CN113203771A - Humidity sensing fiber and preparation method and application thereof - Google Patents

Humidity sensing fiber and preparation method and application thereof Download PDF

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Publication number
CN113203771A
CN113203771A CN202110458566.9A CN202110458566A CN113203771A CN 113203771 A CN113203771 A CN 113203771A CN 202110458566 A CN202110458566 A CN 202110458566A CN 113203771 A CN113203771 A CN 113203771A
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humidity
sensing
moisture
humidity sensing
polymer
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CN113203771B (en
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陶光明
李攀
欧阳静宇
夏治刚
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Wuhan Xinrunxing Material Technology Co ltd
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Huazhong University of Science and Technology
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Priority to PCT/CN2022/088700 priority patent/WO2022228330A1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • 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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt 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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/12—Stretch-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
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/12—Threads containing metallic filaments or strips
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
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    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/048—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance for determining moisture content of the material
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature

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Abstract

The invention provides a humidity sensing fiber which comprises a humidity sensing layer and conductive wires arranged in the humidity sensing layer, wherein the humidity sensing layer comprises a polymer and humidity sensitive materials distributed in the polymer. Compared with the prior art, the invention has the following advantages: firstly, the humidity sensitive material and the polymer substrate material have wide selection range, diversified preparation process and high production efficiency. The thermal softening wire drawing process is adopted, the structural design of the prefabricated rod is diversified, so that fibers with different cross-section structures can be designed, and the distribution of humidity sensitive materials with different concentrations in the fibers can be accurately controlled. Secondly, the humidity sensitive material is integrated into the fiber, and the fabric is prepared through a weaving process, so that the softness of the fabric can be realized, the washing performance and the durability can be realized, and the requirements of wearable equipment are met. Finally, the temperature sensing fiber can have the function of resisting temperature interference by selecting a proper humidity sensitive material.

Description

Humidity sensing fiber and preparation method and application thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a humidity sensing fiber and a preparation method and application thereof.
Background
With the development of artificial intelligence technology, the development of functional fibers is receiving much attention, and the functional fibers are increasingly widely applied due to the unique wearable special new characteristics. Based on the vigorous development of functional fibers, the textile industry is currently developing towards intelligent wearable direction, and the functional fibers can be used in the fields of health monitoring, temperature control, humidity control, electronic skin, flexible luminescence and the like. The patent particularly relates to a humidity sensing fiber, yarn and fabric and a preparation method thereof, and the fiber, the yarn and the fabric can be used in the fields of health monitoring, artificial skin and the like. At present, the humidity sensor mainly has a thin film state, the preparation process is complex, the humidity sensitive layer is easy to fall off, the durability is low, and the thin film state is lack of wearable performance.
Chinese patent CN107655514A discloses a dry-wet temperature and humidity sensing probe using a fiber grating sensor. The temperature sensor senses the external temperature change by adopting the fiber bragg grating, and the humidity sensor measures the relative humidity of the environment by adopting a fiber bragg grating dry-wet contrast method. Chinese patent CN108801497A discloses a hair type temperature and humidity sensing probe using a fiber grating sensor, wherein the temperature sensor uses a fiber grating to sense the external temperature change, and the humidity sensor uses a fiber grating hair type humidity sensing principle to measure the relative humidity of the environment. International patent WO2007137429a1 and canadian patent CA2549084a1 disclose a humidity sensor using fiber grating, which can detect humidity and temperature simultaneously, and has the following main limitations: the cross sensitivity of temperature, humidity, bending, strain, refractive index and the like is high, the demodulation is difficult, and the measurement precision is low. The bragg grating sensor needs a dual-wavelength light source and a spectrometer, and the system cost is relatively high.
Chinese patent CN103064145A discloses a humidity sensing optical fiber and a preparation method and application thereof, the humidity sensing optical fiber comprises a fiber core and a coating layer for coating the fiber core, one section of the humidity sensing optical fiber is a humidity sensitive section optical fiber, a metal film layer and a nano porous film layer are sequentially arranged on the surface of the fiber core of the humidity sensitive section optical fiber, and Chinese patent CN106644959A discloses an evanescent wave coupling humidity sensing optical fiber and a preparation method thereof. The optical fiber comprises a fiber core and a coating layer wrapping the fiber core, wherein one part of the coating layer is a humidity-sensitive coating layer. Chinese patent CN 107561039a discloses a humidity sensor based on graphene oxide coated optical fiber, wherein a layer of graphene oxide is coated on the surface of a second section of optical fiber of an optical fiber sensing head. Chinese invention patent CN 108896199 a discloses a stretchable yarn sensor and a method for making the same. The sensitive fiber is prepared by coating a temperature-sensitive material or a humidity-sensitive material on the surface of a matrix fiber, and the dielectric material is coated after the two ends of the sensitive fiber are connected with an electrode wire, so that the electrode yarn is obtained. The environment humidity condition is analyzed by detecting the light intensity through polishing the surface of the optical fiber, coating humidity sensitive material coatings (gold layer and hydrophilic material) on the surface of the optical fiber, such as U.S. Pat. No. 10527539B2, U.S. Pat. No. 2018238791A1, Canadian Pat. No. CA2996384A1, and the like. The main limitations are as follows: the optical fiber humidity sensor is mainly sensitized by using a humidity sensitive material, but the relation between the thickness of a humidity sensitive film and the sensing performance of the sensor is complex, how to obtain the high-sensitivity humidity sensor is not clear, and the optical fiber humidity sensor is poor in durability and short in service life due to the adoption of a coating process and is not suitable for being worn.
Chinese patent CN110133068A discloses a humidity sensor based on electrostatic spinning nanofiber fabric, which comprises nanofiber fabric, a metal coating and a humidity sensitive material layer; the upper surface and the lower surface of the nanofiber fabric are both provided with metal coatings, and the surfaces of the two metal coatings are both plated with humidity sensitive material layers. Chinese patent CN1104124870A discloses a fabric type flexible composite sensor and a manufacturing method thereof, which realizes the detection of humidity by printed electrodes and functional films. Chinese patent CN109752412A discloses a method for manufacturing a flexible humidity sensor based on a nanofiber membrane, which includes an electrode layer based on a flexible substrate and a humidity sensitive polymer thin film, and US2017082567a1 discloses a trench-based capacitive humidity sensor, which has a plurality of trenches formed in a conductive layer (such as polysilicon or metal) on a substrate. The trenches are arranged parallel to each other and divide the conductive layer into a plurality of trench-shaped silicon electrodes, at least two of which are configured as a capacitive humidity sensor. The main limitations are as follows: the film state lacks wearable performance, fails to realize the softness of fabrics, is uncomfortable to wear by human bodies, and has no water washability and durability. The external conditions may cause the humidity sensitive material to be peeled off and damaged.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a humidity sensing fiber and a preparation method and application thereof.
Specifically, the present invention relates to the following aspects:
1. the humidity sensing fiber is characterized by comprising a humidity sensing layer and conductive filaments arranged in the humidity sensing layer, wherein the humidity sensing layer comprises a polymer and humidity sensitive materials distributed in the polymer.
2. The humidity sensing fiber according to claim 1, wherein the humidity sensing layer comprises a humidity sensing core layer and a humidity sensing cladding layer arranged from inside to outside, conductive filaments are arranged in the humidity sensing cladding layer, the humidity sensing core layer comprises a polymer and humidity sensitive materials distributed in the polymer, and the humidity sensing cladding layer comprises a polymer and humidity sensitive materials distributed in the polymer.
3. The humidity sensing fiber according to claim 1, wherein the humidity sensitive material is one or two or more selected from the group consisting of a metal oxide humidity sensitive material, a silicon humidity sensitive material, a ceramic humidity sensitive material, polyimide, polystyrene, carboxymethyl cellulose and hydroxyethyl cellulose, graphene, MXene, amorphous carbon, graphite powder, and carbon nanotubes.
4. The humidity sensing fiber according to item 3, wherein the humidity sensitive material is graphene and MXene.
5. The humidity sensing fiber according to item 4, wherein the mass ratio of MXene to graphene is 0.01 to 100, and preferably 1 to 10.
6. The humidity sensing fiber according to claim 1, wherein the polymer is selected from the group consisting of Polymethylmethacrylate (PMMA), fluororesin, PMMA composite doped with fluorinated polymer (F-PMMA), styrene-methylmethacrylate copolymer (SMMA), Cyclic Olefin Copolymer (COC), Cyclic Olefin Polymer (COP), Polycarbonate (PC), polyphenylene sulfone resin (PPSU), polyethersulfone resin (PES), Polyethyleneimine (PEI), Polystyrene (PS), Polyethylene (PE), polypropylene (PP), Polyamide (PA), Polyimide (PI), polyethylene terephthalate (PET), Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polyurethane (PU), polyvinyl chloride (PVC), One or more than two of Polystyrene (PS), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), acrylonitrile-butadiene-styrene copolymer (ABS), polyethylene glycol (PEG), thermoplastic elastomer (TPE), low-density polyethylene (LDPE), polyethylene glycol (PEG), high-density polyethylene (HDPE), Polyformaldehyde (POM), polyphenylene oxide (PPO), polyester and sodium isophthalate sulfonate copolymer, acrylate copolymer, vinyl acetate resin and polyvinyl acetal, preferably, the first and second liquid crystal materials are, one or more selected from polyethylene terephthalate (PET), Cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polycarbonate (PC), thermoplastic elastomer (TPE) and fluorine resin.
7. The humidity sensing fiber according to item 1, wherein the moisture sensitive material in the moisture sensing cladding layer is greater in mass content than the moisture sensitive material in the moisture sensing core layer.
8. Moisture-sensing fiber according to item 7, wherein the moisture-sensitive material in the moisture-sensing cladding is present in an amount of 0.01 to 40 wt.%, preferably 20 to 40 wt.%.
9. The moisture-sensing fiber according to item 7, wherein the moisture-sensitive material in the moisture-sensing core layer has a mass ratio of 0.01 wt.% to 20 wt.%.
10. A method for preparing a humidity-sensing fiber, wherein the method is selected from a coextrusion process, a melt spinning process, a wet spinning process or a heat softening and drawing process.
11. The production method according to item 10, characterized in that the coextrusion process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
respectively filling the low-concentration humidity sensing composite master batch and the high-concentration humidity sensing composite master batch into a hopper A (core layer) and a hopper B (cladding layer) of a plastic extruder, adjusting the temperature and the pressure, passing through a core-cladding structure extrusion molding die head, passing through the conductive wire by the perforated cladding extrusion molding die head, slowly conveying the conductive wire, and adjusting the traction speed and the wire feeding speed of the conductive wire to prepare the humidity sensing fiber.
12. The production method according to item 10, wherein the melt spinning process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
respectively filling the low-concentration humidity sensing composite master batch and the high-concentration humidity sensing composite master batch into a hopper A (core layer) and a hopper B (cladding layer) of a melt spinning machine, adjusting the temperature and the pressure, passing through a spinning assembly, opening holes on the side surface of the spinning assembly, conveying conductive wires, adjusting the spinning speed and the conveying speed of the conductive wires, and preparing the humidity sensing fiber.
13. The production method according to item 10, wherein the moisture spinning process comprises the steps of:
preparing a humidity sensing composite material solution;
placing humidity sensing composite material solutions with different concentrations in an extrusion device (double-needle extrusion), synchronously arranging conveying conductive wires on the side surface of an extrusion port, dissolving a chloroform solvent of a mixed polymer material in an analytically pure ethanol solution after the solution passes through the analytically pure ethanol solution contained in the device, changing the mixed polymer material from the solution to a gel state, and controlling the traction speed of the device to prepare the humidity sensing fiber.
14. The production method according to item 10, characterized in that the thermal softening drawing process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
preparing a humidity sensing prefabricated rod from the humidity sensing composite master batch;
and (3) passing the conductive wire through the humidity sensing prefabricated rod, and preparing the humidity sensing fiber through thermal softening and wire drawing.
15. The method of claim 14, wherein said passing an electrically conductive filament through said humidity sensing preform further comprises sleeving an intermediate preform inside said humidity sensing preform, wherein said preparing of said intermediate preform comprises the steps of:
preparing a second humidity sensing composite masterbatch, the second humidity sensing composite masterbatch comprising a humidity sensitive material and a polymer.
16. The method according to item 10, wherein the humidity sensitive material is one or two or more selected from the group consisting of a metal oxide humidity sensitive material, a silicon humidity sensitive material, a ceramic humidity sensitive material, polyimide, polystyrene, carboxymethyl cellulose and hydroxyethyl cellulose, graphene, MXene, amorphous carbon, graphite powder, and carbon nanotubes.
17. The production method according to item 16, wherein the humidity sensitive material is graphene and MXene.
18. The method according to item 17, wherein a mass ratio of MXene to graphene is 0.01 to 100, and preferably 1 to 10.
19. The method according to item 10, wherein the polymer is selected from the group consisting of polymethyl methacrylate (PMMA), fluororesin, PMMA composite material doped with fluorinated polymer (F-PMMA), styrene-methyl dimethacrylate copolymer (SMMA), cycloolefin copolymer (COC), cycloolefin polymer (COP), Polycarbonate (PC), polyphenylene sulfone resin (PPSU), polyethersulfone resin (PES), Polyethyleneimine (PEI), Polystyrene (PS), Polyethylene (PE), polypropylene (PP), Polyamide (PA), Polyimide (PI), polyethylene terephthalate (PET), Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polyurethane (PU), polyvinyl chloride (PVC), One or more than two of Polystyrene (PS), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), acrylonitrile-butadiene-styrene copolymer (ABS), polyethylene glycol (PEG), thermoplastic elastomer (TPE), low-density polyethylene (LDPE), polyethylene glycol (PEG), high-density polyethylene (HDPE), Polyformaldehyde (POM), polyphenylene oxide (PPO), polyester and sodium isophthalate sulfonate copolymer, acrylate copolymer, vinyl acetate resin and polyvinyl acetal, preferably, the first and second liquid crystal materials are, one or more selected from polyethylene terephthalate (PET), Cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polycarbonate (PC), thermoplastic elastomer (TPE) and fluorine resin.
20. The production method according to item 10, wherein the mass ratio of the humidity sensitive material in the humidity sensing composite masterbatch is 0.01 wt.% to 40 wt.%, preferably 20 wt.% to 40 wt.%.
21. The method according to item 15, wherein the mass ratio of the humidity sensitive material in the second humidity sensing composite masterbatch is 0.01 wt.% to 20 wt.%.
22. The production method according to item 10, wherein the humidity sensing composite masterbatch is produced by a physical blending method or a physical/chemical blending method or a solution blending method.
23. A humidity sensing fiber prepared by the method of any one of items 10 to 22.
24. The humidity sensing yarn is characterized by being prepared by twisting n fibers, wherein n is a natural number greater than or equal to 2, and at least one fiber is a humidity sensing fiber.
25. The moisture-sensing yarn of claim 20, wherein the moisture-sensing fiber is the moisture-sensing fiber of any one of claims 1-9, 19.
26. The humidity sensing fabric is characterized by being woven by humidity sensing fibers or humidity sensing yarns.
27. The humidity sensing fabric of claim 22, wherein the humidity sensing fiber is the humidity sensing fiber of any one of claims 1-9, 19.
28. The humidity sensing fabric of item 23, wherein the humidity sensing yarn is the humidity sensing yarn of item 24 or 25.
Compared with the prior art, the invention has the following advantages: firstly, the humidity sensitive material and the polymer substrate material have wide selection range, diversified preparation process and high production efficiency. The thermal softening wire drawing process is adopted, the structural design of the prefabricated rod is diversified, so that fibers with different cross-section structures can be designed, and the distribution of humidity sensitive materials with different concentrations in the fibers can be accurately controlled. Secondly, the humidity sensitive material is integrated into the fiber, and the fabric is prepared through a weaving process, so that the softness of the fabric can be realized, the washing performance and the durability can be realized, and the requirements of wearable equipment are met. Finally, the temperature sensing fiber with the function of resisting temperature interference can be realized by selecting proper humidity sensitive materials
Drawings
Fig. 1 shows the temperature characteristics of graphene and MXexe.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not intended to be limiting.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Although methods and materials similar or equivalent to those described herein can be used in experimental or practical applications, the materials and methods are described below. In case of conflict, the present specification, including definitions, will control, and the materials, methods, and examples are illustrative only and not intended to be limiting. The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The invention provides a humidity sensing fiber which comprises a humidity sensing layer and conductive wires arranged in the humidity sensing layer, wherein the humidity sensing layer comprises a polymer and humidity sensitive materials distributed in the polymer.
Wherein the conductive wire can be one or more, the conductive wire can be selected from metal filaments such as copper wire, tungsten wire, nickel-chromium wire, stainless steel wire, platinum wire, molybdenum wire, silver wire and alloy wire thereof, metal yarns such as stainless steel yarn, iron fiber yarn, copper yarn, silver yarn and the like, polyester fiber, spandex fiber, acrylic fiber, aramid fiber, polyamide fiber, polypropylene fiber, polyvinylidene fluoride (PVDF) fiber, nylon fiber, acrylic fiber, polyester fiber and other synthetic fibers coated with metal conductive materials such as gold/silver nanowire/particles, silver, nickel, gold and alloy thereof, natural fibers such as cotton, wool, flax, silk fiber and other fibers coated with metal conductive materials such as silver, nickel, gold and alloy thereof, carbon materials such as Carbon Nanotube (CNT), Carbon Black (CB), Carbon Fiber (CF), graphene, MXene and the like, PEDOT is PSS, PPY, PANI and other conductive polymers, one or more of eutectic gallium indium (EGaIn) and other liquid metals, and Sn and other low-melting point metals.
The humidity sensitive materials in the temperature sensing layer can be uniformly distributed or distributed in a certain gradient. Therefore, the humidity sensing layer may be an integral structure, and may further include a humidity sensing core layer and a humidity sensing cladding layer disposed from inside to outside, wherein conductive filaments are disposed in the humidity sensing cladding layer, the humidity sensing core layer includes a polymer and a humidity sensitive material distributed in the polymer, and the humidity sensing cladding layer includes a polymer and a humidity sensitive material distributed in the polymer.
The humidity sensitive material refers to a material which can detect the humidity of an object or a space and can give a change of an electric signal according to a change of temperature.
In one embodiment, the humidity sensitive material is selected from one or two or more of metal oxide humidity sensitive material, silicon humidity sensitive material, ceramic humidity sensitive material, polyimide, polystyrene, carboxymethyl cellulose and hydroxyethyl cellulose, graphene, MXene, amorphous carbon, graphite powder and carbon nano tube.
Further, the humidity sensitive material is graphene and MXene. Namely, the humidity sensing layer (comprising the humidity sensing core layer and the humidity sensing cladding layer) simultaneously contains two materials of graphene and MXene. In a preferred embodiment, the mass ratio of MXene to graphene is 0.01 to 100, preferably 1 to 10, and may be, for example, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5, 1:5.5, 1:6, 1:6.5, 1:7, 1:7.5, 1:8, 1:8.5, 1:9, 1:9.5, 1: 10. Within this range, the humidity sensing layer not only has the humidity sensing function, but also has the anti-temperature interference function, and the concrete reason is as follows: MXene has a positive TCR (temperature coefficient of resistance) and Graphene has a negative TCR, and when mixed in the above ratio, TCR → 0 can be realized, thereby eliminating temperature interference.
In a preferred embodiment, the moisture-sensitive material is present in the moisture-sensing cladding layer in a greater mass amount than the moisture-sensitive material in the moisture-sensing core layer.
Further, the mass ratio of the humidity sensitive material in the humidity sensing cladding is 0.01 wt.% to 40 wt.%, preferably 20 wt.% to 40 wt.%. . The mass ratio of the humidity sensitive material in the humidity sensing core layer is 0.01 wt.% to 20 wt.%. . The mass ratio refers to the ratio of the mass of the temperature sensitive material in the cladding layer or the core layer to the mass of the corresponding cladding layer or the core layer.
In one embodiment, the polymer material is selected from the group consisting of Polymethylmethacrylate (PMMA), fluororesin, PMMA composite doped with fluorinated polymer (F-PMMA), styrene-methylmethacrylate copolymer (SMMA), Cyclic Olefin Copolymer (COC), Cyclic Olefin Polymer (COP), Polycarbonate (PC), polyphenylenesulfone resin (PPSU), polyethersulfone resin (PES), Polyethyleneimine (PEI), Polystyrene (PS), Polyethylene (PE), polypropylene (PP), Polyamide (PA), Polyimide (PI), polyethylene terephthalate (PET), Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polyurethane (PU), polyvinyl chloride (PVC), Polystyrene (PS), One or more than two of polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), acrylonitrile-butadiene-styrene copolymer (ABS), polyethylene glycol (PEG), thermoplastic elastomer (TPE), low-density polyethylene (LDPE), polyethylene glycol (PEG), high-density polyethylene (HDPE), Polyformaldehyde (POM), polyphenyl ether (PPO), polyester and sodium isophthalate copolymer, acrylate copolymer, vinyl acetate resin and polyvinyl acetal, preferably, the first and second liquid crystal materials are, one or more selected from polyethylene terephthalate (PET), Cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polycarbonate (PC), thermoplastic elastomer (TPE) and fluorine resin.
The invention also provides a preparation method of the humidity sensing fiber, which comprises but is not limited to a co-extrusion process, a melt spinning process, a wet spinning process, a heat softening and wire drawing process and the like.
In one embodiment, the coextrusion process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
respectively filling the low-concentration humidity sensing composite master batch and the high-concentration humidity sensing composite master batch into a hopper A (core layer) and a hopper B (cladding layer) of a plastic extruder, adjusting the temperature and the pressure, adjusting the temperature at 0-450 ℃ and the pressure at 0-40MPa, passing through a core-cladding structure extrusion molding die head, penetrating through the conductive wire by the perforated cladding extrusion molding die head, slowly conveying the conductive wire, and adjusting the traction speed and the wire feeding speed of the conductive wire to obtain the humidity sensing fiber.
In a specific embodiment, the melt spinning process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
respectively filling the low-concentration humidity sensing composite master batch and the high-concentration humidity sensing composite master batch into a hopper A (core layer) and a hopper B (cladding layer) of a melt spinning machine, adjusting the temperature and the pressure at 0-450 ℃ and 0-20MPa, passing through a spinning assembly, opening a hole on the side surface of the spinning assembly, conveying conductive wires, and adjusting the spinning speed and the conveying speed of the conductive wires to obtain the humidity sensing fiber.
In a specific embodiment, the wet spinning process comprises the steps of:
preparing a humidity sensing composite material solution;
the humidity sensing composite material solutions with different concentrations are placed in an extrusion device (double-needle extrusion), conveying conductive wires are synchronously arranged on the side surface of an extrusion port, after passing through an analytically pure ethanol solution contained in the device, a chloroform solvent of a mixed polymer material is dissolved in the analytically pure ethanol solution, the mixed polymer material is changed into a gel state from the solution, and the traction speed of the device is controlled to obtain the fiber with the target diameter. And (3) drying the fibers in a 50 ℃ ventilation oven for 24h, and drying in a 50 ℃ vacuum drying oven for 24h to remove the residual solvent to obtain the humidity sensing fibers.
In a particular embodiment, the heat softening drawing process comprises the steps of:
preparing a humidity sensing composite master batch, wherein the humidity sensing composite master batch comprises a humidity sensitive material and a polymer;
preparing a humidity sensing prefabricated rod from the humidity sensing composite master batch;
and (3) passing the conductive wire through the humidity sensing prefabricated rod, and preparing the humidity sensing fiber through thermal softening and wire drawing.
Wherein the humidity sensing composite master batch can be prepared by a physical blending method or a physical/chemical blending method or a solution blending method. The preform may be prepared by any method known in the art, for example, by hot pressing or extrusion.
In a preferred embodiment, said passing of the conductive filaments through the moisture-sensing preform further comprises nesting an intermediate preform inside the moisture-sensing preform, wherein the intermediate preform comprises a moisture-sensitive material and a polymer. The moisture sensing fiber prepared in this manner includes a core layer and a cladding layer. Wherein the intermediate preform is prepared in the same manner as the preform.
In the above-mentioned manufacturing method, the humidity-sensitive material, the polymer, and the conductive yarn are selected and defined as described above, that is, the above-mentioned definition with respect to the humidity-sensitive material, the polymer, and the conductive yarn in the humidity sensing fiber.
In a specific embodiment, the mass proportion of the humidity sensitive material in the humidity sensing composite masterbatch is 0.01 wt.% to 40 wt.%, preferably 20 wt.% to 40 wt.%.
In a specific embodiment, the mass of the humidity sensitive material in the second humidity sensing composite masterbatch is 0.01 wt.% to 20 wt.% of the total mass.
The invention also provides a humidity sensing fiber prepared by the preparation method.
The humidity sensing fiber can be further applied to humidity sensing yarns and humidity sensing fabrics.
The invention also provides a humidity sensing yarn which is prepared by twisting n fibers, wherein n is a natural number greater than or equal to 2, and at least one fiber is a humidity sensing fiber. Wherein the humidity sensing fiber is the humidity sensing fiber or the humidity sensing fiber prepared by the method.
The invention also provides a humidity sensing fabric which is formed by weaving the humidity sensing fibers or the humidity sensing yarns. Wherein the humidity sensing fiber is the humidity sensing fiber or the humidity sensing fiber prepared by the method. The humidity sensing yarn is the temperature sensing yarn.
Examples
Example 1
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polymethyl methacrylate (PMMA) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding the polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 30g of graphene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polymethyl methacrylate (PMMA), fluororesin, graphene and polydimethylacetamide (DMAC). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain a humidity sensing composite material, wherein the mass content of the graphene is 30 wt.%;
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material is put into a mold with the length multiplied by the width multiplied by the height of 100mm multiplied by 22mm, the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered with the mold after heat softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) and (3) placing the prepared preform into a lathe fixture, processing the preform by adjusting the rotating speed and the feed distance, wherein the rotating speed of the lathe is 150 + 300r/min, and processing the preform into a round shape with the cross section area of 20mm and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod machined by the lathe by using a drill floor, wherein the drill bit is directly 1.5mm, the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 1.5mm is obtained after the prefabricated rod is machined by the drill floor, and the position 3mm away from the lower end of the hollow prefabricated rod is radially punched, so that the prefabricated rod with the hole structure and capable of sensing the humidity can be obtained.
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Example 2
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polyethylene terephthalate (PET) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 30g of graphene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polyethylene terephthalate (PET), fluororesin, graphene and polydimethylacetamide (DMAC). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain a humidity sensing composite material, wherein the mass content of the graphene is 30 wt.%;
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material is put into a mold with the length multiplied by the width multiplied by the height of 100mm multiplied by 22mm, the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered with the mold after heat softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) the prepared preform is placed in a lathe fixture, the preform is processed by adjusting the rotating speed and the feed distance, the rotating speed of the lathe is 150 and 300r/min, and the preform is processed into a round shape with the cross-sectional area of 20m m and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod machined by the lathe by using a drill floor, wherein the drill bit is directly 1.5mm, the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 1.5mm is obtained after the prefabricated rod is machined by the drill floor, and the position 3mm away from the lower end of the hollow prefabricated rod is radially punched, so that the prefabricated rod with the hole structure and capable of sensing the humidity can be obtained.
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Example 3
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polyethylene terephthalate (PET) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 30g of MXene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polyethylene terephthalate (PET), fluororesin, MXene and Dimethylacetamide (DMAC). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain the humidity sensing composite material, wherein the MXene mass content is 30 wt.%;
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material is put into a mold with the length multiplied by the width multiplied by the height of 100mm multiplied by 22mm, the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered with the mold after heat softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) and (3) placing the prepared preform into a lathe fixture, processing the preform by adjusting the rotating speed and the feed distance, wherein the rotating speed of the lathe is 150 + 300r/min, and processing the preform into a round shape with the cross section area of 20mm and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod machined by the lathe by using a drill floor, wherein the drill bit is directly 1.5mm, the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 1.5mm is obtained after the prefabricated rod is machined by the drill floor, and the position 3mm away from the lower end of the hollow prefabricated rod is radially punched, so that the prefabricated rod with the hole structure and capable of sensing the humidity can be obtained.
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Example 4
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polyethylene terephthalate (PET) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 8.6g of MXene and 21.4g of graphene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polyethylene terephthalate (PET), fluororesin, MXene, graphene and poly (dimethylacetamide). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain the humidity sensing composite material, wherein the total mass content of MXene and graphene is 30 wt.%;
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material is put into a mold with the length multiplied by the width multiplied by the height of 100mm multiplied by 22mm, the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered with the mold after heat softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) and (3) placing the prepared preform into a lathe fixture, processing the preform by adjusting the rotating speed and the feed distance, wherein the rotating speed of the lathe is 150 + 300r/min, and processing the preform into a round shape with the cross section area of 20mm and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod machined by the lathe by using a drill floor, wherein the drill bit is directly 1.5mm, the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 1.5mm is obtained after the prefabricated rod is machined by the drill floor, and the position 3mm away from the lower end of the hollow prefabricated rod is radially punched, so that the prefabricated rod with the hole structure and capable of sensing the humidity can be obtained.
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Example 5
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polyethylene terephthalate (PET) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 15g of MXene and 15g of graphene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polyethylene terephthalate (PET), fluororesin, MXene, graphene and polydimethylacetamide (DMAC). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain a humidity sensing composite material, wherein the mass content of MXene and graphene is 30 wt.%;
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material is put into a mold with the length multiplied by the width multiplied by the height of 100mm multiplied by 22mm, the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered with the mold after heat softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) and (3) placing the prepared preform into a lathe fixture, processing the preform by adjusting the rotating speed and the feed distance, wherein the rotating speed of the lathe is 150 + 300r/min, and processing the preform into a round shape with the cross section area of 20mm and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod machined by the lathe by using a drill floor, wherein the drill bit is directly 1.5mm, the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 1.5mm is obtained after the prefabricated rod is machined by the drill floor, and the position 3mm away from the lower end of the hollow prefabricated rod is radially punched, so that the prefabricated rod with the hole structure and capable of sensing the humidity can be obtained.
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Example 6
The humidity sensing fiber is prepared by the following specific operation steps.
The preparation method of the humidity sensing composite material comprises the following steps: (1) weighing 55g of polyethylene terephthalate (PET) and 15g of fluororesin, measuring 200mL of Dimethylacetamide (DMAC) by using a beaker, adding polymethyl methacrylate and the fluororesin into the beaker, mixing with the Dimethylacetamide (DMAC), placing on a magnetic stirrer, and heating and stirring in a water bath at 80 ℃ until particles are dissolved to obtain a uniform mixed solution. (2) Adding 8.6g of MXene and 21.4g of graphene into the mixed solution, stirring by a magnetic stirrer, and placing in an ultrasonic device for ultrasonic dispersion for 15min to obtain a mixed solution of polyethylene terephthalate (PET), fluororesin, MXene, graphene and poly (dimethylacetamide). (3) The mixed solution was poured into a container of 20cm × 20cm × 2cm (length × width × height) folded with tin foil paper and dried. After air-drying in a fume hood for 24 hours, the dried product was placed in a forced air drying oven or a vacuum drying oven and dried at 70 ℃ for 48 hours. (4) Cutting the dried mixed sample into blocks with the length and width smaller than 8mm by using scissors, and putting the blocks into a drying oven for later use to obtain the humidity sensing composite material, wherein the total mass content of MXene and graphene is 30 wt.%;
preparing the humidity sensing composite material according to the preparation method, wherein the raw materials are as follows: 75g of polyethylene terephthalate (PET) and 15g of fluororesin, 2.8g of MXene and 7.2g of graphene. In the prepared humidity sensing composite material, the total mass content of MXene and graphene is 10 wt.%.
Outer layer preform preparation (total mass content of MXene and graphene 30 wt.%):
the preparation of the preform comprises the following steps: (1) the humidity sensing composite material (the total concentration of MXene and graphene is 30 wt.%) is put into a mold of 100mm × 22mm × 22mm (length × width × height), the mold is a stainless steel groove, and the periphery of the groove is coated with a Teflon film to prevent the polymer material from being adhered to the mold after thermal softening. (2) And covering the upper side and the lower side of the die filled with the mixture material with stainless steel plates, and putting the die into a hot press to ensure uniform stress in the pressurizing process. Setting the temperature on the hot press to be 120 ℃, preheating the mixture in the mould for 3min under the pressure of 1MPa, then increasing the pressure to 5MPa, and repeating the step until the preform is molded. (3) And taking out the hot-pressed preform rod by using a punch and then putting the preform rod into a drying box for later use.
The processing of the hollow structure preform comprises the following steps: (1) and (3) placing the prepared preform into a lathe fixture, processing the preform by adjusting the rotating speed and the feed distance, wherein the rotating speed of the lathe is 150 + 300r/min, and processing the preform into a round shape with the cross section area of 20mm and the length of 100mm by the lathe. (2) And axially punching the prefabricated rod processed by the lathe by using a drill floor, wherein a drill bit is directly 10mm, and the hollow prefabricated rod with the outer diameter of 20mm and the inner diameter of 10mm is obtained after the prefabricated rod is processed by the drill floor.
Inner layer preform preparation (MXene and graphene total mass content 10 wt.%)
Referring to the outer preform preparation method, a hollow preform having an outer diameter of 10mm and an inner diameter of 1.5mm was prepared.
Combining the inner and outer layers of prefabricated rod to perform thermosetting, and radially punching the position 3mm away from the lower end of the obtained hollow prefabricated rod to obtain the prefabricated rod with the porous structure for sensing the humidity
The thermal softening and wire drawing of the prepared humidity sensing prefabricated rod with the porous structure comprises the following steps: (1) a stainless steel wire with the wire diameter of 50 mu m is wound on an annular accommodating coil, the free end of the stainless steel wire penetrates through a through hole of a prefabricated rod fixed on a wire drawing device, the lower end of the prefabricated rod radially penetrates through a metal wire, and a weight of 20g is fixed at the lower ends of the stainless steel wire and the metal wire. (2) And opening the heating furnace, setting the temperature of the upper temperature zone to be 195 ℃ and the temperature of the lower temperature zone to be 295 ℃, and setting the rod when the temperature of the heating zone reaches the preset temperature. (3) After the preform is heated and softened, the stub bar falls down and passes through a diameter measuring instrument, a tensiometer and a traction shaft in sequence, the rod feeding speed is set to be 0.1mm/min, and the stable filament winding speed is set to be 0.16m/min, so that the humidity sensing fiber with the filament diameter of 500 microns is obtained.
Specifically, the main conditions of the above examples are shown in table 1.
TABLE 1
Figure BDA0003041393450000171
Figure BDA0003041393450000181
Application example
Graphene and MXene are humidity sensitive materials with two different characteristics, graphene TCR <0, namely, resistance of the graphene is reduced along with temperature increase, MXene TCR <0, namely, resistance of the graphene is increased along with temperature increase, and the mixing ratio (1:1, 2:1, 2.5:1 and 3:1) of the graphene and the MXene is studied, as shown in FIG. 1, when the mass ratio of the graphene to the MXene is 2.5:1, resistance change (TCR is 0 delta R/R is 0) is almost unchanged along with temperature change. When the mass ratio of graphene to MXene is 1:1, the resistance change of the graphene to MXene is increased along with the temperature change (TCR >0 delta R/R >0), and the temperature change is in positive correlation with the resistance.
In addition, the humidity sensing and temperature interference tests were performed on the humidity sensing fibers prepared in examples 1 to 6, and the resistance of the prepared fibers of examples 1 to 6 was measured by selecting a section (about 10cm) at a constant temperature (25 ℃) and different humidity (20 to 80 RH%). Specific data records as shown in table 2, a section (about 10cm) of the prepared fiber example 2-5 was selected and tested for resistance at different humidities (20-80 RH%), and different temperatures (45, 65 ℃), specifically, a humidity temperature adjustable small chamber (size 15 × 15cm) was prepared, a heater (OCr25Al5 material) was disposed on the chamber floor, the temperature was raised by controlling the floor heater (temperature controller model CN740), and the real-time temperature was measured with a commercial thermocouple (UNI-TUT 325). Dry nitrogen is introduced into deionized water at different flow rates for bubbling, and then is sent into a small chamber, a commercial humidity sensor (CEM DT-83) is arranged in the chamber for detecting the humidity condition, the humidity in the chamber is adjusted by controlling the flow of the nitrogen, the prepared humidity sensing fiber (embodiment 1-6) is placed in the small chamber, a metal electrode and an outer cladding layer in the fiber are respectively connected to a digital original meter (model 6500) COM end and a red end of Gishili for adjusting the test gear to be in a K omega gear, the resistance test resistance condition of the fiber is tested by adjusting different temperature and humidity conditions, and the specific data records are shown in tables 3-4. The moisture sensing fibers in the embodiments 4 and 6 are selected to test the breaking strength, specifically, an LC-202B universal material testing machine is used for testing, the prepared moisture sensing fibers in the embodiments 4 and 6 are selected, the length of the fibers is 10cm, two ends of the fibers are fixed on an upper clamping head and a lower clamping head of an instrument, the lower clamping head is fixed, the upward moving speed of the upper clamping head is adjusted to be 10mm/min, and the load condition of the fibers during breaking is recorded in the stretching process. Specific data records are shown in table 5.
TABLE 225 ℃ resistance results for the fibers of each example at various humidities
T＝25℃ RH(％) 20 40 60 80
Example 1 R(Ω/cm) 117.38 128.35 143.64 173.39
Example 2 R(Ω/cm) 123.45 146.49 160.34 193.43
Example 3 R(Ω/cm) 147.37 167.32 180.45 204.46
Example 4 R(Ω/cm) 130.32 152.23 173.23 199.35
Example 5 R(Ω/cm) 138.35 159.35 179.35 203.34
Example 6 R(Ω/cm) 172.35 211.43 264.35 321.35
TABLE 345 ℃ resistance results for fibers of each example at different humidities
T＝45℃ RH(％) 20 40 60 80
Example 2 R(Ω/cm) 118.34 138.45 152.32 179.45
Example 3 R(Ω/cm) 159.34 180.35 210.24 240.52
Example 4 R(Ω/cm) 137.34 160.34 178.34 204.23
Example 5 R(Ω/cm) 146.90 169.35 190.34 220.45
TABLE 465 ℃ resistance results for fibers of each example at different humidities
Figure BDA0003041393450000191
Figure BDA0003041393450000201
Table 5 fracture strength results for example 4 and example 6
T＝25℃RH＝20％D＝500μm Breaking strength (cN/dtex)
Example 4 1.43
Example 6 1.63
Discussion of experimental results: examples 1-6 it can be seen that as the humidity increases (RH% increases from 20 to 80), the humidity sensing fibers have a significant resistance change, i.e., the resistance gradually increases, and the initial resistance varies for different humidity sensing materials and substrate materials selected, as shown in table 2; as can be seen by comparing example 2 in tables 2-4, the resistance change gradually decreases with increasing temperature, but the humidity sensing characteristic is still positively correlated with the resistance. Comparing example 3 in tables 2 to 4, the resistance change gradually increases with the increase of temperature, and the humidity sensing characteristic is positively correlated with the resistance. Comparing example 4 of tables 2-4, the resistance change remained substantially unchanged with increasing temperature, but the humidity sensing characteristics remained positively correlated with resistance. Comparing example 5 in tables 2 to 4, the resistance change gradually increased with the increase in temperature, and the humidity sensing characteristic was positively correlated with the resistance. Comparative examples 4, 6 mechanical properties are measured as in table 5, and example 6 has better mechanical properties than example 4.

Claims (10)

1. The humidity sensing fiber is characterized by comprising a humidity sensing layer and conductive filaments arranged in the humidity sensing layer, wherein the humidity sensing layer comprises a polymer and humidity sensitive materials distributed in the polymer.
2. The moisture-sensing fiber according to claim 1, wherein the moisture-sensing layer comprises a moisture-sensing core layer and a moisture-sensing cladding layer, the moisture-sensing core layer comprises a polymer and a moisture-sensing material distributed in the polymer, and the moisture-sensing cladding layer comprises a polymer and a moisture-sensing material distributed in the polymer.
3. The humidity sensing fiber according to claim 1, wherein the humidity sensitive material is selected from one or two or more of metal oxide humidity sensitive material, silicon humidity sensitive material, ceramic humidity sensitive material, polyimide, polystyrene, carboxymethyl cellulose and hydroxyethyl cellulose, graphene, MXene, amorphous carbon, graphite powder, and carbon nanotube.
4. The humidity sensing fiber according to claim 3, wherein the humidity sensitive material is graphene and MXene.
5. The humidity sensing fiber according to claim 4, wherein the mass ratio of MXene to graphene is 0.01-100, preferably 1-10.
6. The humidity sensing fiber according to claim 1, wherein the polymer is selected from the group consisting of Polymethylmethacrylate (PMMA), fluororesin, PMMA composite doped with fluorinated polymer (F-PMMA), styrene-methylmethacrylate copolymer (SMMA), Cyclic Olefin Copolymer (COC), Cyclic Olefin Polymer (COP), Polycarbonate (PC), polyphenylene sulfone resin (PPSU), polyethersulfone resin (PES), Polyethyleneimine (PEI), Polystyrene (PS), Polyethylene (PE), polypropylene (PP), Polyamide (PA), Polyimide (PI), polyethylene terephthalate (PET), Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polyurethane (PU), polyvinyl chloride (PVC), and mixtures thereof, One or more than two of Polystyrene (PS), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), acrylonitrile-butadiene-styrene copolymer (ABS), polyethylene glycol (PEG), thermoplastic elastomer (TPE), low-density polyethylene (LDPE), polyethylene glycol (PEG), high-density polyethylene (HDPE), Polyformaldehyde (POM), polyphenylene oxide (PPO), polyester and sodium isophthalate sulfonate copolymer, acrylate copolymer, vinyl acetate resin and polyvinyl acetal, preferably, the first and second liquid crystal materials are, one or more selected from polyethylene terephthalate (PET), Cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), styrene-ethylene/butylene-styrene block copolymer (SEBS), Polycarbonate (PC), thermoplastic elastomer (TPE) and fluorine resin.
7. The moisture-sensing fiber of claim 1, wherein the moisture-sensing cladding layer comprises a greater mass of moisture-sensitive material than the moisture-sensing core layer.
8. Moisture-sensing fibre according to claim 7, characterised in that the mass proportion of moisture-sensitive material in the moisture-sensing envelope is between 0.01 wt.% and 40 wt.%, preferably between 20 wt.% and 40 wt.%.
9. The moisture-sensing fiber of claim 7, wherein the moisture-sensitive material in the moisture-sensing core layer is present in an amount of 0.01 wt.% to 20 wt.%.
10. A method of making a moisture-sensing fiber, comprising a process selected from the group consisting of a coextrusion process, a melt spinning process, a wet spinning process, and a heat softening and drawing process.
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