CN115125728A - Preparation method of polyurethane film loaded with redox graphene and carbon nano tubes - Google Patents
Preparation method of polyurethane film loaded with redox graphene and carbon nano tubes Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
Adding polyurethane PU into N, N-dimethylformamide, uniformly mixing to obtain a solution A, carrying out centrifugal spinning on the solution A to obtain polyurethane nanofibers, collecting the nanofibers, pressing the nanofibers into nanofiber films, repeatedly immersing the nanofiber films into graphene oxide dispersion liquid for N times, taking out, drying and immersing to obtain the graphene oxide-loaded polyurethane films, reducing the graphene oxide-loaded polyurethane films by using a reducing agent to obtain the graphene oxide-loaded polyurethane films, repeatedly immersing the graphene oxide-loaded polyurethane films into carbon nanotube CNTs dispersion liquid for m times, taking out, cleaning and drying to obtain the graphene oxide-and carbon nanotube-loaded polyurethane films. The film prepared by the method has high conductivity and tensile stability, is suitable for a flexible stress sensor, and has high working sensitivity and good stability.
Description
Technical Field
The invention belongs to the technical field of lithium battery materials, and particularly relates to a preparation method of a polyurethane film carrying redox graphene and carbon nanotubes.
Background
With the development of electronic devices towards more integration, portability and intellectualization, the nanofiber film with high conductivity and stretchability is widely noticed as a key material of a flexible stress sensor in the application of flexible wearable electronic devices. The polyurethane PU has the advantages of thermoplasticity, high elasticity, wear resistance and the like, can be used as a flexible matrix material in a sensor, and the carbon nano tube CNTs have excellent conductivity and mechanical property and can be used for enhancing the conductivity of the flexible matrix material.
Chinese patent: application publication No. CN 107674385A discloses a preparation method of a toughening resistance-reducing carbon fiber composite material, which comprises the steps of firstly preparing graphene-carbon nano tube composite filler suspension, uniformly mixing the composite filler suspension with thermoplastic polyurethane or nylon solution to obtain spinning solution, then spinning into nano-scale fiber yarns by adopting an electrostatic spinning method, coating the nano-scale fiber yarns on the surface of a carbon fiber fabric to form a thin fiber film, and finally preparing a carbon fiber composite material laminated board by adopting a vacuum auxiliary forming technology. Therefore, there is a need for a conductive film with high conductivity and high tensile stability suitable for use in flexible stress sensors.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a preparation method of a polyurethane film with negative redox graphene and carbon nanotubes, which has high conductivity and high tensile stability and is suitable for a flexible stress sensor.
In order to achieve the above purpose, the invention provides the following technical scheme:
the preparation method of the polyurethane film carrying the redox graphene and the carbon nano tubes comprises the following steps:
s1, adding Polyurethane (PU) into N, N-dimethylformamide, uniformly mixing to obtain a solution A, carrying out centrifugal spinning on the solution A to obtain polyurethane nanofibers, and finally collecting the polyurethane nanofibers and pressing the polyurethane nanofibers into polyurethane nanofiber films;
s2, firstly, immersing the polyurethane nanofiber film obtained in the step S1 into graphene oxide dispersion liquid, then taking out the polyurethane nanofiber film and drying the polyurethane nanofiber film, and circularly repeating the step S2 for n times to obtain a polyurethane film loaded with graphene oxide;
s3, reducing the polyurethane conductive diaphragm loaded with the graphene oxide by adopting a reducing agent to obtain a polyurethane film loaded with the redox graphene;
s4, immersing the polyurethane film loaded with the redox graphene into the carbon nano tube CNTs dispersion liquid, then taking out, sequentially cleaning and drying, and circularly repeating the step S4 for m times to obtain the polyurethane film loaded with the redox graphene and the carbon nano tube.
In step S1, the mass percentage concentration of the solution A is 17-19%.
In step S1, the rotation speed of the centrifugal spinning is 4400-4600r/min, the collection distance is 28-32cm, and the mixing is specifically stirring for 7.5-8.5h at 78-82 ℃.
In step S1, the collecting of the polyurethane nanofibers is to overlap the polyurethane nanofibers 6-7 times along their orientation, and the pressing of the polyurethane nanofibers is to press the polyurethane nanofibers with a weight of 2-2.5kg, and then dry the polyurethane nanofibers at 58-62 ℃ for 2-2.5 h.
In step S2, n is at least 5 times, and the soaking time is 25-35min each time.
In step S2, the mass-volume concentration of the graphene oxide dispersion liquid is 0.45 to 0.55 mg/mL.
In step S3, the reducing agent is hydrazine hydrate.
In step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 3-12%.
In step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 6% to 9%.
In the step S4, m is 3 times, the first immersion time is 8-10h, ultrasonic dispersion is carried out for 1-1.5h after the second immersion, then the materials are taken out and cleaned and dried in sequence, and the third immersion time is 12-14 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention relates to a preparation method of a polyurethane film loaded with redox graphene and carbon nano tubes, which comprises the steps of adding polyurethane PU into N, N-dimethylformamide, uniformly mixing to obtain a solution A, carrying out centrifugal spinning on the solution A to obtain polyurethane nano fibers, collecting the polyurethane nano fibers, pressing the polyurethane nano fibers into a polyurethane nano fiber film, circularly repeating the steps for N times to immerse the polyurethane nano fiber film into a graphene oxide dispersion liquid, taking out and drying the graphene oxide dispersion liquid to obtain a polyurethane film loaded with the graphene oxide, reducing a polyurethane conductive diaphragm loaded with the graphene oxide by using a reducing agent to obtain a polyurethane film loaded with the redox graphene, circularly repeating the steps for m times to immerse the polyurethane film loaded with the redox graphene into a carbon nano tube CNTs dispersion liquid, taking out, cleaning and drying the polyurethane film loaded with the redox graphene and the carbon nano tubes to obtain the polyurethane film loaded with the redox graphene and the carbon nano tubes, according to the method, graphene is modified, graphene oxide has a polar oxygen-containing functional group, the graphene oxide has good hydrophilicity, can be uniformly dispersed in a solution, the conductivity of the polyurethane film is greatly improved, the polyurethane film prepared according to a special proportion has high tensile stability, and is suitable for a flexible stress sensor, good in working stability and high in sensitivity. Therefore, the invention has high conductivity and high tensile stability, and is suitable for flexible stress sensors.
Drawings
FIG. 1 is a graph showing the change rate of resistance with respect to the elongation in test examples 1 to 4 and comparative example of the present invention.
FIG. 2 is a graph showing the rate of change of resistance of comparative examples in the course of different cycles of stretching in the present invention.
FIG. 3 is a graph showing the rate of change of resistance during different cycles of stretching in test example 1 of the present invention.
FIG. 4 is a graph showing the rate of change of resistance during different cycles of stretching in test example 2 of the present invention.
FIG. 5 shows the rate of change of resistance during different cycles of stretching in test example 3 of the present invention.
FIG. 6 is a graph showing the rate of change of resistance during different cycles of stretching in test example 4 of the present invention.
FIG. 7 shows the resistance value change at the joints of human fingers in test example 3 of the present invention.
FIG. 8 is a graph showing the resistance value changes at the joints of the wrist in test example 3 of the present invention.
FIG. 9 shows the change of resistance at the laryngeal prominence of human body in test example 3 of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
The preparation method of the polyurethane film carrying the redox graphene and the carbon nano tubes comprises the following steps:
s1, adding Polyurethane (PU) into N, N-dimethylformamide, uniformly mixing to obtain a solution A, carrying out centrifugal spinning on the solution A to obtain polyurethane nanofibers, and finally collecting the polyurethane nanofibers and pressing the polyurethane nanofibers into polyurethane nanofiber films;
s2, firstly, immersing the polyurethane nanofiber film obtained in the step S1 into graphene oxide dispersion liquid, then taking out the polyurethane nanofiber film and drying the polyurethane nanofiber film, and circularly repeating the step S2 for n times to obtain a polyurethane film loaded with graphene oxide;
s3, reducing the polyurethane conductive diaphragm loaded with the graphene oxide by adopting a reducing agent to obtain a polyurethane film loaded with the redox graphene;
s4, immersing the polyurethane film loaded with the redox graphene into the carbon nano tube CNTs dispersion liquid, then taking out, sequentially cleaning and drying, and circularly repeating the step S4 for m times to obtain the polyurethane film loaded with the redox graphene and the carbon nano tube.
In step S1, the mass percentage concentration of the solution A is 17-19%.
In step S1, the rotation speed of the centrifugal spinning is 4400-4600r/min, the collection distance is 28-32cm, and the mixing is specifically stirring for 7.5-8.5h at 78-82 ℃.
In step S1, the collecting of the polyurethane nanofibers is to overlap the polyurethane nanofibers 6-7 times along their orientation, the pressing of the polyurethane nanofibers is to press the polyurethane nanofibers with a weight, and then dry the polyurethane nanofibers at 58-62 ℃ for 2-2.5h, and the weight has a mass of 2-2.5 kg.
In step S2, n is at least 5 times, and the soaking time is 25-35min each time.
In step S2, the mass-volume concentration of the graphene oxide dispersion liquid is 0.45 to 0.55 mg/mL.
In step S3, the reducing agent is hydrazine hydrate.
In step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 3% to 12%.
In step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 6% to 9%.
In the step S4, m is 3 times, the first immersion time is 8-10h, ultrasonic dispersion is carried out for 1-1.5h after the second immersion, then the materials are taken out and cleaned and dried in sequence, and the third immersion time is 12-14 h.
Example 1:
a preparation method of a polyurethane film carrying redox graphene and carbon nanotubes comprises the following steps:
s1, adding polyurethane PU into N, N-dimethylformamide according to a required proportion, and stirring in a magnetic stirrer at 82 ℃ for 8.5 hours to obtain a solution A, wherein the mass percentage concentration of the solution A is 19%;
s2, injecting the solution A obtained in the step S1 into a centrifugal spinning machine, adjusting the rotating speed of the centrifugal spinning machine to 4600r/min, and collecting the solution A with the collecting distance of 32cm to obtain polyurethane nano fibers;
s3, overlapping the polyurethane nanofiber obtained in the step S2 for 6 times along the fiber orientation, pressing the polyurethane nanofiber with a 2kg weight, and drying the polyurethane nanofiber in a 62 ℃ forced air drying oven for 2.5 hours to obtain a polyurethane nanofiber film;
s4, firstly, immersing the polyurethane nanofiber film obtained in the step S3 into graphene oxide dispersion liquid for 30min, then taking out the polyurethane nanofiber film, drying the polyurethane nanofiber film, and circularly repeating the step S4 for 5 times to obtain a graphene oxide-loaded polyurethane film, wherein the mass volume concentration of the graphene oxide dispersion liquid is 0.55 mg/mL;
s5, carrying out gas-phase polymerization on the polyurethane conductive membrane loaded with the graphene oxide through a hydrazine hydrate solution for 12h to obtain a polyurethane film loaded with redox graphene;
s6, immersing the polyurethane film loaded with the redox graphene into the carbon nano tube CNTs dispersion liquid, then taking out the polyurethane film to be sequentially cleaned and dried, and circularly repeating the step S6 for 3 times to obtain the polyurethane film loaded with the redox graphene and the carbon nano tube, wherein the mass percentage concentration of the carbon nano tube CNTs dispersion liquid is 6%, the immersion time for the first time is 10h, after the second immersion, the ultrasonic dispersion is carried out for 1h, then the polyurethane film is taken out to be sequentially cleaned and dried, and the immersion time for the third time is 12 h.
Example 2:
the difference from example 1 is that:
in the step S1, the mass percentage concentration of the solution A is 17%, the stirring temperature is 78 ℃, and the time is 7.5 hours;
in step S2, the rotating speed of the centrifugal spinning machine is 4400r/min, and the collecting distance is 28 cm;
in step S3, overlapping for 7 times along the fiber orientation of the polyurethane nanofiber, pressing with a 2.5kg weight, and drying at 58 ℃ for 2h to obtain a polyurethane nanofiber film;
in step S4, the mass-volume concentration of the graphene oxide dispersion liquid is 0.45 mg/mL;
in step S6, the mass percentage concentration of the carbon nanotube CNTs dispersion is 3%, the first immersion time is 8 hours, the second immersion is followed by ultrasonic dispersion for 1.5 hours, and then the carbon nanotube CNTs dispersion is taken out and sequentially washed and dried, and the third immersion time is 14 hours.
Example 3:
the difference from example 1 is that:
in the step S1, the mass percentage concentration of the solution A is 18%, the stirring temperature is 80 ℃, and the time is 8 hours;
in step S2, the rotating speed of the centrifugal spinning machine is 4500r/min, and the collecting distance is 30 cm;
in step S3, drying at 60 ℃ for 2h to obtain a polyurethane nanofiber film;
in step S4, the mass-volume concentration of the graphene oxide dispersion liquid is 0.5 mg/mL;
in step S6, the mass percentage concentration of the carbon nanotube CNTs dispersion is 9%.
Example 4:
the difference from example 3 is that:
in step S6, the mass percentage concentration of the carbon nanotube CNTs dispersion is 12%.
And (3) performance testing:
1. testing of Cyclic tensile Properties and conductivity
The resistance change rate and the fluctuation value of the resistance change rate are important indexes for measuring the conductivity and the working stability of the film, the larger the resistance change rate is, the better the conductivity is and the higher the sensitivity is, the smaller the fluctuation value of the resistance change rate is, the higher the working accuracy is and the stronger the working stability is, the fluctuation range of the peak value of the resistance change rate is larger, and the accuracy is also influenced.
After cutting a polyurethane film obtained in example 2 as test example 1, a polyurethane film obtained in example 1 as test example 2, a polyurethane film obtained in example 3 as test example 3, and a polyurethane film obtained in example 4 as test example 4 into 1cm x 4cm strips, the initial resistance values of test examples 1 to 4 and comparative examples were first measured at 0% elongation using a textile dynamic resistance tester, and the initial resistance values of test examples 1 to 4 and comparative examples were measured as 56863 Ω, 7135 Ω, 5951 Ω, 6015 Ω, 3265 Ω and 2655335 Ω, respectively, and then the resistance change rates of test examples 1 to 4 and comparative examples were measured at 20% elongation at a tensile speed of 30mm/min, the change in resistance with elongation for test examples 1 to 4 and comparative examples is shown in fig. 1, the maximum elongation per cycle is 20% for 20 cycles of the cyclic stretching test, the change in resistance during different cyclic stretching for comparative examples is shown in fig. 2, and the change in resistance during different cyclic stretching for test examples 1 to 4 is shown in fig. 3 to 6, respectively:
as can be seen from fig. 1, the resistance change rate of the film increases with the increase of the elongation, wherein the change of test example 4 (12% CNTs) is most significant, and the next time, test example 3 (9% CNTs), the sensitivity strain factor (GF) of the polyurethane film at different elongations can be calculated by fitting based on fig. 1, the GF value of test example 4 is the largest at an elongation of 20% and is 41.9, while test example 1 is only 12.0, test example 2 is only 17.6, test example 4 is only 27.9, comparative example is only 6.8;
as can be seen from FIG. 2, the peak value of the change rate of resistance of the comparative example fluctuates from 1.2 to 1.3, the average value of the change rate of resistance is 1.28, and the fluctuation value of the change rate of resistance is about 7.8%, as can be seen from FIG. 3, the fluctuation value of the change rate of resistance of test example 1 at the first two cycles of stretching is large because the CNTs dispersion concentration is low and the CNTs fiber is not completely and uniformly adsorbed on the surface of the film, resulting in a large change rate of resistance, the peak value of the change rate of resistance of test example 1 at the latter several cycles of stretching is stable to fluctuate within 2.0 to 2.4, the average value of the change rate of resistance is 2.15, and the fluctuation value of the change rate is about 18.6%, as can be seen from FIG. 4, the peak value of the change rate of resistance of test example 2 fluctuates within 3.6 to 4.6, the average value of the change rate of resistance is 4.36, the fluctuation value of the change rate is about 22.9%, as can be seen from FIG. 5, the peak value of the change rate of resistance of test example 3 is within 5 to 5.6 to 5.8, the average value of the resistance change rate was 5.85, the fluctuation value of the resistance change rate was about 3.4%, as can be seen from fig. 6, the peak value of the resistance change rate of test example 4 fluctuated within 9.0 to 11.3, the average value of the resistance change rate was 9.43, and the fluctuation value of the resistance change rate was about 24.4%, because the amount of CNTs loaded on the conductive film of test example 1 was very small and the resistance change was not significant during stretching, and because the CNTs were stacked and wound on the conductive film due to too high concentration of the impregnated CNTs dispersion in test example 4, so that the conductive network was damaged little during stretching and the resistance change was not significant during stretching, and also, in fig. 2 to 6, a weak shoulder was generated in substantially every cycle, because there was competition between the damage and the restructuring of the conductive network in the film during stretching and releasing, and the damage of the conductive network was more severe with increasing strain, and the relative resistance change value of the fiber sensor was larger, the shoulder peaks are more and more obvious, because the macromolecular chains in the film can not be quickly recovered to the initial state after being stretched under the action of external force, and the hysteresis phenomenon exists;
therefore, the film prepared by the method has high resistance change rate, good sensitivity for testing a human body, small fluctuation value of the resistance change rate, high precision for testing the human body and strong working stability, and the following human body part tests are carried out by adopting the test example 3 for verifying the high sensitivity, the working precision and the working stability:
firstly, cutting the test example 3 into 1 cm-by-3 cm strips, then attaching the strip-shaped film to the finger, wrist and laryngeal node of a human body, connecting the two ends of the film with a digital oscilloscope through coppery glue, wherein the digital oscilloscope is used for recording the change of resistance value in the test process so as to reflect the movement of the human body part, wherein, when the test example 3 is attached to the finger joint of the human body, the finger joint is bent back and forth for 9 times (0-90 degrees) within 20s, the results of monitoring the change in resistance are shown in FIG. 7, and in test example 3, when the wrist joint was attached to a human body, the wrist joint was bent back and forth 5 times (0-90 degree bend) within 15 seconds, the monitoring result of the resistance value change is shown in figure 8, when the test example 3 is attached to the laryngeal prominence of a human body, the laryngeal prominence is sequentially increased to generate sound volume to cause the laryngeal prominence to generate vibration with different amplitudes, and the monitoring result of the resistance value change is shown in figure 9:
as can be seen from fig. 7, the initial resistance of the film is about 6000 Ω, even after stretching for 9 cycles, the resistance is still stable about 6000 Ω, in the figure, the LM section is the resistance change in the bending process of the finger joint, the corresponding resistance value is also increasingly larger along with the gradual increase of the bending angle of the finger joint, the MN section is the resistance change in the straightening recovery process of the finger joint, the corresponding resistance value is also gradually smaller along with the gradual decrease of the bending angle of the finger joint, it can be seen that the conductive film exhibits regular change at the detection position of the finger joint, and the operation is relatively stable, so that the sensitivity for monitoring the movement of the finger joint of the human body is good;
as can be seen from fig. 8, the initial resistance of the film is about 5000 Ω, even after stretching for 5 cycles, the resistance is still stable at about 5000 Ω, in the figure, the OP section is the resistance change during the process of straightening and bending the wrist joint, in the process of bending the wrist joint, along with the gradual increase of the bending angle of the wrist joint, the corresponding resistance value is also larger and larger, the PQ section is the resistance change during the process of recovering the wrist joint, along with the gradual decrease of the bending angle of the wrist joint, the corresponding resistance value is also gradually smaller, it can be seen that the conductive film presents regular change at the detection position of the wrist joint, and the operation is relatively stable, so that the sensitivity for monitoring the movement of the wrist joint of the human body is good;
as can be seen from fig. 9, as the sound volume is larger and larger, the resistance peak value is also larger and larger, and it can be seen that the conductive film is used for monitoring the movement of the human sound organ;
in conclusion, the film prepared by the method has high conductivity and high tensile property, can be used as a flexible film sensor, monitors the movement of finger joints, wrist joints and sounding organs of a human body through the resistance change of the film, and has high sensitivity and good stability.
2. Thermal stability test
The thermal stability of the ordinary PU film of test example 3 was measured by a thermogravimetric analyzer (TGA, model NETZSCH TG 209F 1), and the results were: test example 3 started to decompose when the temperature reached 350 c, whereas the conventional PU film started to decompose at 275 c, and thus it was found that the film prepared by the method had high thermal stability.
Claims (10)
1. The preparation method of the polyurethane film loaded with the redox graphene and the carbon nano tubes is characterized by comprising the following steps of:
the preparation method of the polyurethane film is carried out according to the following steps in sequence:
s1, adding Polyurethane (PU) into N, N-dimethylformamide, uniformly mixing to obtain a solution A, carrying out centrifugal spinning on the solution A to obtain polyurethane nanofibers, and finally collecting the polyurethane nanofibers and pressing the polyurethane nanofibers into polyurethane nanofiber films;
s2, firstly, soaking the polyurethane nanofiber film obtained in the step S1 into graphene oxide dispersion liquid, then taking out the polyurethane nanofiber film to be dried, and repeating the step S2 for n times in a circulating manner to obtain a polyurethane film loaded with graphene oxide;
s3, reducing the polyurethane conductive membrane loaded with the graphene oxide by adopting a reducing agent to obtain a polyurethane film loaded with the redox graphene;
s4, immersing the polyurethane film loaded with the redox graphene into the carbon nano tube CNTs dispersion liquid, then taking out, sequentially cleaning and drying, and circularly repeating the step S4 for m times to obtain the polyurethane film loaded with the redox graphene and the carbon nano tube.
2. The method for preparing a polyurethane film with negative oxidation-reduction graphene and carbon nano tubes according to claim 1, wherein the method comprises the following steps: in step S1, the mass percentage concentration of the solution A is 17-19%.
3. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S1, the rotation speed of the centrifugal spinning is 4400-4600r/min, the collection distance is 28-32cm, and the mixing is specifically stirring for 7.5-8.5h at 78-82 ℃.
4. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S1, the collecting of the polyurethane nanofibers is to overlap the polyurethane nanofibers 6-7 times along their orientation, and the pressing of the polyurethane nanofibers is to press the polyurethane nanofibers with a weight of 2-2.5kg, and then dry the polyurethane nanofibers at 58-62 ℃ for 2-2.5 h.
5. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S2, n is at least 5 times, and the immersion time is 25-35 min.
6. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S2, the mass-volume concentration of the graphene oxide dispersion liquid is 0.45 to 0.55 mg/mL.
7. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S3, the reducing agent is hydrazine hydrate.
8. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 3-12%.
9. The method for preparing a polyurethane film with redox graphene and carbon nanotubes as claimed in claim 8, wherein the method comprises the following steps: in step S4, the mass percentage concentration of the carbon nanotube CNTs dispersion is 6-9%.
10. The method for preparing a polyurethane film carrying redox graphene and carbon nanotubes according to claim 1 or 2, wherein: in the step S4, m is 3 times, the first immersion time is 8-10h, ultrasonic dispersion is carried out for 1-1.5h after the second immersion, then the materials are taken out and cleaned and dried in sequence, and the third immersion time is 12-14 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115710825A (en) * | 2022-12-15 | 2023-02-24 | 武汉纺织大学 | Electrically-driven thermochromic fiber and preparation method thereof |
| CN115710825B (en) * | 2022-12-15 | 2024-05-31 | 武汉纺织大学 | Electrically driven thermochromic fiber and preparation method thereof |
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| CN115710825A (en) * | 2022-12-15 | 2023-02-24 | 武汉纺织大学 | Electrically-driven thermochromic fiber and preparation method thereof |
| CN115710825B (en) * | 2022-12-15 | 2024-05-31 | 武汉纺织大学 | Electrically driven thermochromic fiber and preparation method thereof |
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