate a two-dimensional colloid crystal array, and depositing and transferring the two-dimensional colloid crystal array to a flexible polymer side to prepare a Janus structural color film for visual sensing;
in the step (1), the tween-infiltrating refers to infiltrating the carbon nanotube film with tween 20 solution with the volume fraction of 0.25%, and then washing the surface of the carbon nanotube film with pure water.
2. The method for preparing the Janus structural color film for visual sensing according to claim 1, which is characterized in that: in the step (1), the polymer solution is selected from one or more of polydimethylsiloxane, polyurethane, polyester, polyvinyl alcohol, polyimide or polyethylene naphthalate solution.
3. The method for preparing the Janus structural color film for visual sensing according to claim 2, which is characterized in that: the polymer solution is prepared by means of a volatilizable solvent, and the concentration of the polymer solution is 10% -20% m/v.
4. The method for preparing a Janus structural color film for visual sensing according to claim 3, wherein the method comprises the following steps: in the step (1), the carbon nanotube layer of the flexible carbon nanotube conductor is coated in a flexible polymer to form a carbon nanotube/flexible polymer composite layer, and the thickness is 2-20 mu m.
5. The method for preparing the Janus structural color film for visual sensing according to claim 4, which is characterized in that: in the step (2), the colloidal particle solution is selected from a silica nanoparticle/n-butanol ethanol solution or a polystyrene nanoparticle/acetone ethanol solution.
6. The method for preparing the Janus structural color film for visual sensing according to claim 5, which is characterized in that: in the step (2), the Janus structural color film has a thickness of 50-200 mu m and is in a three-layer structure and is divided into a carbon nano tube conductive layer, a flexible polymer supporting layer and a two-dimensional colloidal crystal structural color layer.
7. The Janus structural color film for visual sensing is characterized by being prepared by the preparation method of any one of claims 1-6.
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