CN113285026A - Full-flexible ultraviolet detector based on high polymer material and preparation and application thereof - Google Patents
Full-flexible ultraviolet detector based on high polymer material and preparation and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to a full-flexible ultraviolet detector based on a high polymer material, and preparation and application thereof, wherein raw materials for preparing the high polymer material comprise a photosensitive material and a piezoelectric polymer; the photosensitive material is an azobenzene liquid crystal elastomer composite material. The invention skillfully takes a liquid crystal elastomer composite system with excellent processing performance, mechanical property and response capability as an optical response component and a flexible substrate, combines the structural design of a piezoelectric stress sensor, constructs a transmission mechanism of an optical signal-stress signal-electric signal, and can prepare a fully flexible ultraviolet detection device with zero power consumption, high durability and high sensitivity. The device can be applied to the fields of wearable sensors, bionic materials, electronic skins, military secret communication and the like.
Description
Technical Field
The invention belongs to the technical field of ultraviolet detectors, and particularly relates to a full-flexible ultraviolet detector based on a high polymer material, and preparation and application thereof.
Background
In the military field, an ultraviolet communication system is a novel communication means and has the unique advantages of low eavesdropping, interference resistance and the like. In order to improve the portability and integration capability of the communication system, the development of a flexible wearable ultraviolet detection device has an urgent need in implementing a mobile communication strategy. At present, most of flexible ultraviolet detectors are limited to photoelectric semiconductors as sensitive elements, but the elastic modulus of rigid semiconductor sensitive elements and the elastic modulus of flexible substrates are not matched, the surface energy difference is large, semiconductor materials are easy to separate and fall off, the flexible ultraviolet detectors are difficult to meet wearable requirements in military extreme environments, and the expansion of material systems and design strategies of the devices has important scientific significance.
Disclosure of Invention
The invention provides an ultraviolet detector based on a high polymer material, wherein raw materials for preparing the high polymer material comprise a photosensitive material and a piezoelectric polymer;
the photosensitive material is an azobenzene liquid crystal elastomer composite material.
The invention discovers that the liquid crystal elastomer has the advantages of high specific strength, fatigue resistance and the like, the synergistic effect of the liquid crystal orientation and the cross-linked network has extremely sensitive response deformation capability to the environment, an optical signal can be converted into a force signal, the liquid crystal elastomer is mixed with conductive particles, an optical-force-electrical signal transmission mechanism can be established, and the durable and high-sensitivity flexible ultraviolet detection high polymer material is prepared.
Preferably, the photosensitive material is poly (ethylene glycol) -block-poly {11- [4- (4-succinimidylphenylazo) phenoxy ] undecyl methacrylate }.
Preferably, the raw materials for preparing the high polymer material also comprise an active amino crosslinking agent with the molecular weight of 100-80000 g/mol.
Further preferably, the molecular weight of the polyethyleneimine is 1000 to 10000 g/mol. The azobenzene liquid crystal elastomer composite material and the piezoelectric polymer mixture have the problems of strong hydrophobicity and weak affinity and adhesion to human skin, the addition of the crosslinking agent with the large molecular weight can improve the hydrophilicity of the film, strengthen the binding force between a liquid crystal elastomer crosslinking network and a piezoelectric polymer molecular chain, further improve the sensing response capability, and the crosslinking agent with the molecular weight in other ranges cannot play corresponding roles.
More preferably, the active amino crosslinking agent is one or more of polyethyleneimine, hexamethylenediamine, diethylenetriamine and triethylenetetramine.
Preferably, the piezoelectric polymer is one or more of polyvinylidene fluoride (PVDF), polyvinylidene fluoride-trifluoroethylene copolymer (PVDF-TrFE), and polyvinylidene fluoride-hexafluoroethylene copolymer (PVDF-HFP). In the invention, the photoinduced deformation of the azobenzene liquid crystal elastomer drives the internal positive and negative charge centers of the piezoelectric material to relatively transfer to generate a polarization phenomenon, thereby realizing the sensing of an ultraviolet light signal-stress signal-electric signal. After the process of mixing the copolymer with the photosensitive material, high-sensitivity ultraviolet sensing can be realized without external voltage, the elastic modulus of each polymer component in the film is matched, the dynamic durability is excellent, and the self-driven flexible ultraviolet sensor with zero power consumption can be prepared. Other piezoelectric ceramic materials such as barium titanate, lead zirconate titanate, and the like may also be used within the scope of the present invention, but are less effective than the above compounds.
Preferably, the photosensitive material is poly (ethylene glycol) -block-poly {11- [4- (4-succinimidylbenzazo) phenoxy ] undecyl methacrylate } and the piezoelectric polymer in a mass ratio of 1: 1-10.
Preferably, the piezoelectric polymer is polyvinylidene fluoride, and the mass ratio of the azobenzene liquid crystal elastomer to the piezoelectric polymer is 1: 2-4.
Preferably, the raw materials for preparing the high molecular material also comprise conductive nanoparticles.
In some preferred embodiments, the conductive particles are preferably one or more of Carbon Nanotubes (CNTs), Ionic Liquids (IL), silver nanowires (AgNWs), Reduced Graphene Oxide (RGO). Wherein the ionic liquid is preferably 1-ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt ([ EMIm)][TFSI]) 1-butyl-3-methylimidazolium tetrafluoroborate ([ BMIm][BF4]) 1-ethyl-3-methylimidazolium hexafluorophosphate ([ EMIm][PF6]) One or more of them. In the invention, the conductive particles can obviously reduce the internal resistance of the liquid crystal elastomer composite material and enhance the output of electric signals.
Preferably, the raw materials for preparing the high molecular material also comprise a thermoplastic elastomer.
In some preferred embodiments, the thermoplastic elastomer is selected from one or more of Thermoplastic Polyurethane (TPU), hydrogenated styrene-butadiene block copolymer (SEBS), Ethylene Propylene Diene Monomer (EPDM). In the invention, the mechanical property of the liquid crystal elastomer composite material can be enhanced by blending the thermoplastic elastomer. Preferably, the mass of the thermoplastic elastomer added is 0% to 50% of the mass of the piezoelectric polymer.
In another aspect of the present invention, a method for preparing a polymer material according to the present invention comprises the following steps:
1) mixing the photosensitive material and the piezoelectric polymer, and preparing the polymer macromolecules obtained by the reaction into a film matrix after the reaction is finished;
2) and compounding the crosslinking agent or the mixture of the crosslinking agent and the conductive nanoparticles on the film substrate.
Preferably, in the step 1), the photosensitive material, the piezoelectric polymer and the thermoplastic elastomer are mixed, and after the reaction is completed, the polymer macromolecules obtained by the reaction are prepared into the film matrix.
Preferably, the film substrate is prepared by a spinning method or a 3D printing method.
Wherein the spinning method is selected from one of wet spinning, dry spinning, electrostatic spinning and microfluid spinning;
in some preferred embodiments, the spinning method is electrostatic spinning, the direct current voltage used in the spinning process is 13-20 KV, the solution propelling speed in the injector is 0.1-2 mL/h, and the distance between the needle head and the receiving device is 10-15 cm. Continuously spinning the mixed solution with the optimal concentration of 0.1-5 mL to obtain a fiber film with the required thickness; the receiving device is a high-speed roller with a layer of aluminum foil attached to the surface, the rotating speed of the roller is 100-5000 rpm, and the fiber film is torn off by using tweezers after spinning is completed. The size of the receiving device can be cut, and the size and the shape of the film can be cut after the fiber film is torn off. The stretched, foldable and breathable fiber film matrix can be better prepared by the spinning method. In the invention, the direct-current voltage process of electrostatic spinning can promote beta-phase crystallization of the piezoelectric polymer, and a subsequent high-voltage polarization step is omitted.
In some preferred embodiments, the method for preparing the ultraviolet light-responsive liquid crystal elastomer composite fiber is specifically as follows: and mixing and dissolving a certain amount of the azobenzene liquid crystal elastomer and the piezoelectric polymer in a solvent, stirring for 3-12 hours at 40-60 ℃ by using a magnetic stirrer, fully mixing and dissolving, preparing the flexible fiber film by using a spinning method, and finishing crosslinking in a dispersion liquid of an active amino crosslinking agent.
The solvent is preferably one or more of N, N-Dimethylformamide (DMF), Tetrahydrofuran (THF), deionized water, ethanol and chloroform.
On the other hand, the invention protects the application of the high polymer material in artificial intelligence, flexible electronics, military secret communication and software robots.
In some preferred embodiments, the invention provides a primary application of the flexible ultraviolet detector prepared by the method in the field of internet of things.
And (4) connecting the liquid crystal elastomer ultraviolet detector into the Arduino single chip microcomputer to prepare the ultraviolet detector monitored by the remote Bluetooth. The method specifically comprises the following steps: the Arduino single chip microcomputer provides stable direct current voltage. Under the irradiation of an ultraviolet light source with unknown intensity, a voltage value or a current value loaded on a device is read by using an analog pin of an Arduino singlechip in a circuit, so that the current ultraviolet light intensity is calculated; connect to Arduino singlechip output pin with bluetooth module, through the bluetooth agreement with current ultraviolet intensity data transmission to the cell-phone on, realize the long-range real-time detection of ultraviolet light, have huge application potential in daily health monitoring, photocuring process monitoring field.
The invention has the following beneficial effects:
the invention utilizes the liquid crystal elastomer composite fiber to generate certain shrinkage stress under the irradiation of ultraviolet light (365nm) with different intensities to drive the piezoelectric effect of the piezoelectric polymer, further amplifies the electric signal through the conductive particles, and can detect the change of the ultraviolet light intensity by detecting the voltage or current change of a device. The result shows that the ultraviolet light detection capability with high sensitivity and high resolution is realized.
The invention skillfully takes a liquid crystal elastomer composite system with excellent processing performance, mechanical property and response capability as an optical response component and a flexible substrate, combines the structural design of a piezoelectric stress sensor, constructs a transmission mechanism of an optical signal-stress signal-electric signal, and prepares the wearable ultraviolet detector with intrinsic flexibility, high durability and high sensitivity. The invention can further realize the regulation and control of the absorption wave band of liquid crystal molecules through the modification of the azobenzene substituent, research the preparation of the intrinsic flexible sensor of the full wave band from deep ultraviolet to visible light, and expand the transfer mechanism to the construction of flexible sensing devices such as heat, humidity and the like. On the basis, the liquid crystal elastomer composite material is designed and shown to be used for preparing intelligent products such as Bluetooth transmission remote detection, ultraviolet safety coding and the like through the singlechip Internet of things technology and mobile phone/computer software control. The liquid crystal elastomer ultraviolet detector provided by the invention has important significance in the application of the fields of wearable sensors, bionic materials, electronic skins, military secret communication and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram illustrating a physical display diagram and a photoresponse mechanism of an azobenzene liquid crystal elastomer composite material in example 1 of the present invention;
FIG. 2 is a stress-strain curve of tensile properties of the composite fiber film in examples 1-2 of the present invention;
FIG. 3 is a Scanning Electron Micrograph (SEM) of the surface and cross section of a composite fiber device in Experimental example 1 of the present invention;
FIG. 4 is a graph of current-intensity curves of different piezoelectric polymers under UV irradiation in Experimental example 1;
FIG. 5 is a graph of current versus time for devices of Experimental example 1 of the present invention under different intensity UV light;
fig. 6 is a schematic physical photograph of a remote bluetooth ultraviolet detection device in experimental example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
In the present invention, the instruments and the like used are conventional products which are purchased from regular vendors, not indicated by manufacturers. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. In the invention, the adopted block copolymer is specifically poly (ethylene glycol) -block-poly {11- [4- (4-succinimidylbenzazo) phenoxy ] undecyl methacrylate } synthesized in a laboratory, and the structural formula is as follows:
example 1
The embodiment provides a preparation method of an azobenzene liquid crystal elastomer composite fiber film, which specifically comprises the following steps:
1) electrostatic spinning of composite fiber: respectively weighing the components in a mass ratio of 1: 3 and polyvinylidene fluoride (PVDF) powder, and poured into a glass bottle. Respectively taking the mixture with a syringe in a volume ratio of 1: 1, and adding the N, N-dimethylformamide and the tetrahydrofuran solvent into a glass bottle for dissolving. The mixed solution was stirred at 60 ℃ for 3 hours using a magnetic stirrer until the solute was completely dissolved. And injecting the uniformly mixed solution into an injector for electrostatic spinning. The direct current voltage used in the spinning process is 15KV, the solution propelling speed in the injector is 1mL/h, the distance between the needle head and the receiving device is 15cm, and 0.5mL of mixed solution is continuously spun to obtain the fiber film with the required thickness. The collecting device is a high-speed roller with a layer of aluminum foil adhered on the surface, the rotating speed is 500 r/min, the fiber film can be torn off by using tweezers after the spinning is finished, and the fiber film is dried overnight at room temperature and normal pressure. The film size can reach A4 paper size, and has certain electrostatic adhesion performance to skin and gloves, as shown in figure 1. Finally, the fiber film is cut into sample pieces of 30mm multiplied by 30mm for standby.
2) Crosslinking the liquid crystal elastomer: 500mg of polyethyleneimine (molecular weight: 10000g/mol) was added to a beaker, and 250mL of absolute ethanol was poured in for dispersion. And (3) placing the beaker into an ultrasonic cleaning machine, oscillating for 1 hour to obtain a uniform polyethyleneimine solution, immersing the fiber film into the polyethyleneimine solution, standing overnight, taking out the sample after the azobenzene liquid crystal block copolymer is fully crosslinked, cleaning for 3 times by using absolute ethyl alcohol, and drying in a vacuum oven for standing overnight. The composite fiber film has good mechanical property, the tensile breaking strength reaches 7.9MPa, the breaking elongation reaches 74%, and the basic performance requirements of wearable equipment are met.
3) Carrying conductive particles: soaking the crosslinked liquid crystal elastomer composite fiber in 1-ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide ([ EMIm ] [ TFSI ]) ionic liquid, fully swelling for 12 hours, sucking excess ionic liquid by using filter paper, and then placing a sample in a fume hood for overnight airing to obtain the conductive liquid crystal elastomer composite fiber film.
Example 2
This example provides a method for preparing an azobenzene liquid crystal elastomer composite fiber film, which is different from example 1 in that the method further includes an operation of loading a thermoplastic elastomer, and includes the following steps: in the step of electrostatic spinning of the composite fiber, an analytical balance is used for respectively weighing the components in a mass ratio of 1: 3 and polyvinylidene fluoride (PVDF) powder, and poured into a glass bottle. Thermoplastic Polyurethane (TPU) was weighed out with an analytical balance to give 0%, 20%, 35% and 50% by mass of PVDF powder and poured into glass bottles. Respectively taking the mixture with a syringe in a volume ratio of 1: 1, and adding the N, N-dimethylformamide and the tetrahydrofuran solvent into a glass bottle for dissolving. The other operations were the same as in example 1. The mechanical property of the composite fiber film is shown in figure 2, the tensile strength is gradually enhanced along with the increase of the addition amount of TPU, the elongation at break can reach 140% to the maximum, and the performance requirements of wearable equipment under various extreme conditions can be met.
Example 3
Compared with the example 1, the difference is only that the molecular weight of the polyethyleneimine crosslinking agent selected in the step 2) liquid crystal elastomer crosslinking process is 70000g/mol, and other operations are the same as the example 1. When the molecular weight of the polyethyleneimine is increased, a cross-linking agent is difficult to enter a molecular network of the composite material, the cross-linking of the liquid crystal elastomer is nonuniform, and the response capability is reduced.
Example 4
Compared with the example 1, the difference is only that the piezoelectric polymer in the step 1) is polyvinylidene fluoride-trifluoroethylene copolymer (PVDF-TrFE), the material has a higher piezoelectric constant, and the other operations are the same as the example 1.
Experimental example 1
In this experimental example, the conductive liquid crystal elastomer composite fiber film is packaged into a flexible ultraviolet detector, and the change of the ultraviolet intensity can be detected by detecting the current change of the detector through an electrometer, which specifically includes the following steps:
the conductive liquid crystal elastomer composite fiber films (30mm × 30mm) in examples 1 to 4 were completely attached to one surface of the conductive silver cloth, and the other surface was placed in a spin coater, and spin-coated with 3mg/mL of an aqueous dispersion of silver nanowires for 2 times. And welding two conductive copper adhesive tapes on two sides of the film through conductive silver paste, wherein the conductive silver paste is used for reducing the contact resistance between the lead and the film, the electrode distance is about 20mm, and after the conductive silver paste is naturally dried for 1 hour, a flexible ultraviolet detection device is obtained. A scanning electron micrograph (SEM image) of the surface and cross section of the composite fiber device is shown in fig. 3. The ultraviolet light intensity detection and analysis system consists of an electrometer (6517B), an ultraviolet light source (365nm), a computer and other equipment. The specific operation is as follows: the device is connected to a circuit, and under the irradiation of different ultraviolet light intensities, the current change in real time is detected by an electrometer (6517B), so that the change of the ultraviolet light intensity is calculated through linear regression analysis.
The current-intensity curve graph of different piezoelectric polymers under ultraviolet irradiation is shown in fig. 4, the piezoelectric polymer PVDF-TrFE has higher piezoelectric constant, and the prepared device has higher response sensitivity; the current-time curve of the device described in example 4 under different intensity uv light intensities is shown in fig. 5. When the mass ratio of the azobenzene liquid crystal elastomer to the piezoelectric polymer is 1: at 3, the resolution of the ultraviolet light intensity detectable by the device is 0.1mW cm-2The response time is about 150ms, the device has good detection performance, and can meet the detection requirements of ultraviolet light intensity in the fields of daily life, industrial photoetching photocuring, military ultraviolet communication and the like.
Experimental example 2
Design and application of remote Bluetooth ultraviolet detection device
The embodiment provides an application idea of a flexible ultraviolet detection device of a liquid crystal elastomer. The device can be connected with Arduino singlechip and prepare the ultraviolet detection device that can real-time long-range bluetooth is connected. The specific implementation steps are as follows:
under the irradiation of an ultraviolet light source with unknown intensity, a voltage value loaded on a device is read by using an analog pin of Arduino in a circuit, the voltage value is converted into a current value of the device through ohm's law, and meanwhile, a linear regression equation of light intensity and the current value is calculated through a current-time curve under the irradiation of ultraviolet light with different intensities, so that the current ultraviolet light intensity is calculated. Connect to Arduino microcontroller output pin with bluetooth module to use App Inventor 2 software programming android mobile phone program App, can realize the long-range real-time detection of ultraviolet light on with current ultraviolet light intensity data transmission to the cell-phone through the bluetooth agreement. Based on the data transmission method, by utilizing the advantages of strong anti-interference capability and strong penetrability of ultraviolet light, the cipher tables corresponding to different ultraviolet intensities can be designed at will for ultraviolet secret communication.
A schematic diagram of a physical photograph of the remote bluetooth ultraviolet detection device according to this embodiment is shown in fig. 6. When there is noWhen the mobile phone is irradiated by ultraviolet light, the intensity of the ultraviolet light displayed by the mobile phone screen is 0mW cm-2", when using a UV light source (60mW cm)-2) When the mobile phone is irradiated, the intensity of ultraviolet light displayed on the mobile phone screen is 59mW cm-2", the detection precision is good.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A full-flexible ultraviolet detector based on high molecular materials is characterized in that raw materials for preparing the high molecular materials comprise photosensitive materials and piezoelectric polymers;
the photosensitive material is an azobenzene liquid crystal elastomer composite material.
2. The fully flexible uv detector of claim 1, wherein the azobenzene liquid crystal elastomer composite is poly (ethylene glycol) -block-poly {11- [4- (4-succinimidylbenzazo) phenoxy ] undecyl methacrylate }.
3. The fully flexible ultraviolet detector according to claim 1 or 2, characterized in that the raw materials for preparing the high polymer material further comprise an active amino crosslinking agent with a molecular weight of 100-80000 g/mol.
4. The fully flexible ultraviolet detector according to claim 3, wherein the active amino crosslinker is one or more selected from polyethyleneimine, hexamethylenediamine, diethylenetriamine and triethylenetetramine;
and/or the piezoelectric polymer is one or more of polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene copolymer and polyvinylidene fluoride-hexafluoroethylene copolymer.
5. The fully flexible ultraviolet detector of claim 2 or claim 4, wherein the mass ratio of the poly (ethylene glycol) -block-poly {11- [4- (4-succinimidylbenzazo) phenoxy ] undecyl methacrylate } to the piezoelectric polymer is 1: 1 to 10.
6. The fully flexible ultraviolet detector according to claim 1, wherein raw materials for preparing the polymer material further include conductive nanoparticles, and preferably, the conductive nanoparticles are one or more of carbon nanotubes, ionic liquid, silver nanoparticles, or reduced graphene oxide.
7. The fully flexible ultraviolet detector according to claim 1, characterized in that the raw material for preparing the polymer material further comprises a thermoplastic elastomer; preferably, the thermoplastic elastomer is one or more of plastic polyurethane, hydrogenated styrene-butadiene block copolymer or ethylene propylene diene monomer.
8. The method for preparing the fully flexible ultraviolet detector as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
1) mixing the photosensitive material and the piezoelectric polymer, and preparing the polymer macromolecules obtained by the reaction into a film matrix after the reaction is finished;
2) and compounding the crosslinking agent or the mixture of the crosslinking agent and the conductive nanoparticles on the film substrate.
9. The method for preparing the fully flexible ultraviolet detector according to claim 8, wherein in the step 1), the photosensitive material, the piezoelectric polymer and the thermoplastic elastomer are mixed, and after the reaction is completed, polymer macromolecules obtained by the reaction are prepared into a film substrate.
10. The use of the fully flexible ultraviolet detector of any one of claims 1 to 7 in artificial intelligence, flexible electronics, military secure communications, and software robots.
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| CN114657705A (en) * | 2022-04-01 | 2022-06-24 | 四川大学 | Piezoelectric polymer fiber membrane with high piezoelectric performance and preparation method thereof |
| CN114932690A (en) * | 2022-05-06 | 2022-08-23 | 哈尔滨工业大学 | Preparation method of cross-medium soft robot based on liquid crystal elastomer |
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