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CN-121977432-A - Preparation method of MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with bimodal fold structure

CN121977432ACN 121977432 ACN121977432 ACN 121977432ACN-121977432-A

Abstract

The invention belongs to the technical field of intelligent wearable electronics, and particularly relates to a preparation method of an MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with a bimodal fold structure. The invention washes and dries TPU fiber film, then soaks in chloroform (CHCl 3 ) to swell, then uses mould to fix and dry, soaks the pretreated fiber film in Cetyl Trimethyl Ammonium Bromide (CTAB) solution to modify, then puts in MXene/CNTs mixed solution to ultrasound, makes MXene/CNTs uniformly attach on the TPU fiber surface, after deswelling, demoulding to retract the fiber film, and repeats the steps of CTAB modification and MXene/CNTs attachment, thus obtaining the MXene/CNTs bimodal fold conductive fiber film with different buckling. And (3) attaching Phytic Acid (PA) on the surface of the fiber by a repeated dipping method, then assembling a copper electrode and packaging by PDMS to obtain the flame-retardant flexible strain sensor with the dual-mode fold conductive structure.

Inventors

  • CHU ZHENMING
  • QIAO MENGLIN
  • Liu Zeda

Assignees

  • 辽宁大学

Dates

Publication Date
20260505
Application Date
20260130

Claims (7)

  1. 1. The preparation method of the MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with the bimodal fold structure is characterized by comprising the following steps of: 1) Dissolving cetyl trimethyl ammonium bromide CTAB in deionized water, and uniformly stirring to obtain a CTAB solution; 2) Placing carboxylated carbon nanotube CNTs into the diluted MXene solution, mixing with ultrasound to obtain uniformly dispersed MXene/CNTs mixed solution; 3) Cleaning and drying a TPU fiber film to be used as an elastic substrate, putting the elastic substrate into chloroform CHCl 3 solution to be swelled, fixing and drying the elastic substrate by a mould, and immersing the elastic substrate into CTAB solution to be modified; 4) Immersing a CTAB modified fiber membrane into a mixed solution of MXene/CNTs, and performing in-situ deposition by ultrasonic assistance to obtain a single-layer MXene/CNTs/TPU fiber membrane, and then forming a fold structure on the surface of the single-layer MXene/CNTs/TPU fiber membrane due to substrate retraction in the swelling elimination process to finally obtain the single-layer fold MXene/CNTs/TPU fiber membrane with the fold structure; 5) Repeating the step 3) and the step 4), and drying to obtain the bimodal wrinkling MXene/CNTs/TPU fiber membrane with different buckling; 6) Attaching phytic acid PA to the surfaces of the two MXene/CNTs/TPU fiber films with single-layer wrinkles and double-mode wrinkles by a repeated impregnation method to respectively obtain a single-layer wrinkle fiber film MWFM and a double-mode wrinkle fiber film BWFM with flame retardance; 7) And assembling a copper electrode on the fiber membrane by using conductive silver paste, and immersing the fiber membrane into a mixed solution containing the PDMS prepolymer and the curing agent for encapsulation, so as to obtain the single-layer pleated fiber membrane MWFM and the bimodal pleated fiber membrane BWFM flame-retardant flexible strain sensor.
  2. 2. The preparation method according to claim 1, wherein the step 1) is realized by adding 22-26 mg of CTAB powder into 115-125 mL of deionized water, and magnetically stirring for 8-12 min to obtain 0.19-0.21 mg/mL of CTAB solution.
  3. 3. The preparation method according to claim 1, wherein step 2) is achieved by: 2.1 Firstly, placing lithium fluoride LiF and HCl in a polytetrafluoroethylene reaction kettle, stirring for 12-18 min at a water bath condition of 35-45 ℃, then, slowly adding titanium aluminum carbide Ti 3 AlC 2 powder in batches, carrying out chemical etching reaction in a sealed environment, washing a product for 2-3 times by using HCl after the reaction is finished, repeatedly washing the product until the product is neutral, carrying out ultrasonic treatment on the obtained sample for 0.5-1 h under the protection of nitrogen, then, centrifuging again, collecting supernatant, and obtaining stable MXene suspension, diluting to 1 mg/mL by using deionized water to obtain MXene solution of 1 mg/mL for later use; 2.2 2.2-2.6 mg of carboxylated carbon nanotube CNTs are weighed and put into 115-125 mL of 1 mg/mL of MXene solution, ultrasonic dispersion is carried out, the ultrasonic power is 120-150W, the ultrasonic dispersion time is 0.5-1.5 h, and finally the mixed solution of MXene/CNTs with the mass ratio of MXene to CNTs of 50:1 is obtained.
  4. 4. The preparation method according to claim 1, wherein step 3) is achieved by: 3.1 Ultrasonic cleaning the TPU fiber film by deionized water, and drying at 50-60 ℃ to obtain an elastic substrate; 3.2 Soaking the TPU fiber membrane in chloroform CHCl 3 for 3-7 min, and after swelling, fixing and drying for 25-35 min by using a die; 3.3 Immersing the TPU fiber film treated in the step 2) into a CTAB solution, carrying out ultrasonic stirring for 25-35 min for surface modification treatment, and then drying at 50-60 ℃.
  5. 5. The preparation method according to claim 1, wherein step 4) is achieved by: 4.1 Immersing the CTAB modified fiber membrane obtained in the step 3) into the MXene/CNTs mixed solution prepared in the step 2), ultrasonically stirring for 0.5-1.5 h, and drying to obtain a single-layer MXene/CNTs/TPU fiber membrane; 4.2 After the single-layer MXene/CNTs/TPU fiber film is deswelled, the single-layer MXene/CNTs/TPU fiber film is demoulded and put into a 50-60 ℃ oven to be dried for 25-35 min, so that the single-layer MXene/CNTs/TPU fiber film is slowly retracted to form a single-layer fold structure.
  6. 6. The preparation method according to claim 1, wherein the step 6) is realized by immersing two types of MXene/CNTs/TPU fiber films, namely single-layer folding and bimodal folding, respectively in a CTAB solution of 0.19-0.21 mg/mL for modification again, immersing the fiber films into a PA solution with the mass fraction of 2-4% for treatment for 25-35 min, and repeating the above processes twice, wherein the finally obtained products are respectively denoted as a single-layer folding fiber film MWFM and a bimodal folding fiber film BWFM.
  7. 7. The method of claim 1, wherein step 7) is accomplished by: 7.1 Assembling MWFM and BWFM of the copper electrode by using conductive silver paste, wrapping a fiber film with the length of 0.9-1.1 cm and the width of 0.4-0.6 cm by using the conductive silver paste during assembly, and then drying and curing for 0.5-1.5 hours at 50-60 ℃; 7.2 Immersing the fiber membrane sensing area provided with the copper electrode into a mixed solution of the PDMS prepolymer and the curing agent for 25-35 seconds, and curing for 3.5-4.5 hours at 50-60 ℃, wherein the mass ratio of the PDMS prepolymer to the curing agent is 10:1, and finally obtaining the MWFM and BWFM flame-retardant flexible strain sensor respectively.

Description

Preparation method of MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with bimodal fold structure Technical Field The invention belongs to the technical field of intelligent wearable electronics, and particularly relates to a preparation method of an MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with a bimodal fold structure. Background In recent years, wearable electronic textiles show great potential in many fields of intelligent human-computer interaction, human health/motion detection, fire alarm and the like due to good air permeability, flexibility and wearing comfort. By combining the functional material with the fabric substrate, not only can the sensitive monitoring of human body movement and physiological signals be realized, but also multiple functions such as energy management, temperature regulation and even fire alarm can be integrated, and the wearable technology is promoted to develop towards the intelligent and multifunctional directions. Disclosure of Invention The invention aims to prepare the high-performance wearable strain sensor with flame retardance, ventilation and comfortable wearing characteristics by constructing the MXene/CNTs/TPU composite fiber membrane with the bimodal fold structure. The invention has high sensitivity and wide strain range, and provides thinking for the application of multifunctional wearable electronic equipment and intelligent fabrics in reality. The technical scheme adopted by the invention is as follows: A preparation method of an MXene/CNTs/TPU fiber membrane flame-retardant flexible strain sensor with a bimodal fold structure comprises the following steps: 1) Dissolving cetyl trimethyl ammonium bromide CTAB in deionized water, and uniformly stirring to obtain a CTAB solution; 2) Placing carboxylated carbon nanotube CNTs into the diluted MXene solution, mixing with ultrasound to obtain uniformly dispersed MXene/CNTs mixed solution; 3) Cleaning and drying a TPU fiber film to be used as an elastic substrate, putting the elastic substrate into chloroform CHCl 3 solution to be swelled, fixing and drying the elastic substrate by a mould, and immersing the elastic substrate into CTAB solution to be modified; 4) Immersing a CTAB modified fiber membrane into a mixed solution of MXene/CNTs, and performing in-situ deposition by ultrasonic assistance to obtain a single-layer MXene/CNTs/TPU fiber membrane, and then forming a fold structure on the surface of the single-layer MXene/CNTs/TPU fiber membrane due to substrate retraction in the swelling elimination process to finally obtain the single-layer fold MXene/CNTs/TPU fiber membrane with the fold structure; 5) Repeating the step 3) and the step 4), and drying to obtain the bimodal wrinkling MXene/CNTs/TPU fiber membrane with different buckling; 6) Attaching phytic acid PA to the surfaces of the two MXene/CNTs/TPU fiber films with single-layer wrinkles and double-mode wrinkles by a repeated impregnation method to respectively obtain a single-layer wrinkle fiber film MWFM and a double-mode wrinkle fiber film BWFM with flame retardance; 7) And assembling a copper electrode on the fiber membrane by using conductive silver paste, and immersing the fiber membrane into a mixed solution containing the PDMS prepolymer and the curing agent for encapsulation, so as to obtain the single-layer pleated fiber membrane MWFM and the bimodal pleated fiber membrane BWFM flame-retardant flexible strain sensor. Further, the preparation method comprises the following step 1) that 22-26 mg of CTAB powder is added into 115-125 mL of deionized water, and magnetic stirring is carried out for 8-12 min to obtain 0.19-0.21 mg/mL of CTAB solution. Further, the preparation method, step 2), is realized by the following steps: 2.1 Firstly, placing lithium fluoride LiF and HCl in a polytetrafluoroethylene reaction kettle, stirring for 12-18 min at a water bath condition of 35-45 ℃, then, slowly adding titanium aluminum carbide Ti 3AlC2 powder in batches, carrying out chemical etching reaction in a sealed environment, washing a product for 2-3 times by using HCl after the reaction is finished, repeatedly washing the product until the product is neutral, carrying out ultrasonic treatment on the obtained sample for 0.5-1 h under the protection of nitrogen, then, centrifuging again, collecting supernatant, and obtaining stable MXene suspension, diluting to 1 mg/mL by using deionized water to obtain MXene solution of 1 mg/mL for later use; 2.2 2.2-2.6 mg of carboxylated carbon nanotube CNTs are weighed and put into 115-125 mL of 1 mg/mL of MXene solution, ultrasonic dispersion is carried out, the ultrasonic power is 120-150W, the ultrasonic dispersion time is 0.5-1.5 h, and finally the mixed solution of MXene/CNTs with the mass ratio of MXene to CNTs of 50:1 is obtained. Further, the preparation method, step 3), is realized by the following steps: 3.1 Ultrasonic cleaning the TPU fiber film by deionized water