CN114059235B - Photoresponse polyurethane conductive nanofiber membrane and preparation method thereof - Google Patents
Photoresponse polyurethane conductive nanofiber membrane and preparation method thereof Download PDFInfo
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- CN114059235B CN114059235B CN202111430133.9A CN202111430133A CN114059235B CN 114059235 B CN114059235 B CN 114059235B CN 202111430133 A CN202111430133 A CN 202111430133A CN 114059235 B CN114059235 B CN 114059235B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/4358—Polyurethanes
Abstract
The invention discloses a photoresponse polyurethane conductive nanofiber membrane and a preparation method thereof, wherein a photocatalyst, europium nitride nano powder, nano zinc oxide doped aluminum oxide powder and polyurethane are added into a binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran, and are fully and uniformly mixed to prepare spinning solution; and then carrying out electrostatic spinning on the obtained spinning solution, and drying to obtain the spinning solution. The photocatalyst is a pyrylium salt photocatalyst. The invention realizes the movement of electrons along with an external electric field under the irradiation of sunlight or incandescent lamps through better fusion and uniform distribution of the organic photocatalyst and the polyurethane matrix. Europium nitride can improve the efficiency of the photocatalyst, and particularly can implement positive feedback of light under the condition that the film is electrified, thereby improving the illumination characteristic of the film. Meanwhile, in order to improve the sensitivity of the photoresistor, zinc oxide is doped with aluminum oxide (AZO). The obtained photoresistor polyurethane film has high sensitivity.
Description
Technical Field
The invention relates to the field of polyurethane materials, in particular to a photoresponse polyurethane conductive nanofiber membrane and a preparation method thereof.
Background
With the continuous development and integration of high and new technical fields such as electronic technology, biotechnology and textile material technology, intelligent textiles are receiving more and more extensive attention. The intelligent textiles are textiles which retain the original characteristics of the textiles, meet basic requirements of wearing and warm keeping of traditional clothes, can sense the stimulation of the environment and make appropriate response, have the functions of sensing, feedback, response, self-diagnosis, self-repair and the like, and have different additional values.
Good pliability is one of the biggest characteristics of intelligent fabrics, and based on this, the human form of intelligent fabrics ability large tracts of land laminating does not influence normal health activity, dresses for a long time, all is difficult for changing the product function under warping by a wide margin, and intelligent clothing fashion, comfortable, flexible wearable technique has also consequently realized more kinds, more stable function.
The flexible matrix photoelectric functional material has good ductility and flexibility, is cuttable, has low cost, is beneficial to large-scale industrial production, is an expansion and extension of the traditional photoelectric device, further brings revolutionary change to the development of the photoelectric device, and has great application value in the fields of new generation display technology, photovoltaics, sensors, photocatalysis, electromagnetic shielding and the like. More and more scientific researchers and resources are put into the research of the flexible device, and the research results are not better.
Although current flexible matrix photoresistors perform well in terms of ductility and flexibility, further improvements in optoelectronic properties are still needed.
Disclosure of Invention
The invention aims to: the invention aims to solve the technical problem of the prior art and provides a photoresponse polyurethane conductive nanofiber membrane and a preparation method thereof so as to obtain the polyurethane conductive nanofiber membrane with excellent photoresistance characteristics.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a photoresponse polyurethane conductive nanofiber membrane comprises the following steps:
(1) Adding a photocatalyst, europium nitride nano powder, nano zinc oxide doped aluminum oxide powder and polyurethane into a binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran, and fully and uniformly mixing to prepare a spinning solution;
(2) And (2) carrying out electrostatic spinning on the spinning solution obtained in the step (1), and drying to obtain the spinning solution.
Specifically, in the step (1), the photocatalyst is a pyrylium salt photocatalyst.
Preferably, the pyrylium salt photocatalyst is selected from any one of 2,4, 6-triphenylpyrylium tetrafluoroborate, 2,4, 6-tri (4-fluorophenyl) pyrylium tetrafluoroborate, 2,4, 6-tri-p-tolylpyrylium tetrafluoroborate and 2,4, 6-tri (4-methoxyphenyl) pyrylium tetrafluoroborate; more preferably 2,4, 6-tris (4-methoxyphenyl) pyrylium tetrafluoroborate.
Preferably, in the step (1), the particle size of the europium nitride nanopowder is 20-50 nm, and more preferably 30nm.
Preferably, in the step (1), the nano zinc oxide doped aluminum oxide powder is a conductive glass material, and the particle size is 20-50 nm, more preferably 40nm; the doping ratio of zinc oxide to aluminum oxide is 99.
Preferably, in step (1), the polyurethane TPU is injection molded grade, transparent grade pellets.
Preferably, in the binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran in step (1), the mixing volume ratio of N, N-dimethylformamide to tetrahydrofuran is from 80 to 50, and more preferably from 70.
Preferably, in the step (1), the mass-to-volume ratio of the photocatalyst, the europium nitride nano powder, the nano zinc oxide doped aluminum oxide powder, the polyurethane, and the binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran is as follows: the photocatalyst comprises europium nitride nano powder, nano zinc oxide doped aluminum oxide powder, polyurethane, a binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran, wherein the binary mixed solvent comprises (0.3-0.5 g), (0.5-1.1 g), (3.1-5.0 g), (15-22 g) 100ml, more preferably 0.4g.
Specifically, in the step (2), the electrostatic spinning condition is 20G flat-head needle, the loading voltage is 15-20 kV, preferably 18kV, the flow rate is 0.5-0.8 ml/h, preferably 0.7ml/h, and the receiving distance is 13-15 cm, preferably 14cm; drying for 6-8 h at 30-40 ℃ after electrostatic spinning is finished.
Further, the invention also claims the photoresponse polyurethane conductive nanofiber membrane prepared by the preparation method.
The photocatalyst is used for responding materials to light, and electron transition and free electron generation are realized under illumination; the europium nitride nano powder is a fluorescent material, can assist the photocatalyst to improve the electron transition efficiency and is used for improving the sensitivity of photoresponse; the nanometer zinc oxide doped aluminum oxide powder reinforced fiber endows the fiber base with the conductive capability and the polyurethane conductive fiber base body.
Has the beneficial effects that:
1. the invention realizes the movement of electrons along with an external electric field under the irradiation of sunlight or an incandescent lamp through better fusion and uniform distribution of the organic photocatalyst and the polyurethane matrix. Europium nitride can improve the efficiency of the photocatalyst, and particularly can implement positive feedback of light under the condition that the film is electrified, thereby improving the sensitivity of the film. Meanwhile, in order to further improve the sensitivity of the photoresistor, zinc oxide doped aluminum oxide (AZO) is doped.
2. The nano zinc oxide doped aluminum oxide powder, the organic photocatalyst and the europium nitride can form a new composite structure ceramic, so that the chemical damage and thermal degradation resistance of the polyurethane nanofiber membrane is improved, and the service life is prolonged.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
FIG. 1 is a scanning electron microscope image of the photoresponsive polyurethane conductive nanofiber film of example 1.
Detailed Description
The invention will be better understood from the following examples.
Example 1
The method comprises the following steps: uniformly mixing 300ml of N, N-dimethylformamide and 200ml of tetrahydrofuran to prepare a binary mixed solvent;
step two: adding 0.4g of photocatalyst 2,4, 6-tri-p-tolyl pyrylium tetrafluoroborate, 0.8g of europium nitride nano powder with the particle size of 30nm, 4.0g of nano zinc oxide doped aluminum oxide powder with the particle size of 40nm (the doping ratio of zinc oxide to aluminum oxide is 99;
step three: and (3) performing electrostatic spinning on the spinning solution prepared in the step two by using a 20G flat-head needle under the conditions that the loading voltage is 18kV, the flow rate is 0.7ml/h and the receiving distance is 14cm, and then putting the spinning solution into a drying oven at the temperature of 35 ℃ for drying for 7h to obtain the photoresponse polyurethane conductive nanofiber membrane, wherein the figure 1 is a scanning electron microscope image of the example 1.
Example 2
The method comprises the following steps: 400mlN, N-dimethylformamide and 100ml tetrahydrofuran are mixed evenly to prepare a binary mixed solvent;
step two: adding 0.3g of photocatalyst 2,4, 6-tris (4-fluorophenyl) pyrylium tetrafluoroborate, 1.1g of europium nitride nano powder with the particle size of 50nm, 3.1g of nano zinc oxide doped aluminum oxide powder with the particle size of 20nm (the doping ratio of zinc oxide to aluminum oxide is 99);
step three: and (3) performing electrostatic spinning on the spinning solution prepared in the second step by using a 20G flat-head needle under the conditions that the loading voltage is 15kV, the flow rate is 0.5ml/h and the receiving distance is 15cm, and then drying the spinning solution in an oven at the temperature of 30 ℃ for 8 hours to obtain the photoresponse polyurethane conductive nanofiber membrane.
Example 3
The method comprises the following steps: 250mlN, N-dimethylformamide and 250ml of tetrahydrofuran are mixed evenly to prepare a binary mixed solvent;
step two: adding 0.5g of photocatalyst 2,4, 6-triphenylpyrylium tetrafluoroborate, 0.5g of europium nitride nano powder with the particle size of 20nm, 5.0g of nano zinc oxide doped aluminum oxide powder with the particle size of 50nm (the doping ratio of zinc oxide to aluminum oxide is 98;
step three: and (3) performing electrostatic spinning on the spinning solution prepared in the step two by using a 20G flat-head needle under the conditions that the loading voltage is 20kV, the flow rate is 0.8ml/h and the receiving distance is 13cm, and then putting the spinning solution into a drying oven at the temperature of 40 ℃ for drying for 6h to obtain the photoresponse polyurethane conductive nanofiber membrane.
Comparative example 1 (Matt catalyst)
The method comprises the following steps: uniformly mixing 300ml of N, N-dimethylformamide and 200ml of tetrahydrofuran to prepare a binary mixed solvent;
step two: adding 0.8g of europium nitride nano powder with the particle size of 40nm, 4.0g of nano zinc oxide doped aluminum oxide powder with the particle size of 40nm (the doping ratio of zinc oxide to aluminum oxide is 99;
step three: and (3) performing electrostatic spinning on the spinning solution prepared in the step two by using a 20G flat-head needle under the conditions that the loading voltage is 18kV, the flow rate is 0.7ml/h and the receiving distance is 14cm, and then drying the spinning solution in a drying oven at the temperature of 35 ℃ for 7h to obtain the polyurethane film A.
Comparative example 2 (europium nitride free)
The method comprises the following steps: evenly mixing 300mlN, N-dimethylformamide and 200ml tetrahydrofuran to prepare a binary mixed solvent;
step two: adding 0.4 photocatalyst 2,4, 6-tri-p-tolyl pyrylium tetrafluoroborate, 4.0g of nano zinc oxide doped aluminum oxide powder with the particle size of 40nm (the doping ratio of zinc oxide to aluminum oxide is 99: 1) and 18g of injection-grade transparent granular polyurethane TPU into 100ml of the binary mixed solvent prepared in the first step, and fully and uniformly mixing to prepare a spinning solution;
step three: and (3) performing electrostatic spinning on the spinning solution prepared in the step two by using a 20G flat-head needle under the conditions that the loading voltage is 18kV, the flow rate is 0.7ml/h and the receiving distance is 14cm, and then putting the spinning solution into a drying oven at the temperature of 35 ℃ for drying for 7h to obtain the polyurethane film B.
Comparative example 3 (cast film)
The method comprises the following steps: evenly mixing 300mlN, N-dimethylformamide and 200ml tetrahydrofuran to prepare a binary mixed solvent;
step two: adding 0.4 photocatalyst 2,4, 6-tri-p-tolylpyrylium tetrafluoroborate, 0.8g of europium nitride nano powder with the particle size of 40nm, 4.0g of nano zinc oxide doped aluminum oxide powder with the particle size of 40nm (the doping ratio of zinc oxide to aluminum oxide is 99;
step three: and (3) after the mixed solution prepared in the step two is completely defoamed, pouring the mixed solution into a clean glass plate, horizontally pushing the mixed solution into a film by using a glass rod, and drying the film in a drying oven at the temperature of 35 ℃ for 7 hours to obtain the polyurethane film C.
Determination of the resistivity
The resistivity of the polyurethane conductive nanofiber membrane is measured by using an RTS-8 type digital linear four-probe tester. In the test, the polyurethane film samples of examples 1-3 and comparative examples 1-3 were placed in a probe test stand, four probes were contacted with the surface of the film under a certain pressure, and after a certain amount of current was applied between the probes, the resistivity of the film was automatically given by the instrument, and the results are shown in table 1.
TABLE 1 resistivity and sensitivity of the films
As can be seen from the resistivity comparison of the examples 1-3 and the comparative examples 1-3 under the dark environment and the illumination condition, the polyurethane conductive nanofiber film prepared by doping the organic photocatalyst, the europium nitride nanoparticles and the zinc oxide doped aluminum oxide nanoparticles has basic conductivity under the dark environment, the resistivity is reduced by 30-50 times after illumination, and the conductivity is greatly enhanced. In contrast, comparative example 1 does not incorporate an organic photocatalyst, and thus the conductive properties of the thin film have no photoresponsive ability; the comparative example 2 does not contain the nano europium nitride powder, and the positive feedback amplification cannot be generated on the photoelectron transfer caused by the organic photocatalyst, so the resistivity is only reduced by about 40% after the irradiation of light, and the photoresponse performance is inferior to that of the material of the example. In comparative example 3, the tape casting is adopted to form a film, the electron migration in the film is isotropic and can interfere with each other, and the nano fibers in the embodiment have gaps, so that the radial electromagnetic interference of the fibers is prevented, the polarization of the fiber bundles can be realized under the electric field force, and the conductive effect is mentioned.
The nanometer zinc oxide doped aluminum oxide powder can improve the chemical damage and thermal degradation resistance of the polyurethane nanometer fiber film and prolong the service life
Chemical injury treatment: the polyurethane film samples of examples 1 to 3 and comparative examples 1 to 3 were sequentially placed in a 5% mass fraction hydrochloric acid solution, a 5% mass fraction sodium hydroxide solution and ethyl acetate for soaking for 24 hours, taken out, vacuum-dried at normal temperature for 48 hours, and the resistivity was measured using an RTS-8 digital linear four-probe tester.
Thermal degradation damage treatment: the polyurethane film samples of examples 1 to 3 and comparative examples 1 to 3 were placed in an oven at 160 ℃ for 12 hours, and after taking out, they were naturally cooled to room temperature, and the resistivity and sensitivity were measured by using an RTS-8 digital linear four-probe tester, and the results are shown in tables 2 and 3.
TABLE 2 resistivity and sensitivity of the films after chemical Damage treatment
TABLE 3 resistivity and sensitivity of films after thermal degradation damage treatment
Tables 2 and 3 show that the film materials of examples 1 to 3 and comparative examples 1 to 3 have increased dark resistance by the chemical damage treatment and the thermal degradation damage treatment, indicating that the film structure is damaged, resulting in a decrease in the conductive properties. However, the sensitivity of the photoresistor of examples 1 to 3 was still maintained at a higher level, above 18, than that of comparative examples 1 to 3; the sensitivity of the comparative examples was 2 or less. The conductive nanofiber films of examples 1-3 are shown to have some resistance to chemical damage and thermal degradation. The reason is that in the preparation process of the film materials in the embodiments 1-3, the organic photocatalyst, europium nitride and zinc oxide doped aluminum oxide nanoparticles form a stable composite ceramic structure under the action of an electrostatic field.
The present invention provides a photoresponsive polyurethane conductive nanofiber membrane and a method and a way for preparing the same, and a plurality of methods and ways for implementing the technical scheme are provided, the above description is only a preferred embodiment of the present invention, it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the present invention, and these improvements and decorations should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (7)
1. A preparation method of a photoresponse polyurethane conductive nanofiber membrane is characterized by comprising the following steps:
(1) Adding a photocatalyst, europium nitride nano powder, nano zinc oxide doped aluminum oxide powder and polyurethane into a binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran, and fully and uniformly mixing to prepare a spinning solution;
(2) Performing electrostatic spinning on the spinning solution obtained in the step (1), and drying to obtain the spinning solution;
in the step (1), the photocatalyst is a pyrylium salt photocatalyst; the pyrylium salt photocatalyst is selected from any one of 2,4, 6-triphenyl pyrylium tetrafluoroborate, 2,4, 6-tri (4-fluorophenyl) pyrylium tetrafluoroborate, 2,4, 6-tri-p-tolyl pyrylium tetrafluoroborate and 2,4, 6-tri (4-methoxyphenyl) pyrylium tetrafluoroborate;
in the step (1), the mass-to-volume ratio of the photocatalyst, the europium nitride nano powder, the nano zinc oxide doped aluminum oxide powder, the polyurethane, the N, N-dimethylformamide and the tetrahydrofuran binary mixed solvent is as follows: the photocatalyst is europium nitride nanopowder, nano zinc oxide doped aluminum oxide powder, polyurethane, and a binary mixed solvent of N, N-dimethylformamide and tetrahydrofuran, wherein the binary mixed solvent comprises (0.3-0.5 g) = (0.5-1.1g): (3.1-5.0 g): (15-22g): 100ml.
2. The method for preparing the photoresponse polyurethane conductive nanofiber membrane as claimed in claim 1, wherein in the step (1), the particle diameter of the europium nitride nanopowder is 20 to 50nm.
3. The preparation method of the photoresponse polyurethane conductive nanofiber membrane as claimed in claim 1, wherein in the step (1), the particle diameter of the nano zinc oxide doped aluminum oxide powder is 20 to 50nm, and the doping ratio of zinc oxide to aluminum oxide is (99).
4. The method for preparing the photo-responsive polyurethane conductive nanofiber membrane as claimed in claim 1, wherein in step (1), the polyurethane is injection-molded grade, transparent grade particles.
5. The method for preparing the photoresponse polyurethane conductive nanofiber membrane as claimed in claim 1, wherein in the step (1), the mixing volume ratio of the N, N-dimethylformamide to the tetrahydrofuran in the binary mixed solvent of the N, N-dimethylformamide and the tetrahydrofuran is 80 to 50.
6. The preparation method of the photoresponse polyurethane conductive nanofiber membrane as claimed in claim 1, wherein in the step (2), the electrostatic spinning condition is a 20G flat-head needle, the loading voltage is 15-20kV, the flow rate is 0.5-0.8ml/h, and the receiving distance is 13-15cm; and drying the obtained product at 30 to 40 ℃ for 6 to 8 hours after electrostatic spinning is finished.
7. The photoresponse polyurethane conductive nanofiber membrane prepared by the preparation method of any one of claims 1-6.
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