EP4444942A2 - Faser und verfahren zur herstellung davon - Google Patents

Faser und verfahren zur herstellung davon

Info

Publication number
EP4444942A2
EP4444942A2 EP23753293.2A EP23753293A EP4444942A2 EP 4444942 A2 EP4444942 A2 EP 4444942A2 EP 23753293 A EP23753293 A EP 23753293A EP 4444942 A2 EP4444942 A2 EP 4444942A2
Authority
EP
European Patent Office
Prior art keywords
mxene
fibers
fiber
various embodiments
cross
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP23753293.2A
Other languages
English (en)
French (fr)
Other versions
EP4444942A4 (de
Inventor
Lei Wei
Tianzhu ZHOU
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanyang Technological University
Original Assignee
Nanyang Technological University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanyang Technological University filed Critical Nanyang Technological University
Publication of EP4444942A2 publication Critical patent/EP4444942A2/de
Publication of EP4444942A4 publication Critical patent/EP4444942A4/de
Pending legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/34—Core-skin structure; Spinnerette packs therefor

Definitions

  • Various embodiments of this disclosure may relate to a fiber.
  • Various embodiments of this disclosure may relate to a method of forming a fiber.
  • Fibers as the basic building blocks of textiles, have been actively engaged in a wide range of our daily activities, including health management, human-computer interaction, movement monitoring, soft robotics, disease prevention, and more.
  • Research focus is directed on achieving fibers with high mechanical and good electrical performance, with emphasis on conductive materials making up the fibers.
  • These conductive materials range from carbon-based materials, metal-based materials, and conductive polymers-based materials.
  • MXenes as a new class of two-dimensional (2D) inorganic compounds, are promising materials for the development of fiber-based devices, owing to their combined outstanding mechanical, electrical, and electromagnetic properties.
  • MXene (TisC2T x ) nanosheets can be prepared into high-performance nanocomposites due to their surface terminated moieties (T x ), such as -OH, -O, and -F.
  • T x surface terminated moieties
  • Many studies have been carried out to fabricate MXene fibers based on MXene (TisC2T x ) nanosheets by various processes, including wet spinning, coating, electrospinning, and biscrolling method.
  • MXene fibers have therefore been successfully fabricated with the desired electrical conductivity and mechanical properties, such as MXene/reduced graphene oxide (rGO), MXene/cellulose nanofibrils, Kevlar/MXene, and nylon/MXene.
  • FIG. 1 shows a schematic of a method of forming a fiber according to various embodiments.
  • FIG. 2 shows a schematic of a fiber according to various embodiments.
  • FIG. 3A is a schematic illustrating the fabrication of ultra-compact MXene-based fibers with the protective layer (MGP-T) via continuous wet spinning and thermal drawing, and the formation of MXene-based textiles according to various embodiments.
  • MGP-T protective layer
  • FIG. 3B shows (top left) scanning electron microscopy (SEM) images of pure MXene fibers (normal and zoomed in) according to various embodiments; (top right) a wide-angle X-ray scattering (WAXS) pattern of the pure MXene fibers according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stress-strain curve of the pure MXene fibers according to various embodiments.
  • SEM scanning electron microscopy
  • WAXS wide-angle X-ray scattering
  • FIG. 3C shows (top left) a scanning electron microscopy (SEM) images of resulting wet spun MXene fibers (MGP) (normal and zoomed in) according to various embodiments; (top right) a wide-angle X-ray scattering (WAXS) pattern of the resulting wet spun MXene fibers (MGP) according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stress-strain curve of the resulting wet spun MXene fibers (MGP) according to various embodiments.
  • SEM scanning electron microscopy
  • FIG. 3D shows (top left) a scanning electron microscopy (SEM) images of resulting MXene- based fibers with protective layers (MGP-T) (normal and zoomed in) according to various embodiments; (top right) a wide-angle X-ray scattering (WAXS) pattern of the resulting fibers with protective layers (MGP-T) according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stressstrain curve of the resulting fibers with protective layers (MGP-T)) according to various embodiments.
  • SEM scanning electron microscopy
  • FIG. 4A shows a scanning electron microscopy (SEM) image of titanium aluminum carbide (TisAKZy according to various embodiments.
  • FIG. 4B shows a scanning electron microscopy (SEM) image of accordion-like MXene according to various embodiments.
  • FIG. 5A shows a scanning electron microscopy (SEM) image of exfoliated MXene nanosheets with a lateral size of about 10 pm according to various embodiments.
  • FIG. 5B shows a plot of count as a function of lateral size (in micrometers or pm) illustrating the size distribution for the exfoliated MXene nanosheets shown in FIG. 5A according to various embodiments.
  • FIG. 5C shows an atomic force microscopy (AFM) image of exfoliated MXene nanosheets with a thickness of about 10 pm according to various embodiments.
  • AFM atomic force microscopy
  • FIG. 5D shows a plot of height (in nanometers or nm) as a function of lateral size (in micrometers or pm) illustrating the thickness of the exfoliated MXene nanosheets shown in FIG. 5C according to various embodiments.
  • FIG. 6A shows a transmission electron microscopy (TEM) image of exfoliated MXene nanosheets according to various embodiments.
  • TEM transmission electron microscopy
  • FIG. 6B shows the corresponding high-resolution transmission electron microscopy (HR-TEM) image of the exfoliated MXene nanosheets; and (inset) selected area electron diffraction (SAED) pattern of the exfoliated MXene nanosheets according to various embodiments.
  • HR-TEM transmission electron microscopy
  • SAED selected area electron diffraction
  • FIG. 7 is a plot of intensity (in arbitrary units or a.u.) as a function of angle (29) showing the X-ray diffraction (XRD) patterns of primitive titanium aluminum carbide (TisAlC2) and exfoliated MXene (TisC2T x ) nanosheets according to various embodiments.
  • XRD X-ray diffraction
  • FIG. 8 show polarizing optical microscope (POM) images of MXene-glutaraldehyde (GA) spinning dispersion with concentrations from ⁇ 5 mg mL 1 to ⁇ 30 mg mL 1 according to various embodiments.
  • POM polarizing optical microscope
  • FIG. 9A shows a plot of viscosity (in Pascals seconds or Pa.s) as a function of shear rate (in per second or 1/s) illustrating the variation of viscosity with shear rate of different concentrations of the spinning dispersion according to various embodiments.
  • FIG. 9B shows a plot of shear stress (in Pascals or Pa) as a function of shear rate (in per second or 1/s) illustrating the variation of shear stress with shear rate of different concentrations of the spinning dispersion according to various embodiments.
  • FIG. 9C shows a plot of modulus (in Pascals or Pa) as a function of frequency (in per second or 1/s) illustrating the variation of modulus with frequency of different concentrations of the spinning dispersion according to various embodiments.
  • FIG. 10A shows a line drawing of several meter long wet spun (MGP) fibers according to various embodiments; and (inset) a magnified line drawing showing the axial SEM morphology of a wet spun (MGP) fiber according to various embodiments.
  • MGP meter long wet spun
  • FIG. 10B shows a plot of intensity (in arbitrary units or a.u.) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the obtained fibers according to various embodiments, glutaraldehyde (GA), polyvinyl alcohol (PVA) and pure MXene.
  • FTIR Fourier transform infrared
  • FIG. IOC shows a plot of reflectance (in percent or %) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the obtained fibers according to various embodiments, glutaraldehyde (GA), polyvinyl alcohol (PVA) and pure MXene.
  • FTIR Fourier transform infrared
  • FIG. 10D shows a plot of reflectance (in percent or %) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the wet spun (MGP) fibers with different weight ratios of polyvinyl alcohol (PVA) according to various embodiments.
  • FTIR Fourier transform infrared
  • FIG. 11 shows a plot of intensity (in arbitrary units or a.u.) as a function of wavenumbers (per centimeter or cm 1 ) showing the X-ray photoelectron spectroscopy (XPS) spectra of the fabricated fibers according to various embodiments, pure MXene and MAX (TisAlC2).
  • FIG. 12A shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron volts or eV) showing the titanium (Ti) 2p spectra of the fabricated fibers according to various embodiments and pure MXene fibers.
  • FIG. 12B shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron volts or eV) showing the oxygen (O) Is spectra of the fabricated fibers according to various embodiments and pure MXene fibers.
  • FIG. 12C shows a table illustrating the atomic percentage of O-Ti-O, C-Ti-OX, O-C, and C-Ti- OH according to the oxygen (O) Is peak in the obtained X-ray photoelectron spectroscopy (XPS) spectra of the obtained fibers according to various embodiments and pure MXene fibers.
  • FIG. 13A illustrates one possible mechanism for the formation of Ti-O-C covalent bond between MXene nanosheets and glutaraldehyde molecules according to various embodiments.
  • FIG. 13B shows a structure graph of the covalent bond between MXene nanosheets and glutaraldehyde (GA) and the hydrogen bond between MXene nanosheets and polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 14A shows (a) wide-angle X-ray scattering (WAXS) patterns of the fabricated intermediate (MG) fibers with different weight ratios of glutaraldehyde molecules from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments; and (b) small-angle X-ray scattering (SAXS) patterns of the fabricated intermediate (MG) fibers with different weight ratios of glutaraldehyde molecules from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments.
  • WAXS wide-angle X-ray scattering
  • SAXS small-angle X-ray scattering
  • FIG. 14B shows a plot of orientation order (f) as a function of percentage of glutaraldehyde (in weight percent or wt%) showing the variation of the orientation of the intermediate (MG) fibers with different amounts of glutaraldehyde based on wide-angle X-ray scattering (WAXS) patterns according to various embodiments.
  • FIG. 14C shows a plot of density (in grams per cubic centimeter) / porosity (in percent or %) as a function of percentage of glutaraldehyde (in weight percent or wt%) showing the variation of density and porosity of the intermediate (MG) fibers with different amounts of glutaraldehyde according to various embodiments.
  • FIG. 15 shows the wide-angle X-ray scattering (WAXS) and (inset) small-angle X-ray scattering (SAXS) patterns of the fabricated wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • WAXS wide-angle X-ray scattering
  • SAXS small-angle X-ray scattering
  • FIG. 16A shows a plot of orientation order (f) as a function of percentage of polyvinyl alcohol (PVA) (in weight percent or wt%) showing the variation of the orientation of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) based on wide-angle X-ray scattering (WAXS) patterns according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 16B shows a plot of density (in grams per cubic centimeter) / porosity (in percent or %) as a function of percentage of polyvinyl alcohol (in weight percent or wt%) showing the variation of density and porosity of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 16C shows a plot of tensile strength (in mega-Pascals or MPa) / toughness (in mega-Joules or MJ m -3 ) as a function of percentage of polyvinyl alcohol (PVA) (in weight percent or wt%) showing the variation of strength and toughness of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 17A shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the intermediate (MG) fibers with different amounts of glutaraldehyde from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments.
  • FIG. 17B shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) from 1 weight percent (wt%) to 15 weight percent (wt%) according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 17C shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the various fabricated fibers according to various embodiments.
  • FIG. 18 shows a plot of weight loss (in percent or %) as a function of temperature (in degrees Celsius or °C) illustrating the thermogravimetric analysis (TGA) results of polyvinyl alcohol (PVA), glutaraldehyde (GA) and various fabricated fibers according to various embodiments.
  • FIG. 19 shows a table illustrating the orientation order (f) and porosity (in percent or %) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • FIG. 20 shows a table illustrating the orientation order (f) and porosity (in percent or %) of the fabricated wet spun (MGP) fibers with different weight percentage of polyvinyl alcohol (PVA) molecules according to various embodiments.
  • FIG. 21 shows a table illustrating the tensile strengths (in mega-Pascals or MPa), strain (in percent or %) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • FIG. 22A is a plot comparing the tensile strengths and toughness of fabricated intermediate (MG) fibers with different weight percentages of glutaraldehyde molecules from 0 wt% to 20 wt% according to various embodiments.
  • FIG. 22B is a plot comparing the electrical conductivity of fabricated intermediate (MG) fibers with different weight percentages of glutaraldehyde molecules from 0 wt% to 20 wt% according to various embodiments.
  • FIG. 23A shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of pure Mxene fibers according to various embodiments.
  • FIG. 23B shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 2 weight percent (2 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23C shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 5 weight percent (5 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23D shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 10 weight percent (10 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23E shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 15 weight percent (15 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23F shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 20 weight percent (20 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 24 shows a table illustrating the electrical conductivity (in siemens per centimeter or S cm' 1 ) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • FIG. 25A shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 5 weight percent (5 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 25B shows a plot of stress (in mega-Pascals or Mpa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 1 weight percent (1 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • MGP wet spun
  • FIG. 25C shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 2 weight percent (2 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25D shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 5 weight percent (5 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25F shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 15 weight percent (15 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25G shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of pure polyvinyl alcohol (PVA) fibers.
  • FIG. 26 shows a table illustrating the tensile strengths (in mega-Pascals or MPa), strain (in percent or %) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of various fibers with different weight percentage of polyvinyl alcohol (PVA) according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 27 is a plot comparing the electrical conductivity of MXene fibers, intermediate (MG) fibers, and wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 28 shows a table illustrating the electrical conductivity (in siemens per centimeter or S cm' ’) of intermediate fibers and wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 29 shows scanning electron microcopy images of the cross-sections of intermediate (MG) fibers with different weight percentages (wt%) of polyvinyl alcohol (PVA) from 0 wt% to 20 wt% according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 30 shows scanning electron microcopy images of the cross-sections of wet spun (MGP) fibers with different weight percentages (wt%) of polyvinyl alcohol (PVA) from 1 wt% to 15 wt% according to various embodiments.
  • MGP wet spun
  • PVA polyvinyl alcohol
  • FIG. 31 A shows a plot of temperature (in degree Celsius or °C) as a function of scattering vector (per Angstrom or A 1 ) illustrating the in-situ X-ray diffraction (XRD) patterns of a wet spun (MGP) fiber according to various embodiments.
  • FIG. 3 IB shows a plot of d-spacing (in Angstroms or A) as a function of temperature (in degree Celsius or °C) illustrating the d-spacing curve according to the in-situ X-ray diffraction (XRD) pattern according to various embodiments.
  • FIG. 31C shows a plot of intensity (in arbitrary units or a.u.) as a function of scattering vector q (per Angstrom or A 1 ) showing the in-situ X-ray diffraction (XRD) patterns of fabricated wet spun (MGP) fibers being heated under various temperatures from 25 °C to 350 °C according to various embodiments.
  • XRD in-situ X-ray diffraction
  • FIG. 3 ID shows a plot of porosity (in percent or %) as a function of temperature (in degree Celsius or °C) illustrated the porosity of wet spun (MGP) fibers being heated according to various embodiments.
  • FIG. 32A shows a schematic diagram of wet spun (MGP) fibers being heated according to various embodiments.
  • FIG. 32B shows the in-situ small-angle X-ray scattering (SAXS) patterns of fabricated wet spun
  • MGP polyvinyl alcohol
  • FIG. 32C shows a plot of intensity as a function of scattering vector q (per Angstrom or A 1 ) illustrating the intensity curves of wet spun fibers under different temperatures based on the small-angle X-ray scattering (SAXS) patterns according to various embodiments.
  • SAXS small-angle X-ray scattering
  • FIG. 33A shows a schematic diagram of forming the cross-linked MXene-based (MGP-T) fibers with protective layers from wet spun (MGP) fibers with axial stress and perpendicular stress during thermal drawing according to various embodiments.
  • FIG. 33B shows a line drawing of several meters long cross-linked MXene-based fibers (MGP- T) fibers with protective layers according to various embodiments.
  • FIG. 33C shows another line drawing of cross-linked MXene-based (MGP-T) fibers with protective layers according to various embodiments.
  • FIG. 34A is a plot comparing the orientation orders (f) of three cross-linked MXene-based (MGP-T) fibers with protective layers fabricated by various draw-down ratios according to various embodiments, with the inset showing the wide-angle X-ray scattering (WAXS) pattern of the various fibers according to various embodiments.
  • MGP-T cross-linked MXene-based
  • WAXS wide-angle X-ray scattering
  • FIG. 34B shows a plot of intensity (in arbitrary units or a.u.) as a function of azimuthal angle (in degrees or °) showing the variation across fibers formed by different draw-down ratios based on wide-angle X-ray scattering (WAXS) patterns according to various embodiments.
  • WAXS wide-angle X-ray scattering
  • FIG. 34C shows a table comparing the orientation order (f) and porosity (in percent or %) of the fabricated MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios according to various embodiments.
  • FIG. 35A shows a plot of porosity (in percent or %)/conductivity (in X 10 3 siemens per centimeter or S cm 1 ) comparing the porosity and electrical conductivity of the various fabricated MXene-based fibers with protective layers (MGP-T) formed using different drawdown ratios according to various embodiments.
  • FIG. 35B shows the scanning electron microscopy (SEM) cross-sectional images of the MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios (a: MGP-Ti, b: MGP-T2, c: MGP-T3) with energy-dispersive X-ray spectroscopy (EDX) according to various embodiments.
  • SEM scanning electron microscopy
  • FIG. 36A shows a high resolution transmission electron microscopy (HR-TEM) image of a Mxene-based fiber with protective layer (MGP-T) according to various embodiments.
  • HR-TEM transmission electron microscopy
  • FIG. 36B shows a zoomed in view of the area indicated in FIG. 36A according to various embodiments.
  • FIG. 36C shows the EDX spectrum of the selected area shown in FIG. 36A according to various embodiments.
  • FIG. 37 shows a table illustrating the electrical conductivity of the fabricated MXene-based fibers with protective layers (MGP-T) formed using various draw-down ratios according to various embodiments.
  • FIG. 38A shows a plot of tensile strength (in mega-Pascals or MPa)/toughness (in mega-Joules per cubic meter or MJ m -3 ) comparing the tensile strength and toughness of the various fabricated cross-linked MXene-based (MGP-T) fibers formed using different draw-down ratios according to various embodiments.
  • FIG. 38B shows a table illustrating the tensile strength (in mega-Pascals or MPa) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of the fabricated MXene-based fibers with protective layers (MGP-T) formed using various draw-down ratios according to various embodiments and polycarbonate (PC).
  • FIG. 39A shows a plot of tensile strength (in mega-Pascals or MPa) as a function of electrical conductivity (in X 10 3 siemens per centimeter or S cm 1 ) comparing the tensile strength and electrical conductivity of the obtained compact MXene-based fibers according to various embodiments with other reported MXene-based fibers.
  • FIG. 39B shows a table comparing the tensile strength (in mega-Pascals or MPa), toughness (in mega-Joules per cubic meter or MJ m -3 ) and electrical conductivity (in siemens per centimeter or S cm 1 ) of the obtained compact MXene-based fibers according to various embodiments with that of other reported MXene-based fibers
  • FIG. 40A shows a plot of toughness (in mega-Joules per cubic meter or MJ m -3 ) as a function of electrical conductivity ((in siemens per centimeter or S cm 1 ) comparing the toughness and electrical conductivity of the ultra-compact MXene fibers according to various embodiments with that for other reported MXene-based fibers, graphene fibers, and carbon nanotube (CNT) fibers.
  • toughness in mega-Joules per cubic meter or MJ m -3
  • electrical conductivity (in siemens per centimeter or S cm 1 )
  • FIG. 40B shows a table comparing the tensile strength (in mega-Pascals or MPa), toughness (in mega-Joules per cubic meter or MJ m -3 ) and electrical conductivity (in siemens per centimeter or S cm 1 ) of the obtained compact MXene-based fibers according to various embodiments with that of other reported carbon -based fibers.
  • FIG. 41 shows (a) a schematic diagram of the apparatus used for the thermal drawing according to various embodiments; and (b) a polycarbonate (PC) hollow tube model with an inner diameter of 0.06 mm, an outer-diameter of 0.08 mm, and a length of 0.50 mm long constructed to study the mechanical behavior of the PC hollow tube via finite element analysis according to various embodiments.
  • PC polycarbonate
  • FIG. 42A shows a simulation of the stress distribution of the polycarbonate (PC) hollow tube model according to various embodiments.
  • FIG. 42B shows plots of stress (in mega-Pascals or MPa) as a function of draw-down ratio illustrating the Y and Z stress curves with the increment of the draw-down ratio according to finite element analysis according to various embodiments.
  • FIG. 43A shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) as a function of frequency (in gigahertz or GHz) illustrating the EMI reflection shielding efficiency (SER), absorption shielding efficiency (SEA) and total efficiency (SET) of the textiles according to various embodiments at the frequencies of 8.2 GHz - 12.4 GHz.
  • EMI SE electromagnetic interference shielding efficiency
  • SER EMI reflection shielding efficiency
  • SEA absorption shielding efficiency
  • SET total efficiency
  • FIG. 43B is a schematic illustrating plain-weaved textiles based on MXene-based fibers according to various embodiments for electromagnetic interference (EMI) measurements.
  • EMI electromagnetic interference
  • FIG. 44A shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) comparing the reflection shielding efficiency (SER), absorption shielding efficiency (SEA) and total efficiency (SET) of textiles fabricated from the MXene-based fibers with protective layers (MGP-T) obtained using various draw-down ratios according to various embodiments at the frequency of 8.2 GHz.
  • EMI SE electromagnetic interference shielding efficiency
  • FIG. 44B shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) as a function of frequency (in gigahertz or GHz) illustrating the electromagnetic interference (EMI) properties of 3 -layered textiles fabricated using various MXene-based fibers with protective layers (MGP-T) according to various embodiments at frequencies from 8.2 GHz to 12.4 GHz.
  • EMI SE electromagnetic interference shielding efficiency
  • FIG. 44C shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) comparing the electromagnetic interference (EMI) properties of 3 -layered textiles fabricated using various fabricated and pure MXene fibers according to various embodiments at the frequency of 8.2 GHz.
  • EMI SE electromagnetic interference shielding efficiency
  • FIG. 45A is a schematic illustrating the electromagnetic interference (EMI) mechanism of textiles fabricated using the MXene-based fibers with protective layers (MGP-T) according to various embodiments.
  • EMI electromagnetic interference
  • FIG. 45B shows a plot of electromagnetic interference shielding efficiency (EMI SE) retention (in percent or %) as a function of number of bending cycles illustrating the electromagnetic interference shielding efficiency retention of the textile according to various embodiments after 5 X 10 4 bending cycles.
  • EMI SE electromagnetic interference shielding efficiency
  • FIG. 46A shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating the temperature-time curves of single MXene-based fibers with protective layers (MGP-T) according to various embodiments when a direct current (DC) voltage of 6 V is applied.
  • MGP-T protective layers
  • FIG. 46B shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating the temperature-time curves of a MXene-based fiber with protective layer (MGP-T) according to various embodiments when voltages from 2 V to 8 V are applied.
  • MGP-T protective layer
  • FIG. 46C shows a plot of performance retention (in percent or %) as a function of the number of cycles illustrating the cycling life of a MXene-based fiber with protective layer (MGP-T) according to various embodiments, while the inset is a plot of temperature (in degrees Celsius or °C) as a function of time (in seconds or s) illustrating the temperature variation profile in the first and last few cycles according to various embodiments.
  • MGP-T MXene-based fiber with protective layer
  • FIG. 46D shows images of various MXene-based fibers with protective layers (MGP-T) arranged in shapes of different letters upon application of various direct current (DC) voltages of 2 V to 8 V according to various embodiments.
  • MGP-T protective layers
  • FIG. 46E shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating temperature-time curves of a single MXene-based fiber with protective layer (MGP-T) according to various embodiments at the bending angles from 0° to 180°.
  • MGP-T protective layer
  • FIG. 46F shows a plot of performance retention (in percent or %) as a function of diameter (in millimeters or mm) illustrating the temperature performance retention of the knots of MXene- based fibers with protective layers (MGP-T) according to various embodiments.
  • FIG. 46G shows a plot of performance retention (in percent or %) as a function of the number of bending cycles illustrating the temperature performance retention of a single MXene-based fiber with protective layer (MGP-T) according to various embodiments after l.lxlO 5 bending cycles from the bending angles of 0° to 180°.
  • FIG. 47A shows a line drawing of the piece of cotton cloth with the size of 0.6 m by 2.0 m woven by 18 meter- long ultra-compact MXene -based fibers with protective layers (MGP-T) according to various embodiments.
  • FIG. 47B shows an enlarged line drawing of a portion of the cloth shown in FIG. 47A according to various embodiments.
  • FIG. 47C shows a line drawing of designed patterns woven into the cotton cloth according to various embodiments; and (inset) the cloth according to various embodiments being subjected to complex deformation.
  • FIG. 47D shows a line drawing of a sweater woven with several MXene-based fibers with protective layers (MGP-T) according to various embodiments to generate heat.
  • FIG. 47E shows a thermal image of the sweater in FIG. 47D according to various embodiments when a potential difference of 2 V is applied.
  • FIG. 47F shows a thermal image of the sweater in FIG. 47D according to various embodiments when a potential difference of 4 V is applied.
  • FIG. 47G shows an enlarged line drawing of a portion of the sweater shown in FIG. 47D according to various embodiments.
  • the term “about” or “approximately” as applied to a numeric value encompasses the exact value and a reasonable variance, e.g. within 10% of the specified value.
  • Various embodiments may seek to meet the abovementioned requirements. Various embodiments may seek to address the abovementioned issues/shortcomings facing current fibers. Various embodiments may seek to address issues facing fibers without protective layers. Various embodiments may relate to a continuous and controllable route to fabricate ultracompact MXene-based fibers.
  • FIG. 1 shows a schematic of a method of forming a fiber according to various embodiments.
  • the method may include, in 102, forming a wet spun fiber from a plurality of
  • the method may also include, in 104, forming the fiber by heating the wet spun fiber using a thermal drawing process.
  • the fiber may be a crosslinked MXene-based fiber including a MXene core including the plurality of MXene sheets which are cross-linked.
  • the fiber may further include a protective layer surrounding the MXene core.
  • the method may include wet-spinning MXene sheets into a wet-spun fiber, and subjecting the wet spun fiber to a thermal drawing process.
  • the resultant fiber may have a MXene core, and a protective layer covering the circumferential surface of the core.
  • the MXene core may include the plurality of cross-linked MXene sheets.
  • MXene-based fibers or cross-linked MXene based fibers having the MXene cores and the protective layers surrounding the MXene cores
  • MGP-T fibers the wet spun fibers prior to the thermal drawing process
  • wet spun MXene fibers may be referred to as MGP fibers.
  • a MXene sheet may include a sheet including a MXene material.
  • a MXene core/fiber may be a core/fiber including a MXene material.
  • MXene sheets or fibers/cores may include transition metal carbides, nitrides or carbonitrides.
  • the MXene sheets may be TisC2T x sheets, wherein Ti is titanium, C is carbon, T is a functional group (e.g. -OH, -O, or -F) and x is any number.
  • the MXene fibers/cores may be or include TisC2T x .
  • the TisC2T x sheets may be formed from TisAlC2.
  • the MXene sheets or fibers/cores may, for instance, be V2CT X , wherein V is vanadium, C is carbon, T is a functional group and x is any number.
  • the MXene sheets or fibers/cores may, for instance, be Nb2CT x , wherein Nb is niobium, C is carbon, T is a functional group and x is any number.
  • the one or more MXene sheets may be nanosheets.
  • the MXene sheets may have a thickness of a few atoms.
  • forming the wet spun fiber from the plurality of MXene sheets may include forming an intermediate fiber by extruding a spinning dispersion including the plurality of MXene sheets into a coagulant bath. Forming the wet spun fiber from the plurality of MXene sheets may also include forming the wet spun fiber by passing the intermediate fiber through a cross-linking solution.
  • the intermediate fiber, the wet spun fiber and/or the fiber including the MXene core and the protective layer may be nanofibers.
  • the MXene core may include a plurality of cross-linked sheets, e.g. nanosheets.
  • cross-linked MXene sheets or the term “the plurality of MXene sheets which are cross-linked” may refer to the plurality of MXene sheets of the MXene core, in which each MXene sheet of the MXene core is cross-linked to one or more other MXene sheets of the MXene core.
  • cross-linked MXene nanosheets or the term “the plurality of MXene nanosheets which are cross-linked” may refer to the plurality of MXene nanosheets of the MXene core, in which each MXene nanosheet of the MXene core is cross-linked with one or more other MXene nanosheets of the MXene core.
  • there may be cross-linking between fibers For instance, in situations such as when the fibers are in wet condition, there may also be crosslinking between the fibers in addition to cross-linking between sheets of each fiber.
  • Various embodiments may relate to a plurality of fibers (i.e.
  • the spinning dispersion may include glutaraldehyde (GA).
  • the intermediate fiber formed may be a cross-linked MXene- glutaraldehyde (GA) fiber.
  • GA may function as a cross-linker.
  • GA may form covalent bonds (titanium-oxygen-carbon or Ti-O-C bonds) between different sheets or nanosheets of an intermediate fiber, a wet spun fiber, or a fiber including the protective layer.
  • the GA molecules may form the covalent bond(s) via a nucleophilic substitution and dehydration reaction.
  • the spinning dispersion may include nanocrystalline cellulose such that the intermediate fiber formed is a cross-linked MXene-nanocrystalline cellulose fiber.
  • nanocrystalline cellulose may function as a cross -linker.
  • the cross-linking solution may include polyvinyl alcohol (PVA).
  • PVA may form hydrogen bonds between different sheets or nanosheets of a wet spun fiber, or a fiber including the protective layer.
  • the wet spun fiber formed may be a cross-linked MXene- glutaraldehyde (GA) - polyvinyl alcohol (PVA) fiber.
  • G cross-linked MXene- glutaraldehyde
  • PVA polyvinyl alcohol
  • the cross-linking solution may include chitosan or sodium alginate.
  • the coagulant bath may include ammonium ions.
  • the method may further include passing the intermediate fiber through a first washing bath before forming the wet spun fiber. In various embodiments, the method may also include passing the wet spun fiber through a second washing bath before forming the cross-linked MXene-based fiber. The first washing bath and the second washing bath may include deionized water.
  • the intermediate fibers may be referred to as MG fibers.
  • the protective layer may be a polymer layer.
  • the protective layer may include polycarbonate, cyclo olefin polymer (COP), chlorinated polyethylene (CPE), polyethylene (PE), or polyetherimide (PEI).
  • the protective layer may cover a circumferential surface of the MXene core. In various embodiments, the protective layer may also cover end surfaces of the MXene core.
  • the cross-linked MXene-based fiber may have a tensile strength selected from a range of between about 350 MPa and about 600 MPa, e.g. between about 372.5 MPa and about 585.5 MPa. In various embodiments, the cross-linked MXene-based fiber may have a tensile strength selected from a range of between 350 MPa and 600 MPa, e.g. between 372.5 MPa and 585.5 MPa.
  • the cross-linked MXene-based fiber may have a toughness selected from a range of between about 60 MJ m -3 and about 80 MJ m -3 , e.g. between about 66.7 MJ m -3 and about 77.9 MJ m -3 .
  • the cross-linked MXene-based fiber may have a toughness selected from a range of between 60 MJ m -3 and 80 MJ m -3 , e.g. between 66.7 MJ m -3 and 77.9 MJ m -3 .
  • the cross-linked MXene-based fiber may have an electrical conductivity selected from a range of between about 8,000 S cm 1 and about 9,000 S cm 1 , e.g. between about 8,344.5 cm 1 and about 8,802.4 S cm 1 . In various embodiments, the cross-linked MXene-based fiber may have an electrical conductivity selected from a range of between 8,000 S cm 1 and 9,000 S cm 1 , between 8,344.5 cm 1 and 8,802.4 S cm 1 .
  • the thermal drawing process may include feeding the wet spun fiber into a tube passing through a furnace.
  • the furnace may have a hot zone having a temperature of about 200 °C, e.g. 200 °C.
  • a ratio of pull to feed speed of the thermal drawing process may be of any value selected from a range of between about 1.2 and about 1.5, e.g. about 1.26, about 1.34 and about 1.41. In various embodiments, a ratio of pull to feed speed of the thermal drawing process may be of any value selected from a range of between 1.2 and 1.5, e.g. 1.26, 1.34 and 1.41.
  • the cross-linked MXene-based fiber may show a porosity selected from a range of between about 5.5 % to about 9 %, between about 5.7% to about 8.6%.
  • the cross-linked MXene-based fiber may show a porosity selected from a range of between 5.5 % to 9 %, between 5.7% to 8.6%.
  • the cross-linked MXene-based fiber may show an orientation order selected from a range of between about 0.8 to about 0.9, e.g. between about 0.84 to about 0.89.
  • the cross-linked MXene-based fiber may show an orientation order selected from a range of between 0.8 to 0.9, e.g. between 0.84 to 0.89.
  • the cross-linked MXene-based fiber may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 40 dB to about 55 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 42 dB to about 51 dB (e.g. at about 8.2GHz). In various embodiments, the cross-linked MXene-based fiber may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between 40 dB to 55 dB, e.g. a range of between 42 dB to 51 dB.
  • EMI absorption electromagnetic interference
  • the cross-linked MXene-based fiber may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 50 dB to about 65 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 52 dB to about 61 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between 50 dB to 65 dB, e.g. a range of between 52 dB to 61 dB.
  • SE total electromagnetic interference
  • the cross-linked MXene-based fiber including the protective layer may be configured to reach an equilibrium temperature selected from a range of between about 90 °C to about 100 °C within about 300 s upon applying a direct current (DC) voltage of about 6 V. In various embodiments, the cross-linked MXene-based fiber including the protective layer may be configured to reach an equilibrium temperature selected from a range of between 90 °C to 100 °C within 300 s upon applying a direct current (DC) voltage of 6V.
  • DC direct current
  • Various embodiments may relate to a fiber formed by a method as described herein.
  • Various embodiments may relate to a fiber formed by a method including forming a wet spun fiber from a plurality of MXene sheets using a wet spinning process, and forming the fiber by heating the wet spun fiber using a thermal drawing process.
  • the fiber may be a cross-linked MXene-based fiber including a MXene core including the plurality of MXene sheets which are cross-linked.
  • the fiber may further include a protective layer surrounding the MXene core.
  • Various embodiments may relate to a method of forming one or more fibers.
  • the method may include forming one or more wet spun fibers, each of the one or more wet spun fibers from a plurality of MXene sheets, using a wet spinning process.
  • the method may also include forming one or more fibers by heating the one or more wet spun fibers using a thermal drawing process.
  • the one or more fibers may be cross-linked MXene-based fibers, each of the one or more fibers including a MXene core including the plurality of MXene sheets which are cross-linked.
  • the fiber may further include a protective layer surrounding the MXene core(s).
  • various embodiments may relate to a method of forming a fiber bundle containing a plurality of fibers.
  • the method may include forming a plurality of wet spun fibers, each of the plurality of wet spun fibers from a plurality of MXene sheets, using a wet spinning process.
  • the method may also include forming the fiber bundle containing the plurality of fibers by heating the plurality of wet spun fibers using a thermal drawing process.
  • the plurality of fibers may be cross-linked MXene-based fibers, each of the plurality of fibers including a MXene core including the plurality of MXene sheets which are cross -linked.
  • the fiber bundle may further include a protective layer surrounding the plurality of fibers or the MXene cores.
  • FIG. 2 shows a schematic of a fiber 202 according to various embodiments.
  • the 202 may include a MXene core 204.
  • the fiber 202 may also include a protective layer 206 surrounding the MXene core 204.
  • the fiber 202 may be a cross-linked MXene-based fiber such that the MXene core includes a plurality of MXene sheets which are cross-linked.
  • various embodiments may relate to a cross-linked MXene-based fiber including a MXene core which has multiple cross-linked sheets.
  • the cross-linked MXene-based fiber may also have a protective layer covering the circumferential surface of the MXene core.
  • FIG. 2 is intended to illustrate some features according to some embodiments, and is not intended to limit, for instance, the dimensions, aspect ratios, arrangement, orientation etc. of the fibers.
  • the fiber 202 may be a cross -linked MXene- glutaraldehyde (GA) - polyvinyl alcohol (PVA) fiber.
  • GA MXene- glutaraldehyde
  • PVA polyvinyl alcohol
  • the sheets or nanosheets of the MXene core 204 may alternatively be cross-linked by nanocrystalline cellulose.
  • PVA polyvinyl alcohol
  • the sheets or nanosheets of the MXene core 204 may alternatively be cross-linked by chitosan or sodium alginate.
  • the protective layer 206 may be a polymer layer.
  • the protective layer may be a polymer layer.
  • the protective layer may include polycarbonate, cyclo olefin polymer (COP), chlorinated polyethylene (CPE), polyethylene (PE), or poly etherimide (PEI).
  • COP cyclo olefin polymer
  • CPE chlorinated polyethylene
  • PE polyethylene
  • PEI poly etherimide
  • the cross-linked MXene-based fiber 202 may have a tensile strength selected from a range of between about 350 MPa and about 600 MPa, e.g. between about 372.5 MPa and about 585.5 MPa. In various embodiments, the cross-linked MXene-based fiber 202 may have a tensile strength selected from a range of between 350 MPa and 600 MPa, e.g. between 372.5 MPa and 585.5 MPa.
  • the cross-linked MXene-based fiber 202 may have a toughness selected from a range of between about 60 MJ m -3 and about 80 MJ m -3 , e.g. between about 66.7 MJ m -3 and about 77.9 MJ m -3 .
  • the cross-linked MXene- based fiber 202 may have a toughness selected from a range of between 60 MJ m -3 and 80 MJ m -3 , e.g. between 66.7 MJ m -3 and 77.9 MJ m -3 .
  • the cross-linked MXene-based fiber 202 may have an electrical conductivity selected from a range of between about 8,000 S cm 1 and about 9,000 S cm 1 , between about 8,344.5 cm 1 and about 8,802.4 S cm 1 . In various embodiments, the crosslinked MXene-based fiber 202 may have an electrical conductivity selected from a range of between 8,000 S cm 1 and 9,000 S cm 1 , between 8,344.5 cm 1 and 8,802.4 S cm 1 .
  • the cross-linked MXene-based fiber 202 may show a porosity selected from a range of between about 5.5 % to about 9 %, between about 5.7% to about 8.6%. In various embodiments, the cross-linked MXene-based fiber 202 may show a porosity selected from a range of between 5.5 % to 9 %, between 5.7% to 8.6%.
  • the cross-linked MXene-based fiber 202 may show an orientation order selected from a range of between about 0.8 to about 0.9, e.g. between about 0.84 to about 0.89. In various embodiments, the cross-linked MXene-based fiber 202 may show an orientation order selected from a range of between 0.8 to 0.9, e.g. between 0.84 to 0.89.
  • the cross-linked MXene-based fiber 202 may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 40 dB to about 55 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber 202 may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 42 dB to about 51 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber 202 may show an absorption electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between 40 dB to 55 dB, e.g. selected from a range of between 42 dB to 51 dB.
  • EMI absorption electromagnetic interference
  • SE absorption electromagnetic interference
  • the cross-linked MXene-based fiber 202 may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 50 dB to about 65 dB (e.g. at about 8.2 GHz). In various embodiments, the cross-linked MXene-based fiber 202 may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between about 52 dB to about 61 dB (e.g. at about 8.2 GHz).
  • EMI electromagnetic interference
  • SE total electromagnetic interference
  • the cross-linked MXene-based fiber 202 may show a total electromagnetic interference (EMI) shielding efficiency (SE) selected from a range of between 50 dB to 65 dB, a range of between 52 dB to 61 dB.
  • EMI electromagnetic interference
  • SE shielding efficiency
  • the cross-linked MXene-based fiber 202 including the protective layer may be configured to reach an equilibrium temperature selected from a range of between about 90 °C to about 100 °C within about 300 s upon applying a direct current (DC) voltage of about 6 V.
  • the cross-linked MXene-based fiber 202 including the protective layer may be configured to reach an equilibrium temperature selected from a range of between 90 °C to 100 °C within 300 s upon applying a direct current (DC) voltage of 6 V.
  • Various embodiments may relate to an object including one or more fibers as described herein.
  • the object may, for instance, be a textile cloth, an electromagnetic shield or a clothing such as a sweater.
  • Various embodiments may relate to one or more fibers, each of the one or more fibers including a MXene core.
  • the one or more fibers may also include a protective layer surrounding the MXene core(s).
  • Each of the one or more fibers may be a cross-linked MXene-based fiber such that the MXene core includes a plurality of MXene sheets which are cross-linked.
  • various embodiments may relate to a fiber bundle containing a plurality of fibers, each of the plurality of fibers include a MXene core.
  • the fiber bundle may include a protective layer surrounding the MXene cores or the plurality of fibers.
  • Each of the plurality of fibers may be a cross-linked MXene-based fiber such that the MXene core includes a plurality of MXene sheets which are cross-linked.
  • Various embodiments may relate to a continuous and controllable route to fabricate ultra-compact MXene fibers. To start, interfacial interactions in the wet spinning may enable the transfer from MXene nanosheets to compact MXene fibers. Then, these fibers may continuously be fed into a polymer tube in thermal drawing, resulting in (1) ultra-compact MXene fibers due to the drawing-induced stresses, and (2) in-situ generated protective layer.
  • the resulting ultra-compact MXene fibers with protective layers may not only offer remarkable tensile strength of -585.5 MPa and ultra-high toughness of -66.7 MJ m -3 , but may also exhibit high electrical conductivity of -8,802.4 S cm 1 and excellent long-term mechanical durability and stability.
  • Two representative applications based on large-scale MXene textiles fabricated using these fibers are also explored herein.
  • One relates to electromagnetic interference shielding with high shielding efficiency of -57 dB and -87.8% retention of performance after 5xl0 4 bending cycles.
  • the other one relates to electrothermal effect with the demonstration of a sweater generating heat, with temperatures reaching -35 °C— 70 °C.
  • the demonstrated synergy of interfacial interactions and thermal drawing-induced stresses may attract interests for other applications of the compact MXene-based fibers.
  • the flexible MXene fibers with high compactness may be fabricated by a continuous and controllable synergy of wet spinning with interfacial interactions and thermal drawing - induced stresses, as schematically illustrated in FIG. 3A.
  • FIG. 3A is a schematic illustrating the fabrication of ultra-compact MXene-based fibers with the protective layer (MGP-T) via continuous wet spinning and thermal drawing, and the formation of MXene-based textiles according to various embodiments.
  • Large-area multi-functional fabrics can be constructed by the resulting fibers for applications in electromagnetic interference (EMI) shielding and thermal management based on electrothermal (ET) effect.
  • EMI electromagnetic interference
  • ET electrothermal
  • the resulting wet spun MXene fibers may achieve increased orientation orders (f) from -0.82 to -0.87, and low porosity due to synergistic interfacial interactions. This may result in the enhancement of the tensile strength from -167.1 MPa to -565.2 MPa with increase in toughness from -0.4 MJ m -3 to -19.2 MJ m -3 .
  • FIG. 1 A perspective view of the tensile strength from -167.1 MPa to -565.2 MPa with increase in toughness from -0.4 MJ m -3 to -19.2 MJ m -3 .
  • FIG. 3B shows (top left) scanning electron microscopy (SEM) images of pure MXene fibers (normal and zoomed in) according to various embodiments; (top right) a wide-angle X-ray scattering (WAXS) pattern of the pure MXene fibers according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stressstrain curve of the pure MXene fibers according to various embodiments.
  • SEM scanning electron microscopy
  • WAXS wide-angle X-ray scattering
  • 3C shows (top left) a scanning electron microscopy (SEM) images of resulting wet spun MXene fibers (MGP) (normal and zoomed in) according to various embodiments; (top right) a wide-angle X-ray scattering (WAXS) pattern of the resulting wet spun MXene fibers (MGP) according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stress-strain curve of the resulting wet spun MXene fibers (MGP) according to various embodiments.
  • SEM scanning electron microscopy
  • the ultra-compact MXene -based fibers with protective layer may be obtained with the significantly promoted orientation orders (/) of -0.90, accompanied by the further reduction of the porosity.
  • the obtained MGP-T fibers with the protective layer may offer the highest strength of -585.5 MPa and toughness of - 66.7 MJ m -3 , thanks to the enhancement of alignment and reduction of voids.
  • 3D shows (top left) a scanning electron microscopy (SEM) images of resulting MXene-based fibers with protective layers (MGP-T) (normal and zoomed in) according to various embodiments; (top right) a wide- angle X-ray scattering (WAXS) pattern of the resulting fibers with protective layers (MGP-T) according to various embodiments; and (below) a plot of the stress (in mega Pascals or MPa) as a function of strain (in percent or %) showing the stress-strain curve of the resulting fibers with protective layers (MGP-T)) according to various embodiments.
  • SEM scanning electron microscopy
  • MXene (TisC2T ) nanosheets may be prepared by etching and shaking from preliminary titanium aluminum carbide (TisAlC2) and accordion-like MXene.
  • FIG. 4A shows a scanning electron microscopy (SEM) image of titanium aluminum carbide (TisAlC2) according to various embodiments.
  • FIG. 4B shows a scanning electron microscopy (SEM) image of accordion-like MXene according to various embodiments.
  • the obtained MXene nanosheets have a lateral size of ⁇ 10 pm with a thickness of ⁇ 1.5 nm according to the scanning electron microscopy (SEM) and atomic force microscopy (AFM) images.
  • FIG. 5A shows a scanning electron microscopy (SEM) image of exfoliated MXene nanosheets with a lateral size of about 10 pm according to various embodiments.
  • FIG. 5B shows a plot of count as a function of lateral size (in micrometers or pm) illustrating the size distribution for the exfoliated MXene nanosheets shown in FIG. 5A according to various embodiments.
  • FIG. 5C shows an atomic force microscopy (AFM) image of exfoliated MXene nanosheets with a thickness of about 10 pm according to various embodiments.
  • FIG. 5D shows a plot of height (in nanometers or nm) as a function of lateral size (in micrometers or pm) illustrating the thickness of the exfoliated MXene nanosheets shown in FIG. 5C according to various embodiments.
  • the exfoliated MXene nanosheets may have the expected high crystallinity hexagonal structures without defects, confirmed by the high-resolution transmission electron microscopy (HR-TEM) images and the selected area electron diffraction patterns.
  • FIG. 6A shows a transmission electron microscopy (TEM) image of exfoliated MXene nanosheets according to various embodiments.
  • FIG. 6B shows the corresponding high- resolution transmission electron microscopy (HR-TEM) image of the exfoliated MXene nanosheets; and (inset) selected area electron diffraction (SAED) pattern of the exfoliated MXene nanosheets according to various embodiments.
  • the SAED patterns indicates hexagonal single crystals structure without obvious defects.
  • FIG. 7 is a plot of intensity (in arbitrary units or a.u.) as a function of angle (29) showing the X-ray diffraction (XRD) patterns of primitive titanium aluminum carbide (TEAICT) and exfoliated MXene (Ti 3 C2T ) nano sheets according to various embodiments.
  • the X-ray diffraction (XRD) patterns of exfoliated MXene (Ti 3 C 3 T ) nanosheets do not show the 104 and 105 peaks characteristics of TEAIC2, demonstrating the complete etching of the aluminum (Al) layer and indicating that the MXene nanosheets have been successfully prepared from Ti 3 AlC2.
  • the disappearance of the (002) and (004) peaks of Ti 3 AlC2 and a new peak at the 29 of ⁇ 6° may also indicate that the MXene nanosheets were successfully fabricated from the Ti 3 AlC 2 .
  • MXene nanosheets in the MXene-glutaraldehyde (GA) spinning dispersion may present lyotropic liquid-crystalline properties in the range of ⁇ 15 mg ml? to ⁇ 30 mg mL 1 .
  • FIG. 8 show polarizing optical microscope (POM) images of MXene-glutaraldehyde (GA) spinning dispersion with concentrations from ⁇ 5 mg mL 1 to ⁇ 30 mg mL 1 according to various embodiments. As shown in FIG. 8, optical birefringence may be observed in concentrations of ⁇ 15 mg mL 1 to ⁇ 30 mg mL 1 . This may indicate the formation of liquid-crystalline phase as a result of the local orientation without aggregation.
  • POM polarizing optical microscope
  • FIG. 9A shows a plot of viscosity (in Pascals seconds or Pa.s) as a function of shear rate (in per second or 1/s) illustrating the variation of viscosity with shear rate of different concentrations of the spinning dispersion according to various embodiments. Similar to most complex fluid systems with rigid polymer chains, the viscosity of MXene nanosheets in spinning dispersions may decrease with an increasing shear rate, and may increase with an increasing concentration.
  • FIG. 9B shows a plot of shear stress (in Pascals or Pa) as a function of shear rate (in per second or 1/s) illustrating the variation of shear stress with shear rate of different concentrations of the spinning dispersion according to various embodiments.
  • the shear stress of the spinning dispersion may decrease sharply at the initial stage and may then gradually increase with the shear rate. It suggests that the randomly oriented MXene nanosheets may turn into an ordered state because of the shear-induced deformation.
  • FIG. 9C shows a plot of modulus (in Pascals or Pa) as a function of frequency (in per second or 1/s) illustrating the variation of modulus with frequency of different concentrations of the spinning dispersion according to various embodiments.
  • the ratio of the storage modulus to the loss modulus (G7G”) of a spinning dispersion may be in the range from about 1.86 to about 6.01 with the concentration of about 30 mg mL 1 to about 15 mg mL 1 , acting as an indicator for the spinnability of liquid-crystalline MXene nanosheets colloidal dispersions.
  • MXene nanosheets may initially crosslink with GA at a concentration of 30 mg mL 1 to form MXene-GA (MG) fibers, and sequentially crosslinked with polyvinyl alcohol (PVA) to fabricate several meters long MXene-GA-PVA (MGP) fibers with a diameter of ⁇ 60 pm by wet spinning.
  • FIG. 10A shows a line drawing of several meter long wet spun (MGP) fibers according to various embodiments; and (inset) a magnified line drawing showing the axial SEM morphology of a wet spun (MGP) fiber according to various embodiments.
  • FIG. 10B shows a plot of intensity (in arbitrary units or a.u.) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the obtained fibers according to various embodiments, glutaraldehyde (GA), polyvinyl alcohol (PVA) and pure MXene.
  • G glutaraldehyde
  • PVA polyvinyl alcohol
  • FIG. 10C shows a plot of reflectance (in percent or %) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the obtained fibers according to various embodiments, glutaraldehyde (GA), polyvinyl alcohol (PVA) and pure MXene.
  • FIG. 10D shows a plot of reflectance (in percent or %) as a function of wavenumbers (per centimeter or cm 1 ) showing the Fourier transform infrared (FTIR) spectra of the wet spun (MGP) fibers with different weight ratios of polyvinyl alcohol (PVA) according to various embodiments.
  • FTIR Fourier transform infrared
  • FIG. 11 shows a plot of intensity (in arbitrary units or a.u.) as a function of wavenumbers (per centimeter or cm 1 ) showing the X-ray photoelectron spectroscopy (XPS) spectra of the fabricated fibers according to various embodiments, pure MXene and MAX (TisAKZy. The peaks for Ti and the disappeared Al peak may indicate that MXene nanosheets have been successfully etched from the primitive MAX (TisAlC2). [0072] FIG.
  • FIG. 12A shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron volts or eV) showing the titanium (Ti) 2p spectra of the fabricated fibers according to various embodiments and pure MXene fibers.
  • FIG. 12B shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron volts or eV) showing the oxygen (O) Is spectra of the fabricated fibers according to various embodiments and pure MXene fibers.
  • FIG. 12A shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron volts or eV) showing the titanium (Ti) 2p spectra of the fabricated fibers according to various embodiments and pure MXene fibers.
  • FIG. 12B shows a plot of intensity (in arbitrary units or a.u.) as a function of binding energy (in electron
  • 12C shows a table illustrating the atomic percentage of O-Ti-O, C-Ti-OX, O-C, and C-Ti-OH according to the oxygen (O) Is peak in the obtained X-ray photoelectron spectroscopy (XPS) spectra of the obtained fibers according to various embodiments and pure MXene fibers.
  • O oxygen
  • XPS X-ray photoelectron spectroscopy
  • a new peak at -456.4 eV for MGP and MG fibers indicates the formation of Ti-O-C between MXene nanosheets and GA compared with pure MXene fibers according to Ti 2p spectra.
  • the atomic percentage for O-C for MG and MGP fibers is increased to 16.4% and 22.0%, compared to pure MXene fibers of 6.2% in O Is spectra, indicating the formation of Ti-O-C bond between MXene nanosheets and GA, and hydrogen bonding between MXene nanosheets and PVA.
  • compact MXene fibers may be fabricated via interfacial interactions, which are firstly crosslinked with GA via Ti-O-C bond of nucleophilic substitution (FIG. 13A), and then crosslinked with PVA via hydrogen bonding between MXene nanosheets and PVA (FIG. 13B)
  • FIG. 13A illustrates one possible mechanism for the formation of Ti-O-C covalent bond between MXene nanosheets and glutaraldehyde molecules according to various embodiments.
  • the aldehyde group (-CHO) of glutaraldehyde (GA) molecules may react with hydroxyl functional group (OH) of a MXene nanosheet to form Ti-O-C covalent bond via nucleophilic substitution and dehydration reaction.
  • FIG. 13A(b) shows the corresponding structure schematic of formed Ti-O-C bond between MXene nanosheets and glutaraldehyde molecules.
  • FIG. 13B shows a structure graph of the covalent bond between MXene nanosheets and glutaraldehyde (GA) and the hydrogen bond between MXene nanosheets and polyvinyl alcohol (PVA) according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 14A shows (a) wide- angle X-ray scattering (WAXS) patterns of the fabricated intermediate (MG) fibers with different weight ratios of glutaraldehyde molecules from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments; and (b) small-angle X-ray scattering (SAXS) patterns of the fabricated intermediate (MG) fibers with different weight ratios of glutaraldehyde molecules from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments.
  • WAXS wide- angle X-ray scattering
  • SAXS small-angle X-ray scattering
  • FIG. 14B shows a plot of orientation order (f) as a function of percentage of glutaraldehyde (in weight percent or wt%) showing the variation of the orientation of the intermediate (MG) fibers with different amounts of glutaraldehyde based on wide-angle X-ray scattering (WAXS) patterns according to various embodiments.
  • FIG. 14C shows a plot of density (in grams per cubic centimeter) / porosity (in percent or %) as a function of percentage of glutaraldehyde (in weight percent or wt%) showing the variation of density and porosity of the intermediate (MG) fibers with different amounts of glutaraldehyde according to various embodiments.
  • the results show that MG fibers with 5 wt% glutaraldehyde may have achieved the highest orientation order (f) and the lowest porosity.
  • FIG. 15 shows the wide-angle X-ray scattering (WAXS) and (inset) small-angle X- ray scattering (SAXS) patterns of the fabricated wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 16A shows a plot of orientation order (f) as a function of percentage of polyvinyl alcohol (PVA) (in weight percent or wt%) showing the variation of the orientation of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) based on wide-angle X- ray scattering (WAXS) patterns according to various embodiments.
  • FIG. 16B shows a plot of density (in grams per cubic centimeter) / porosity (in percent or %) as a function of percentage of polyvinyl alcohol (in weight percent or wt%) showing the variation of density and porosity of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 16B shows a plot of density (in grams per cubic centimeter) / porosity (in percent or %) as a function of percentage of polyvinyl alcohol (in weight percent or wt%) showing the variation of density and porosity of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) according to various embodiments.
  • MGP wet spun
  • 16C shows a plot of tensile strength (in mega-Pascals or MPa) / toughness (in mega-Joules or MJ m -3 ) as a function of percentage of polyvinyl alcohol (PVA) (in weight percent or wt%) showing the variation of strength and toughness of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) according to various embodiments.
  • PVA polyvinyl alcohol
  • FIG. 17A shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the intermediate (MG) fibers with different amounts of glutaraldehyde from 0 weight percent (wt%) to 20 weight percent (wt%) according to various embodiments.
  • FIG. 17B shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the wet spun (MGP) fibers with different amounts of polyvinyl alcohol (PVA) from 1 weight percent (wt%) to 15 weight percent (wt%) according to various embodiments.
  • FIG. 17C shows a plot of intensity (in arbitrary units or a.u) as a function of scattering vector q (per Angstrom or A 1 ) illustrating the variation of intensity of the various fabricated fibers according to various embodiments.
  • FIG. 18 shows a plot of weight loss (in percent or %) as a function of temperature (in degrees Celsius or °C) illustrating the thermogravimetric analysis (TGA) results of polyvinyl alcohol (PVA), glutaraldehyde (GA) and various fabricated fibers according to various embodiments.
  • FIG. 19 shows a table illustrating the orientation order (f) and porosity (in percent or %) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • FIG. 20 shows a table illustrating the orientation order (f) and porosity (in percent or %) of the fabricated wet spun (MGP) fibers with different weight percentage of polyvinyl alcohol (PVA) molecules according to various embodiments.
  • FIG. 21 shows a table illustrating the tensile strengths (in megaPascals or MPa), strain (in percent or %) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • the orientation orders (f) of the obtained MG fibers may increase to -0.85 with -5 wt% GA and may decrease to -0.72 with 20 wt% GA compared with the orientation order of -0.82 for pure MXene fibers.
  • the porosity of fibers reduces to 14.1% with -5 wt% GA lower than that of -17.2% for pure MXene fibers. This is because that more GA molecules are hindered in the inter-layer, resulting in the appearing wrinkles and voids according to the increasing intensity of SAXS patterns (FIG. 17A).
  • PVA with more than 5 wt% may lead to the increase of wrinkles of MXene nanosheets and voids between MXene nanosheets, which is testified by the increasing intensity of SAXS patterns for MGP fibers (FIG. 17B). Therefore, the compact MGP fibers may be achieved with low porosity than MG and MXene fibers according the decreased intensity of SAXS patterns (FIG. 17C).
  • FIG. 22A is a plot comparing the tensile strengths and toughness of fabricated intermediate (MG) fibers with different weight percentages of glutaraldehyde molecules from 0 wt% to 20 wt% according to various embodiments.
  • FIG. 22B is a plot comparing the electrical conductivity of fabricated intermediate (MG) fibers with different weight percentages of glutaraldehyde molecules from 0 wt% to 20 wt% according to various embodiments.
  • FIGS. 22A-B show that the MG fibers containing 5 wt% glutaraldehyde molecules may have maximum tensile strengths, toughness, and conductivity.
  • FIG. 23A shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of pure MXene fibers according to various embodiments.
  • FIG. 23B shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 2 weight percent (2 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23A shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 2 weight percent (2 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23C shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 5 weight percent (5 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23D shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 10 weight percent (10 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23E shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 15 weight percent (15 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 23F shows a plot of stress (in mega-Pascals or MPa) as a function of strain
  • the prepared MG fibers Due to the high alignment and low porosity achieved by the interfacial interactions, the prepared MG fibers have a higher tensile strength of -335.6 MPa with the toughness of -4.0 MJ m -3 , compared to that of -167.1 MPa and -0.4 MJ m- 3 for pure MXene fiber via Ti-O-C covalent bond between MXene nanosheets and GA molecules (FIGS. 21, 22A, 23A-F).
  • FIG. 24 shows a table illustrating the electrical conductivity (in siemens per centimeter or S cm 1 ) of the fabricated intermediate (MG) fibers with different weight percentage of glutaraldehyde (GA) molecules according to various embodiments.
  • FIGS. 22B, 24 show that the conductivity of MG fibers decreases from -11,360.4 S cm 1 to -4,536.4 S cm 1 , due to the introduction of non-conductive GA molecules into the MXene nanosheets.
  • MG fibers with 5 wt% GA can still keep a high conductivity of -9,860.6 S cm 1 , because of the high alignment and low porosity of MG fibers.
  • FIG. 25A shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of intermediate (MG) fibers with 5 weight percent (5 wt%) glutaraldehyde molecules according to various embodiments.
  • FIG. 25B shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 1 weight percent (1 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • MGP wet spun
  • PVA polyvinyl alcohol
  • FIG. 25C shows a plot of stress (in mega- Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 2 weight percent (2 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25D shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 5 weight percent (5 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25E shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 10 weight percent (10 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25F shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of wet spun (MGP) fibers with 15 weight percent (15 wt%) polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 25G shows a plot of stress (in mega-Pascals or MPa) as a function of strain (in percent or %) illustrating the stress-strain curves of pure polyvinyl alcohol (PVA) fibers.
  • FIG. 26 shows a table illustrating the tensile strengths (in mega-Pascals or MPa), strain (in percent or %) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of various fibers with different weight percentage of polyvinyl alcohol (PVA) according to various embodiments.
  • the tensile strength and toughness are further enhanced to -565.2 MPa and -19.2 MJ m -3 due to the significant improvement of alignment and decrease of porosity via the synergistic interfacial interactions of the covalent bonds and hydrogen bonds, shown in FIGS. 6C, 25A-G, 26.
  • the mechanical properties of MGP fibers may be weakened by increasing the weight percentage more than -5 wt% PVA due to the hindering effect.
  • FIG. 27 is a plot comparing the electrical conductivity of MXene fibers, intermediate (MG) fibers, and wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 28 shows a table illustrating the electrical conductivity (in siemens per centimeter or S cm 1 ) of intermediate fibers and wet spun (MGP) fibers with different weight percentages of polyvinyl alcohol (PVA) according to various embodiments.
  • FIG. 29 shows scanning electron microcopy images of the cross-sections of intermediate (MG) fibers with different weight percentages (wt%) of polyvinyl alcohol (PVA) from 0 wt% to 20 wt% according to various embodiments.
  • FIG. 30 shows scanning electron microcopy images of the cross-sections of wet spun (MGP) fibers with different weight percentages (wt%) of polyvinyl alcohol (PVA) from 1 wt% to 15 wt% according to various embodiments.
  • FIG. 31A shows a plot of temperature (in degree Celsius or °C) as a function of scattering vector (per Angstrom or A 1 ) illustrating the in-situ X-ray diffraction (XRD) patterns of a wet spun (MGP) fiber according to various embodiments.
  • FIG. 31C shows a plot of intensity (in arbitrary units or a.u.) as a function of scattering vector q (per Angstrom or A 1 ) showing the in-situ X-ray diffraction (XRD) patterns of fabricated wet spun (MGP) fibers being heated under various temperatures from 25 °C to 350 °C according to various embodiments. The results showed the d-spacing between MXene nanosheets was decreased with the increase of heating temperature.
  • the porosity increases sharply from 7.7% to 16.7% when increasing the heating temperature, indicating that the voids and wrinkles between
  • FIG. 3 ID shows a plot of porosity (in percent or %) as a function of temperature (in degree Celsius or °C) illustrated the porosity of wet spun (MGP) fibers being heated according to various embodiments.
  • FIG. 32A shows a schematic diagram of wet spun (MGP) fibers being heated according to various embodiments.
  • FIG. 32B shows the in-situ small-angle X-ray scattering (SAXS) patterns of fabricated wet spun (MGP) fibers (with 5% polyvinyl alcohol (PVA)) being heated under variable temperatures from 25°C to 350 °C according to various embodiments.
  • FIG. 32C shows a plot of intensity as a function of scattering vector q (per Angstrom or A 1 ) illustrating the intensity curves of wet spun fibers under different temperatures based on the small-angle X-ray scattering (SAXS) patterns according to various embodiments.
  • the increasing intensity of SAXS patterns for MGP fibers may confirm the generation of voids and wrinkles of MXene nanosheets when increasing annealing temperature.
  • the voids may mainly be generated via the removal of intercalated water and partial hydroxyl surface terminations at elevated temperatures.
  • thermal drawing enabled physical compression was developed. More importantly, such a continuous drawing process may offer a path to protect the resulting ultra-compact MXene fibers with an in-situ formed polymer layer, resulting in a packaged fiber device to directly engage various applications.
  • a hollow polycarbonate (PC) tube passed through the hot zone of the drawing furnace, while a MGP fiber was continuously fed into the PC tube from the top of it (see FIG.3A).
  • MGP-T cross-linked MXene-based
  • MGP wet spun
  • FIG. 33A shows a schematic diagram of forming the cross-linked MXene-based (MGP-T) fibers with protective layers from wet spun (MGP) fibers with axial stress and perpendicular stress during thermal drawing according to various embodiments.
  • MGP fibers in the PC tube may generate voids and wrinkles when the whole tube entered the hot zone at the central temperature of -200 °C, which was proved by the in-situ XRD and SAXS patterns.
  • the generated voids and wrinkles were significantly reduced by the drawing -induced stresses, including both axial stress and perpendicular stress.
  • FIG. 33B shows a line drawing of several meters long cross-linked MXene-based fibers (MGP-T) fibers with protective layers according to various embodiments.
  • FIG. 33C shows another line drawing of cross-linked MXene-based (MGP-T) fibers with protective layers according to various embodiments.
  • FIG. 34A is a plot comparing the orientation orders (/) of three cross-linked MXene-based (MGP-T) fibers with protective layers fabricated by various draw-down ratios according to various embodiments, with the inset showing the wide-angle X-ray scattering (WAXS) pattern of the various fibers according to various embodiments.
  • WAXS wide-angle X-ray scattering
  • FIG. 34B shows a plot of intensity (in arbitrary units or a.u.) as a function of azimuthal angle (in degrees or °) showing the variation across fibers formed by different draw-down ratios based on wide-angle X-ray scattering (WAXS) patterns according to various embodiments.
  • FIG. 34C shows a table comparing the orientation order (f) and porosity (in percent or %) of the fabricated MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios according to various embodiments.
  • the alignment of MGP fibers may be enhanced from -0.84 to -0.89 when increasing the draw-down ratio, according to the WAXS patterns presented in FIGS. 34A-C.
  • the stress perpendicular to the axis may effectively compress the MGP fibers and reduce the porosity from -8.6% to -5.7% during the thermal drawing.
  • 35A shows a plot of porosity (in percent or %)/conductivity (in X 10 3 siemens per centimeter or S cm 1 ) comparing the porosity and electrical conductivity of the various fabricated MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios according to various embodiments.
  • FIG. 35B shows the scanning electron microscopy (SEM) cross- sectional images of the MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios (a: MGP-Ti, b: MGP-T2, c: MGP-T3) with energy-dispersive X-ray spectroscopy (EDX) according to various embodiments.
  • SEM scanning electron microscopy
  • MGP-T fibers get more compact with the increase of the draw-down ratio from MGP-Ti to MGP-T3, which may significantly reduce the porosity and enhance the alignment of fibers.
  • the EDX mapping of the cross-sections of the MGP-T fibers clearly show that the fibers become more compact with low porosity when increasing the draw-down ratio.
  • FIG. 36A shows a high resolution transmission electron microscopy (HR-TEM) image of a MXene-based fiber with protective layer (MGP-T) according to various embodiments.
  • FIG. 36B shows a zoomed in view of the area indicated in FIG. 36A according to various embodiments. The results showed that the PVA/GA polymers (light color) were successfully introduced into the Tr ⁇ Tv layers (dark color) to form MGP-T fibers with high alignment.
  • FIG. 36C shows the EDX spectrum of the selected area shown in FIG. 36A according to various embodiments. The EDX spectrum suggests the existence of O, C, and Ti element of MXene (Tr ⁇ Tv) nanosheets, PVA, and GA polymers.
  • FIG. 37 shows a table illustrating the electrical conductivity of the fabricated MXene-based fibers with protective layers (MGP-T) formed using various draw-down ratios according to various embodiments.
  • MGP-T fibers may exhibit ultra-high tensile strength of -585.5 MPa and toughness of - 66.7 MJ m -3 due to the promoted alignment and reduction of porosity during the thermal drawing process with increasing stresses.
  • FIG. 38A shows a plot of tensile strength (in mega-Pascals or MPa)/toughness (in mega-Joules per cubic meter or MJ m -3 ) comparing the tensile strength and toughness of the various fabricated MXene-based fibers with protective layers (MGP-T) formed using different draw-down ratios according to various embodiments.
  • MGP-T protective layers
  • 38B shows a table illustrating the tensile strength (in mega-Pascals or MPa) and toughness (in mega-Joules per cubic meter or MJ m -3 ) of the fabricated MXene-based fibers with protective layers (MGP-T) formed using various draw-down ratios according to various embodiments and polycarbonate (PC).
  • FIG. 39A shows a plot of tensile strength (in mega-Pascals or MPa) as a function of electrical conductivity (in X 10 3 siemens per centimeter or S cm 1 ) comparing the tensile strength and electrical conductivity of the obtained compact MXene-based fibers according to various embodiments with other reported MXene-based fibers.
  • FIG. 39A shows a plot of tensile strength (in mega-Pascals or MPa) as a function of electrical conductivity (in X 10 3 siemens per centimeter or S cm 1 ) comparing the tensile strength and electrical conductivity of the obtained compact MXene-based fibers according to various embodiments with other reported MXene-based fibers.
  • 39B shows a table comparing the tensile strength (in mega-Pascals or MPa), toughness (in mega-Joules per cubic meter or MJ m -3 ) and electrical conductivity (in siemens per centimeter or S cm 1 ) of the obtained compact MXene-based fibers according to various embodiments with that of other reported MXene-based fibers.
  • various embodiments may offer the highest performance on both tensile strength and conductivity, compared with the reported MXene fibers without protective layers.
  • the toughness of the ultra-compact MGP-T fibers may reach ⁇ 66.7 MJ m -3 , higher than that of the reported MXene -based fibers, graphene -based fibers, and CNT fibers via different preparation strategies (FIGS. 39B, 40A- B).
  • FIG. 40A shows a plot of toughness (in mega-Joules per cubic meter or MJ m -3 ) as a function of electrical conductivity ((in siemens per centimeter or S cm 1 ) comparing the toughness and electrical conductivity of the ultra-compact MXene fibers according to various embodiments with that for other reported MXene-based fibers, graphene fibers, and carbon nanotube (CNT) fibers.
  • FIG. 40A shows a plot of toughness (in mega-Joules per cubic meter or MJ m -3 ) as a function of electrical conductivity ((in siemens per centimeter or S cm 1 ) comparing the toughness and electrical conductivity of the ultra-compact MXene fibers according to various embodiments with that for other reported MXene-based fibers, graphene fibers, and carbon nanotube (CNT) fibers.
  • 40B shows a table comparing the tensile strength (in mega-Pascals or MPa), toughness (in mega-Joules per cubic meter or MJ m -3 ) and electrical conductivity (in siemens per centimeter or S cm 1 ) of the obtained compact MXene-based fibers according to various embodiments with that of other reported carbon -based fibers.
  • MGP-T fibers with high alignment and low porosity have been achieved, which further enhance their mechanical and electrical properties.
  • finite element analysis was conducted by the Abaqus software.
  • PC hollow tube model with an inner diameter of 0.06 mm, an outer diameter of 0.08 mm, and 0.50 mm long was constructed to study the mechanical behavior of PC hollow tube.
  • FIG. 41 shows (a) a schematic diagram of the apparatus used for the thermal drawing according to various embodiments; and (b) a polycarbonate (PC) hollow tube model with an inner diameter of 0.06 mm, an outer-diameter of 0.08 mm, and a length of 0.50 mm long constructed to study the mechanical behavior of the PC hollow tube via finite element analysis according to various embodiments.
  • PC polycarbonate
  • FIG. 42A shows a simulation of the stress distribution of the polycarbonate (PC) hollow tube model according to various embodiments.
  • the stress parallel to the axial (Y) may be generated accompanied by compressing stress perpendicular to the axial (Z) of PC hollow tube. Therefore, the alignment of inner MGP fibers may be promoted due to axial stress, while the porosity may be reduced because of the perpendicular stress.
  • FIG. 42B shows plots of stress (in mega-Pascals or MPa) as a function of drawdown ratio illustrating the Y and Z stress curves with the increment of the draw-down ratio according to finite element analysis according to various embodiments.
  • the increasing stresses may further enhance the alignment and reduce the porosity, resulting in ultra-compact MGP-T fibers with high mechanical and electrical properties.
  • EMI SE electromagnetic interference shielding efficiency
  • dB electromagnetic interference shielding efficiency
  • SER EMI reflection shielding efficiency
  • SEA absorption shielding efficiency
  • SET total efficiency
  • FIG. 43B is a schematic illustrating plain-weaved textiles based on MXene -based fibers according to various embodiments for electromagnetic interference (EMI) measurements.
  • the as-synthesized MGP and MGP-T fiber textiles show a SET of ⁇ 50 dB and ⁇ 57 dB, compared to that of pure MXene fiber textile ( ⁇ 74 dB) at the frequency of 8.2 GHz, because the electrical conductivity of MGP and MGP-T fibers is lower than that of pure Mxene fibers.
  • the SEA (such as ⁇ 60 dB, ⁇ 47 dB, and ⁇ 40 dB) may be higher than SER ( ⁇ 15 dB, ⁇ 10 dB, and ⁇ 10 dB) for pure MXene, MGP fiber, and MGP-T fiber textiles, respectively. Therefore, the EMI shielding may mainly be dependent on the absorption mechanism.
  • the EMI SE of MGP-T fibers textiles fabricated via increasing draw-down ratios is also summarized in FIGS. 44A-C.
  • FIG. 44A shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) comparing the reflection shielding efficiency (SER), absorption shielding efficiency (SEA) and total efficiency (SET) of textiles fabricated from the MXene-based fibers with protective layers (MGP-T) obtained using various draw-down ratios according to various embodiments at the frequency of 8.2 GHz.
  • EMI SE electromagnetic interference shielding efficiency
  • FIG. 44B shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) as a function of frequency (in gigahertz or GHz) illustrating the electromagnetic interference (EMI) properties of 3 -layered textiles fabricated using various MXene-based fibers with protective layers (MGP-T) according to various embodiments at frequencies from 8.2 GHz to 12.4 GHz.
  • FIG. 44C shows a plot of electromagnetic interference shielding efficiency (EMI SE, in decibels or dB) comparing the electromagnetic interference (EMI) properties of 3 -layered textiles fabricated using various fabricated and pure MXene fibers according to various embodiments at the frequency of 8.2 GHz.
  • the MGP-T fibers textiles may exhibit a higher SEA than SER.
  • the SET of MGP-Ti changes from ⁇ 52 dB to ⁇ 61 dB of MGP-T3, accompanied with an increment of SEA from ⁇ 42 dB to ⁇ 51 dB at the shielding frequency of 8.2 GHz.
  • the increase may be attributed to the reduction of porosity and enhancement of alignment of MGP-T fibers when applying the high draw-down ratio.
  • the MGP-T fibers textiles may show higher SEA and SET, compared with these of MGP fiber textiles, due to the enhanced compactness of fibers during the thermal drawing procedure.
  • FIG. 45A is a schematic illustrating the electromagnetic interference (EMI) mechanism of textiles fabricated using the MXene-based fibers with protective layers (MGP- T) according to various embodiments.
  • EMI electromagnetic interference
  • the EMI shielding mechanism of MGP-T fibers may be explained as follows: when electromagnetic waves (EMWs) strike the surface of an MGP-T fiber, some EMWs may be immediately reflected at the surface because of enormous free electrons of the highly conductive MXene nanosheets. Then, the remaining waves may go through the lattice structure of MXene nanosheets, which interact with the high electron density of MXene nanosheets and induce currents to reduce the energy of the EMWs with the ohmic losses. After going through the first layer (i.e. first nanosheet) of MXene, the surviving EMWs may encounter the next MXene barrier layer with the repetition of EMW attenuation.
  • EMWs electromagnetic waves
  • the second layer i.e. the second nanosheet as the surface reflects the surviving
  • FIG. 45B shows a plot of electromagnetic interference shielding efficiency (EMI SE) retention (in percent or %) as a function of number of bending cycles illustrating the electromagnetic interference shielding efficiency retention of the textile according to various embodiments after 5 X 10 4 bending cycles.
  • EMI SE electromagnetic interference shielding efficiency
  • the obtained MGP-T fibers may also show excellent electrothermal (ET) performance for human thermal management in wearable textiles.
  • FIG. 46A shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating the temperature-time curves of single MXene -based fibers with protective layers (MGP-T) according to various embodiments when a direct current (DC) voltage of 6 V is applied.
  • DC direct current
  • the MGP-T fibers may immediately generate thermal energy and reach the equilibrium temperature from -90 °C to -100 °C (from MGP-Ti to MGP-T3), owing to the mechanism of Joule heat. It may be attributed to the high compactness of MGP-T fibers with the low porosity and high alignment induced by thermal drawing under the high stress.
  • FIG. 46B shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating the temperature-time curves of a MXene-based fiber with protective layer (MGP-T) according to various embodiments when voltages from 2 V to 8 V are applied.
  • FIG. 46B shows that after being applied with different voltages at a broad range of 2 V to 8 V, MGP-T3 fibers can generate the heat with the temperature increasing up to -130 °C, suggesting that the maximum temperature generated by the MGP-T fiber may be tunable by applying various DC voltages.
  • MGP-T fibers may provide excellent ET behavior for their Joule heating.
  • a single MGP-T fiber may also show an excellent cycling life with performance retention of -99% after 5,000 cycles as shown in FIG. 46C.
  • FIG. 46C shows a plot of performance retention (in percent or %) as a function of the number of cycles illustrating the cycling life of a MXene-based fiber with protective layer (MGP-T) according to various embodiments, while the inset is a plot of temperature (in degrees Celsius or °C) as a function of time (in seconds or s) illustrating the temperature variation profile in the first and last few cycles according to various embodiments.
  • FIG. 46D shows images of various MXene-based fibers with protective layers (MGP-T) arranged in shapes of different letters upon application of various direct current (DC) voltages of 2 V to 8 V according to various embodiments.
  • FIG 46D shows that, as an example to achieve the practical applications of MGP-T fibers for thermal management, fabrics with different shapes of the letters based on MGP-T fibers may effectively generate the heat by varying the applied voltages.
  • FIG. 46E shows a plot of temperature (in degree Celsius or °C) as a function of time (in seconds or s) illustrating temperature-time curves of a single MXene-based fiber with protective layer (MGP-T) according to various embodiments at the bending angles from 0° to 180°.
  • MGP-T MXene-based fiber with protective layer
  • FIG. 46F shows a plot of performance retention (in percent or %) as a function of diameter (in millimeters or mm) illustrating the temperature performance retention of the knots of MXene-based fibers with protective layers (MGP-T) according to various embodiments.
  • the performance of ET behavior remained stable evaluated through IR images.
  • the obtained MGP-T fibers could keep the temperature performance retention of -81% after suffering from -l.lxlO 5 bending cycles as shown in FIG. 46G.
  • FIG. 46G shows a plot of performance retention (in percent or %) as a function of diameter (in millimeters or mm) illustrating the temperature performance retention of the knots of MXene-based fibers with protective layers (MGP-T) according to various embodiments.
  • the performance of ET behavior remained stable evaluated through IR images.
  • the obtained MGP-T fibers could keep the temperature performance retention of -81% after suffering from -l.lxlO 5 bending cycles as shown in FIG. 46G.
  • 46G shows a plot of performance retention (in percent or %) as a function of the number of bending cycles illustrating the temperature performance retention of a single MXene-based fiber with protective layer (MGP-T) according to various embodiments after l.lxlO 5 bending cycles from the bending angles of 0° to 180°.
  • FIG. 47 A shows a line drawing of the piece of cotton cloth with the size of 0.6 m by 2.0 m woven by 18 meter-long ultra-compact MXene-based fibers with protective layers (MGP- T) according to various embodiments.
  • FIG. 47B shows an enlarged line drawing of a portion of the cloth shown in FIG. 47A according to various embodiments.
  • FIG. 47C shows a line drawing of designed patterns woven into the cotton cloth according to various embodiments; and (inset) the cloth according to various embodiments being subjected to complex deformation.
  • FIG. 47D shows a line drawing of a sweater woven with several MXene-based fibers with protective layers (MGP-T) according to various embodiments to generate heat.
  • FIG. 47E shows a thermal image of the sweater in FIG. 47D according to various embodiments when a potential difference of 2 V is applied.
  • FIG. 47F shows a thermal image of the sweater in FIG. 47D according to various embodiments when a potential difference of 4V is applied.
  • FIG. 47G shows an enlarged line drawing of a portion of the sweater shown in FIG. 47D according to various embodiments.
  • FIGS. 47D - G show a sweater with several MGP-T fibers that could quickly generate the heat with the temperature of ⁇ 35 °C and ⁇ 70 °C by applying the DC voltages of 2 V and 4 V for wearable human thermal management. Each fiber may be ⁇ 30 cm in length. The obtained results indicate that the ultra-compact MGP-T fibers may be very suitable for constructing smart textiles with excellent ET behavior and remarkable mechanical durability.
  • Various embodiments may relate to an effective and continuous strategy to fabricate ultra-compact MXene fibers with an in-situ generated protective layer. The fibers may be developed via the combination of wet spinning and thermal drawing.
  • MGP-T fibers Due to the interfacial interactions and drawing-induced stresses, the alignment of MGP-T fibers may be significantly enhanced together with the effective reduction of porosity of MXene nanosheets. Consequently, the resulting ultra-compact MGP-T fibers may show excellent mechanical and electrical properties. In addition, the MGP-T fibers may not only offer remarkable electromagnetic interference shielding performance but may also have excellent electrothermal performance with ultra-stable mechanical durability. Meanwhile, the woven textiles based on MGP-T fibers (for large scale applications) may work properly even under complex deformations. These results demonstrate that the strategy may provide an effective means to fabricate compact fibers with multiple functions, paving a way for smart textiles. Various embodiments may generally be applied to the fabrication of other materials to construct the compact fibers with remarkable properties.
  • D3AIC2 powders (particle size ⁇ 400 mesh) were obtained from Jilin 11 Technology Co., Ltd. Lithium fluoride, ammonium chloride, ammonium hydroxide solution (28.0-30.0 wt%), and glutaraldehyde solution (25 wt%) were purchased from Sigma-Aldrich Co., Ltd. Polyvinyl alcohol (PVA) with a molecular weight of MW ⁇ 130,000 was purchased from Sigma- Aldrich. All materials were used as received. PVA solutions used for wet spinning were prepared by dissolving 15 g of PVA powder in 1 L of 95 °C deionized water under vigorous stirring for 12 hours. Polycarbonate (PC) was purchased from Goodfellow Co., Ltd.
  • the solutions with MXene nanosheets were prepared as follows. 1.8 g TisAlC2 powders were added to 40 mL solution (9 M HC1) that contained 3.8 g of lithium fluoride (LiF). Then the solution was stirred at 45 °C for 30 hours. After complete reaction, the accordion-like MXene product was washed with 9 M HC1 solution for three cycles and deionized water for about eight cycles. Each cycle involved 5 minutes of centrifugation at 3500 revolutions per minute (rpm). Until a supernatant solution of MXene nanosheets reached at pH ⁇ 7, the resulting sediments were dispersed into 200 mL deionized water with continuous vibration for 13 minutes.
  • MXene (TisC2T ) nanosheets with different weight percentages of glutaraldehyde solution were used as spinning dispersion.
  • the MXene spinning dispersion was placed in a syringe and extruded through the nozzle with the diameter of 250 pm into the prepared coagulant bath at a velocity of 300 pL min 1 .
  • the coagulant bath included ammonium chloride (12.5 g), ammonium hydroxide solution (5 mL), and deionized water (1 L). After that, the extruded MG fibers in the coagulate bath solution were transferred to a washing bath of deionized water, PVA solutions, and another washing bath of deionized water by rollers.
  • the MG fibers were prepared via adjusting the weight ratios of MXene nanosheets and glutaraldehyde. Furthermore, the MGP fibers with different weight of PVA were obtained by adjusting the rates of roller. Pure PVA fibers were prepared by the same wet spinning with the coagulant of acetone.
  • the PC hollow column was prepared via the wrapped PC on the ceramic rod with the diameter of -6.35 mm and stored in the vacuum oven at 160 °C for 2 hours. Then the compactness MXene-based fibers were fabricated by the thermal drawing process via placing the preform in a two-zone heating furnace, where the top and bottom zones were heated to 150 °C and 350 °C, respectively. The perform with PC hollow column was fed into the furnace with various draw-down ratio (r) when the MGP fibers were fed into the top of hollow column. Finally, the ultra-compact fibers were collected labeled as MGP-T.
  • the rheological behaviors of the MXene- glutaraldehyde spinning dispersions were investigated with a rheometer (Anton Paar MCR 501) under both steady shear and dynamic oscillatory conditions.
  • the viscoelastic properties of the spinning dispersions were measured by measuring the storage and loss modulus as a function of frequency from 0.1 to 100 rad s’ 1 .
  • the strain amplitude remained at 0.1% with a gap of 1 mm at 25 °C for the frequency sweep.
  • Polarized optical microscopy (POM) images were recorded to exhibit optical birefringence via Olympus BX51.
  • FTIR spectra were recorded at room temperature with Diamond ATR by an FTIR Frontier from PerkinElmer.
  • XPS spectra were obtained using an XPS Kratos AXIS Supra. Electrical conductivities were tested using a standard two-probe method with a Keithley 2700 source meter. WAXS/SAXS measurements were conducted on a SWAXS Xenocs Nanoinxider, which was equipped with a Cu-Ka source (operated at 30 W) with a beam diameter of 200 to 800 mm on SAXS (200 K) and WAXS (100 K) detectors. In- situ XRD variable temperature tests were also conducted with the Linkam temperature stage by a SWAXS Xenocs Nanoinxider.
  • the cross-section morphology of MGPT fibers was obtained by Focused Ion Beam (FIB) with the equipment of ZEISS Crossbeam 540 FIB-SEM. Tensile stress-strain curves were measured on 20 mm long, 3 mm wide samples using a SUNS EUT4103X Tester at a loading rate of 0.3 mm min’ 1 with a 10 N sensor at room temperature. The area of fibers was measured by SEM. The results for each fiber were evaluated from the average value of at least three samples.
  • FIB Focused Ion Beam
  • the finite element model was conducted by the commercial software Abaqus 2019 with Abaqus/explicit. During the thermal drawing, the PC tube did not contact the MGP fibers at hot zone at the central temperature of -200 °C. Instead, the MGP fiber contacted the PC tube at a temperature of -160 °C in the drawing furnace according to the experiments.
  • the compressed mechanical behavior of PC hollow tube was the focus of research when the PC hollow tube and MGP fiber came into contact until passing through the drawing furnace at the temperature of 160 °C.
  • the PC hollow tube model due to the diameter of ⁇ 60 pm for MGP fibers, the PC hollow tube model with an inner diameter of 0.06 mm, an outer diameter of 0.08 mm, and
  • the mechanical behavior of PC hollow tube during thermal drawing was simulated based on the isotropic bulk modulus (E) of 0.18 GP and Poison ratio (u) of 0.35.
  • E isotropic bulk modulus
  • u Poison ratio
  • the mechanical property of PC at the temperature of 160 °C was characterized by the direct mechanical analyzer (DMA) instrument (DMA Q800).
  • the woven textiles prepared by three layers of MXene-based fibers, were tested for EMI shielding in a DR-WX rectangular waveguide with using the ENA5071C network analyzer (USA) at the Xband frequency range of 8.2 GHz to 12.4 GHz.
  • the MXene-based fibers were weaved into the rectangular shape textiles of 30 mmxl6 mm for the test.
  • the textiles’ ability to attenuate the energy of the incident electromagnetic waves was evaluated as EMI SE.
  • EMI SE As an electromagnetic radiation into electromagnetic interference shielding equipment, the absorption (A), reflection (A), and transmission (T) should add up to 1, exhibiting the shielding phenomenon, that is,
  • the shielding reflection (SER) and absorption (SEA) can be estimated according to the as coefficients of R and T follows:
  • the multiple internal reflections can be generally negligible as more than 15 dB.
  • the total EMI SET is the contributions of reflection (SER) and absorption (SEA), which can be evaluated as follows:
  • SE T SE R + SE A (8)
  • Electrothermal property of a single fabricated fibers and textiles was investigated using a DC power supply (MP5020D). Silver paste was used as a contact point to connect the MXene-based fibers and conductive copper wires to accelerate the test.
  • the thermal images and temperature-time curves of the fibers were recorded by an IR thermal imaging instrument of FLIR A3255SC camera.
  • the electrical-thermal behavior of textiles was performed as same as that of single MXene-based fibers
  • the electrical conductivity of the fabricated MXene-based fibers was measured using a Keithley 2700 source meter with the two-point probe method. Silver paste was conducted as a contact point to connect the MXene fibers and conductive probes.
  • the porosity ( ) of the fabricated MXene-based fibers were calculated according to the structural parameters via equation (12): where p MF is the density of MXene-based fibers, p M is the TEC2 density of 5.2 g cm -3 , d 002 is the d-spacing (002) of the MXene-based fibers, and d M is the d-spacing of TisC2 crystals (1.02 nm).

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  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
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