CN113322670A - Highly conductive organic fiber, conductive yarn, conductive fiber structure, and method for producing same - Google Patents
Highly conductive organic fiber, conductive yarn, conductive fiber structure, and method for producing same Download PDFInfo
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- 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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- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9, 10 or 18 of the Periodic System; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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Abstract
Hair brushA high-conductivity organic fibre, conductive yarn, conductive fibre structure and its preparing process are disclosed, which features that the one-dimensional conductive nano material and adhesive slurry dispersed in solvent are coated on the surface of continuous fibre, the size of the drop of said fibre is controlled to uniformly coat the surface of fibre with the liquid film and conductive layer, the thickness of conductive layer is controlled, and the adhesive layer slurry with certain conductivity and penetrability is alternatively coated on the surface of fibre, so forming a continuous adhesive layer between said adhesive layer and one-dimensional conductive nano material network, resulting high-conductivity fibre with excellent physical characteristics (antiwear nature and extension stability) and specific resistance (10)0～104Ohm/centimeter is adjustable, high-speed continuous production is realized, the problem that the existing high-conductivity fiber cannot be comprehensively provided with good conductivity, strain conductivity stability, bending resistance, abrasion resistance, low cost and high production efficiency is solved, and the high-conductivity fiber has wide application prospects in the fields of intelligent textiles, aerospace, national defense and military industry and the like.
Description
Technical Field
The invention relates to the technical field of conductive fibers, in particular to a high-conductivity organic fiber, a conductive yarn, a conductive fiber structure and a preparation method thereof.
Background
The organic fiber is endowed with high conductivity and has important application value, and various products with new performance can be manufactured in a plurality of application fields based on the conductive organic fiber, for example, in the biomedical field, the conductive fiber with good weaving performance is taken as a signal transmission line, and the garment for monitoring the physiological indexes of the human body can be manufactured to monitor the electrocardio, the blood oxygen, the blood sugar and the pulse of the human body surface in real time; in the field of consumer electronics, conductive fibers and infrared emission materials are compounded to prepare infrared emission electric heating products for electric heating clothes and indoor heating; in the field of national defense and military industry, the conductive fiber and the magnetic nano material are compounded to prepare the electromagnetic absorption material with adjustable electromagnetic absorption performance, thereby providing a basic material for electromagnetic shielding and microwave stealth. The existing metal fiber or carbon fiber is limited by poor deformation and bending resistance in different degrees, and has far lower flexibility and spinnability than organic fiber, so that the common application of common chemical fiber can not be achieved. In recent years, many people compound a new carbon-based material with an organic fiber to prepare various conductive fibers, and a typical technology is to coat graphene or carbon nanotubes on the surface of a monofilament or a bundle to form a continuous conductive layer, since the conductive phase is mixed with a polymer to reduce the conductivity, the high conductivity is achieved by simply increasing the thickness of the carbon nanotube layer, the wear resistance of the conductive layer is reduced, the bending stability is reduced, and the elongation strain resistance of the fiber is weak.
The high-performance conductive fiber has good comprehensive performance while meeting the requirement of high conductivity, and comprises the advantages of high processing efficiency, stable conductivity, certain strain tolerance, low cost, proper fineness and uniform coverage of a conductive layer on the surface of a monofilament, the uniform coating of the conductive layer on the surface of the monofilament is difficult to achieve by adopting a bundled wire impregnation method, the high conductivity and high production efficiency are difficult to achieve simultaneously by adopting a simple carbon nano tube and a bonding layer for coating, in order to increase the conductivity, the thickness of the carbon nano tube is increased, the bending resistance is reduced, a silver nano wire is used as a conductive phase, the pure silver nano wire has low elongation resistance, the conductivity is compounded with a polymer to lose, the thickness of a composite conductive layer is increased, the silver content is increased, and the large-scale use is not facilitated. Therefore, a technical route for comprehensively solving the problems of production efficiency, conductivity, mechanical property and quality stability is needed.
Disclosure of Invention
The invention aims to provide a preparation method of one-dimensional nano-material multilayer coated continuous high-conductivity organic fiber, which solves the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
compared with the prior art, the invention has the beneficial effects that: the preparation method of the one-dimensional nano material multilayer coated continuous high-conductivity organic fiber comprises the following steps:
sequentially passing the pretreated organic fiber core material through a plurality of glue pools; the diameter phi of the liquid drop at the outlet of the glue pool is less than or equal to 3D; d is the diameter of the organic fiber core material;
and the organic fiber core material is dried before or after entering the glue pool;
at least comprises two groups of glue pools: one group of glue pools is filled with conductive adhesive slurry, and the other group of glue pools is filled with one-dimensional conductive nano-material slurry.
The pretreatment here is a corona treatment in the prior art. The diameter of the liquid drops passing through the tip of the inlet and the outlet of the glue pool is controlled, so that the liquid layer thickness on the surface of the fiber is lower than the Pleteau-Rayleigh instability thickness at a certain speed (the speed is 0.1-5 m/s) under the condition that the diameter of the liquid drops is not more than 3 times of the diameter of the fiber, the discontinuous liquid drops generated by liquid film instability and the non-uniform conducting layer after drying are inhibited, the thin conducting layer is uniformly coated on the surface of the fiber, the number of layers is adjusted through repeated coating, and continuous fibers with different conductivities can be obtained.
Based on the overall concept of the invention, the method comprises the selection of materials and the control of the liquid film on the surface of the fiber during high-speed coating, thereby realizing the continuous and high-efficiency production of the high-conductivity fiber. Specifically, the method solves the inherent obstacles that the production efficiency and the conductivity cannot be simultaneously met in the existing high-conductivity fiber production technology.
Preferably, the conductive adhesive comprises the following components: one or two of waterborne polyurethane and waterborne acrylic resin, one or two of nano carbon black and mechanically stripped graphene, a defoaming agent, a wetting agent and a thickening agent;
wherein, the content of carbon black is not higher than 15%, and the content of graphene is not higher than 0.3%.
Preferably, the conductive adhesive comprises the following components: 70-80 parts of waterborne polyurethane, 10-15 parts of nano conductive carbon black, 0.1-0.3 part of mechanically-stripped graphene, 1 part of defoaming agent, 1 part of wetting agent and 1 part of thickening agent.
With regard to "conductive adhesives", in particular adhesives with conductive materials: the kind of the binder and the conductive material are not particularly limited, and here, as an example, aqueous polyurethane and aqueous acrylic resin are used; nano carbon black and mechanically stripped graphene; those skilled in the art can formulate on a routine choice. The use of "conductive adhesive" is intended to: imparting electrical conductivity to the binder. Based on the structure of the forming material, the bonding layer formed by the conductive adhesive and the conductive layer formed by the one-dimensional conductive nano material network are similar to a parallel structure (namely, the interlayer bonding is realized, and a vertical conductive path is realized), so that the conductivity is improved.
Preferably, the one-dimensional conductive nanomaterial slurry is single-walled carbon nanotube slurry or silver nanowire slurry.
Preferably, the components of the one-dimensional conductive nanomaterial slurry further include deionized water, ethanol and isopropanol.
Preferably, the one-dimensional conductive nanomaterial slurry comprises an ionic surfactant in the components. The specific implementation link is that on the basis of the scheme, a proper amount of ionic surfactant (which can be selected by a person skilled in the art, such as sodium alkenyl sulfonate or sodium dodecyl sulfate) is added into the one-dimensional conductive nano-material slurry, and the amount of the ionic surfactant is optimally kept between 10% and 20%; the one-dimensional conductive nano-material slurry has certain wettability so as to improve the combination efficiency of the one-dimensional conductive nano-material slurry and the binder, realize uniform coating (0.1-5 seconds/meter) of the conductive material under the state of rapid fiber traction, and simultaneously keep excellent conductive performance and other physical properties.
Preferably, the device also comprises another group of glue pools, wherein the glue pools are filled with a binder with infrared emission nano particles;
and/or;
a binder with magnetic nanoparticles.
Preferably, the infrared emission nanoparticles comprise one or a combination of several of metal nanoparticles, ferroferric oxide nanoparticles and tungsten-doped vanadium dioxide nanoparticles;
the magnetic nanoparticles comprise nano ferroferric oxide.
Different functional particles are combined with a binder for coating purposes to impart different functional properties to the final fiber product.
Preferably, a coaxial vertebral canal is arranged at the inlet and/or the outlet of the glue pool, and the output end of the vertebral canal is annularly provided with flexible capillary cilia; the fiber is input/output from the vertebral canal in the preparation stage, and the coaxial design is adopted, so that the fiber can smoothly pass through the vertebral canal without rubbing with the wall of the vertebral canal, and the friction loss of surface materials is avoided; the adoption of the flexible capillary cilia is convenient for accurately controlling the liquid drop, and the adoption of the mode to operate the fiber ensures that the material penetration (the adhesive and the one-dimensional conductive material layer) is uniform; the method is also suitable for the stability characteristic of high-speed fiber passing operation, and the production efficiency is improved.
Preferably, the angle of inclination of the spinal canal is 10 °, and the diameter of the exit opening of the spinal canal is 2 mm.
The composite functional clad comprises an organic fiber core material and a composite functional clad layer at least comprising a conductive layer from inside to outside, wherein the diameter of the inner core material is 30-70 micrometers, and the thickness of the composite functional clad layer is 2-4 micrometers.
Preferably, the conductive layer is a multilayer structure, and the thickness of a single layer is not more than 50 nm.
Preferably, the composite functional cladding further comprises an infrared emission characteristic layer and a magnetic layer.
Preferably, the total number of layers of the composite functional cladding is 8-30.
The organic fiber core material is continuous filament of any one of PA6, PA66, PET, PE and PP, and the diameter of the organic fiber core material is between 15D1F and 60D 1F.
The conductive yarn comprises the one-dimensional nano material and continuous high-conductivity organic fibers coated in a multi-layer mode.
The conductive fiber structure comprises the conductive yarn.
These features and advantages are described in more detail in the following figures and detailed description.
Drawings
FIG. 1 is a schematic diagram of the steps for preparing the conductive fiber of the present invention.
Fig. 2 is a schematic diagram of a flexible capillary structure according to the present invention.
FIG. 3 is a scanning electron micrograph of carbon nanotubes on the fiber surface (left), partially enlarged carbon nanotubes on the surface (upper right), and partially enlarged silver nanowires on the surface (lower right);
fig. 4 is a graph of the repetitive tensile stress-strain curve and the resistance-strain curve of a fiber monofilament.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
carrying out corona treatment on 20D1F nylon filaments produced by a melt spinning method, and then, referring to FIG. 1, carrying out primary drying (drying temperature is 110 ℃) on fibers and then feeding the fibers into a glue pool;
the glue pool of this embodiment is totally provided with 12 (named glue pool 1-glue pool 12 according to the order of fiber penetration, respectively), and divided into four groups according to the different substances (i.e. coating) therein, the first group is glue pool 1, glue pool 5, glue pool 9-glue pool 12; the coating in the conductive adhesive is a conductive adhesive, and the conductive adhesive comprises the following specific components: 70-80 parts of waterborne polyurethane, 10-15 parts of nano conductive carbon black, 0.1-0.3 part of mechanically-stripped graphene, 1 part of defoaming agent, 1 part of wetting agent and 1 part of thickening agent, and mechanically mixing;
the second group is glue pool 2-glue pool 4 and glue pool 6-glue pool 8, the coating in the glue pool is conductive nano material slurry with ionic surfactant, and the specific components are as follows: the single-wall carbon nanotube slurry is water slurry of single-wall carbon nanotube produced in Chinese academy of sciences, contains ionic surfactant and has carbon nanotube content of 0.2% and evaporated water phase concentrated to 0.8%.
With continued reference to fig. 1, a drying pipe is also installed between the glue pools for drying.
Referring to fig. 2, the inlet and outlet of the glue pool are flexible capillary cones, the inclination angle of the vertebral canal is 10 degrees, the diameter of the outlet of the vertebral canal is 2 mm, and the output end of the vertebral canal is annularly provided with flexible capillary cilia; as shown in FIG. 2, the distance between the inlet and the outlet is not less than 10 mm, the inlet and the outlet are coaxial, and the liquid in the glue pool is circulated by a positive displacement pump.
In the embodiment, the single-walled carbon nanotube slurry is adopted, a proper amount of ionic surfactant is added, a flexible capillary coating method is adopted, the diameter of the liquid drop at the tip of the fiber is brushed through controlling the fiber to penetrate through the capillary, so that the liquid layer thickness on the surface of the fiber is lower than the Pluteau-Rayleigh instability thickness at a certain speed under the condition that the diameter of the liquid drop is not more than 3 times of the diameter of the fiber, the discontinuous liquid drops generated by the instability of the liquid film and the dried conductive layer are inhibited from being uneven, the thin conductive layer is uniformly coated on the surface of the fiber, the number of layers is adjusted through repeated coating, and continuous fibers with different conductivities can be obtained.
The drying temperature of the heating pipe between the glue pools is 110-130 ℃, the fiber tension is not more than 0.01N, and the speed is not more than 0.3 m/s;
after the fiber is output from the last glue pool, the fiber is coiled after being brushed by oil, then the fiber is dried for 20 minutes at 120 ℃, and the conductivity of the monofilament of the fiber is measured, wherein the specific resistance is not higher than 20 kiloohm/cm;
in other preferred embodiments, when the number of the carbon nanotube gel pools is increased to 10, the specific resistance is not higher than 2 kilo-ohm/cm, and the total film thickness (i.e., the portion excluding the fiber core material) is not more than 3 micrometers.
Example 2: the structure in this embodiment is the same as that in embodiment 1, and includes the structure of the glue pool, the structure of the inlet and outlet of the glue pool, the structure of the drying tube, and the setting of the drying temperature.
Except for the processing flow of the fiber.
Specifically, the fiber having a specific resistance of 20 kilo-ohm obtained in example 1 after passing through the glue pool 9 and drying was wound, and then was treated as follows:
according to the mode of the embodiment shown in the figure 1, 10 glue pools, namely a glue pool I-a glue pool X, are arranged, wherein silver nanowire slurry is contained in the glue pool I-a glue pool III and the glue pool V-a glue pool VI; the silver nanowires are long nanowires prepared by a polyol method, the average diameter is less than 40 nanometers, the average length is more than 10 micrometers, the silver nanowires are dispersed in 50% deionized water, 20% ethanol and 20% isopropanol solution, and the solution contains 10-20% of ionic surfactant;
the glue bath IV and the glue bath VII-glue bath X are conductive adhesives, and the compositions are the same as in example 1.
Winding the fiber after passing through an oil brush, drying for 20 minutes at 120 ℃, measuring the conductivity of the fiber monofilament, measuring the specific resistance of the unit length not higher than 100 ohm/cm,
in another preferred embodiment of the invention, when the number of the silver nanowire glue pools is increased to 10, the specific resistance is not higher than 30 ohm/cm, and the total film thickness is not more than 4 microns.
Example 3:
the structure in this embodiment is the same as that in embodiment 1, and includes the structure of the glue pool, the structure of the inlet and outlet of the glue pool, the structure of the drying tube, and the setting of the drying temperature.
The difference is the treatment process of the fiber;
specifically, the 15D1F nylon filament produced by the melt spinning method is subjected to corona treatment. According to the form of fig. 1, the heating pipe and the glue pool are sequentially passed through.
14 glue pools are arranged, and the glue pools a-n sequentially pass through the fiber; wherein, all splendid attire has electrically conductive binder in gluing pond a, gluing pond e and gluing pond i, and its composition is: 70-80 parts of water-based acrylic resin, 10-15 parts of nano conductive carbon black, 0.1-0.3 part of mechanically-stripped graphene, 1 part of defoaming agent, 1 part of wetting agent and 1 part of thickening agent, and mechanically mixing.
The glue pools b-d and f-h are filled with the single-walled carbon nanotube slurry same as that in the embodiment 1;
the glue pool j-glue pool m is filled with the same silver nanowire slurry as in the embodiment 2, the glue pool n is filled with a water-based acrylic resin binder containing copper, zinc nanoparticles, or ferroferric oxide nanoparticles, or tungsten-doped vanadium dioxide nanoparticles, and the binder comprises 60-70 parts of water-based acrylic resin, 5-10 parts of nano conductive carbon black, 0.1-0.3 part of mechanically-exfoliated graphene, 15-20 parts of one or more of copper, zinc nanoparticles, or ferroferric oxide nanoparticles, or tungsten-doped vanadium dioxide nanoparticles, 1 part of a defoaming agent, 1 part of a wetting agent, 1 part of a thickening agent, and mechanical mixing.
In this example, an aqueous acrylic resin binder containing copper, zinc nanoparticles, or iron oxide nanoparticles, or tungsten-doped vanadium dioxide nanoparticles was added to provide a fiber with current-controlled ir emission characteristics tuning when ir-emitting nanoparticles were added.
And (3) after the fibers pass through all the glue pools, the fibers pass through an oil brush and are wound, the fibers are dried for 20 minutes at 120 ℃, the conductivity of the monofilaments of the fibers is measured, the specific resistance is not higher than 300 ohm/cm, and the total film thickness is not more than 4 micrometers.
Example 4
The structure in this embodiment is the same as that in embodiment 1, and includes the structure of the glue pool, the structure of the inlet and outlet of the glue pool, the structure of the drying tube, and the setting of the drying temperature.
The difference is the treatment process of the fiber;
carrying out corona treatment on 15D1F nylon filaments produced by a melt spinning method, and sequentially passing through a heating pipe and a glue pool according to the form shown in figure 1;
the adhesive is characterized in that 10-20 parts of waterborne polyurethane, 40-50 parts of waterborne acrylic resin, 5-10 parts of nano conductive carbon black, 0.1-0.3 part of mechanically stripped graphene, 15-20 parts of ferroferric oxide nanoparticles, 1 part of defoaming agent, 1 part of wetting agent, 1 part of thickening agent and mechanical mixing are adopted as the components of the adhesive, wherein the waterborne acrylic resin adhesive containing copper, zinc nanoparticles, or ferroferric oxide nanoparticles or tungsten-doped vanadium dioxide nanoparticles in the adhesive pool n in the embodiment 3 is replaced by the waterborne polyurethane and waterborne acrylic resin mixed adhesive containing the ferroferric oxide nanoparticles.
In the embodiment, the adjustable magnetism of the fiber is realized by adding magnetic nanoparticles (namely ferroferric oxide nanoparticles with the size less than 10 nanometers) to the fiber; the adjustability can be achieved by the degree of layering of the coating.
To sum up all the embodiments, the key of the invention, which is different from other coating methods for preparing the carbon nanotubes and the graphene conductive fibers, is that no polymer is doped into the carbon nanotube or silver nanowire slurry for improving the adhesion of the conductive layer;
referring to fig. 3, the core of improving the adhesion of the conductive layer is to control the thickness of the liquid drop so that the adhesive layer slurry with certain conductivity and permeability can penetrate into the conductive layerForming a continuous bonding layer in the gaps of the one-dimensional nano material network; adjusting the thickness of the bonding layer to ensure that the conductivity of the fiber is not too much due to the loss of the bonding layer, the thickness of the whole conductive layer is lower than 4 microns, and the specific resistance of the fiber is between dozens of ohms and thousands of ohms (100-10) by adjusting the number of layers of the carbon nano tube and the silver nano wire4Ohm/cm), the resistance is reduced by increasing the thickness of the conductive layer and the number of the silver nanowire layers, and the defects of high conductivity, wear resistance and continuity existing in continuous organic conductive fibers coated with the conductive layer are overcome.
In addition, in order to obtain functional fiber with designable performance, different nanoparticles can be added into the surface layer of the fiber, when infrared emission nanoparticles are added, the fiber has current control infrared emission characteristic adjustment, and when ferromagnetic nanoparticles are added, the fiber has current control ferromagnetic paramagnetic transition characteristic.
The final finished fiber is coated with a conductive layer, an interlayer combined conductive bonding layer (mainly composed of a conductive bonding agent) and a surface functional layer (such as an infrared emission nano layer and a magnetic layer) outside an organic fiber core material. The total number of layers is 8-30, the organic fiber core material refers to any one of continuous filaments of PA6, PA66, PET, PE and PP, the diameter is 15D 1F-60D 1F, and the thickness of other skin layers is 2-4 microns. Wherein the conductive layer has a monolayer thickness of no more than 50 nanometers.
Referring to fig. 4 again, the final finished fiber has corrosion resistance, and after being soaked in 30% saline water for 1000 hours, the resistance change is lower than 5% after being dried; the bending resistance is high, the bending curvature is 1 mm, the bending is performed for 105 times, and the resistance is increased by less than 10%; has repeated tensile strain resistance, 30 percent of stretching and 100 times of stretching, and the resistance is increased by less than 10 percent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the one-dimensional nano material multilayer coated continuous high-conductivity organic fiber is characterized by comprising the following steps of: the method comprises the following steps:
sequentially passing the pretreated organic fiber core material through a plurality of glue pools, wherein the diameter phi of liquid drops at the outlet of each glue pool is less than or equal to 3D, and D is the diameter of the organic fiber core material;
and the organic fiber core material is dried before or after entering the glue pool;
at least comprises two groups of glue pools: one group of glue pools is filled with conductive adhesive slurry, and the other group of glue pools is filled with one-dimensional conductive nano-material slurry.
2. The method for preparing one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber according to claim 1, characterized in that: the conductive adhesive slurry comprises the following components: one or the combination of the waterborne polyurethane and the waterborne acrylic resin, the nano carbon black and the mechanically exfoliated graphene, a defoaming agent, a wetting agent and a thickening agent.
3. The method for preparing one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber according to claim 1, characterized in that: the one-dimensional conductive nano-material slurry is single-walled carbon nanotube slurry or a mixed solution of silver nanowire water and isopropanol.
4. The method for preparing one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber according to claim 1 or 3, characterized in that: the components of the one-dimensional conductive nano-material slurry comprise ionic surfactants.
5. The method for preparing one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber according to claim 1, characterized in that: the device also comprises another group of glue pools, wherein the glue pools are filled with binders with infrared emission nano particles;
and/or;
a binder with magnetic nanoparticles.
6. The method for preparing one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber according to claim 1, characterized in that: the output port of the glue pool for the fiber to pass through is annularly provided with flexible capillary cilia.
7. The one-dimensional nano material multilayer coated continuous high-conductivity organic fiber is characterized in that: prepared by the preparation method of any one of claims 1 to 6;
the composite functional clad comprises an organic fiber core material and a composite functional clad layer at least comprising a conductive layer from inside to outside, wherein the diameter of the inner core material is between 30 and 70 mu m, and the thickness of the composite functional clad layer is between 2 and 4 mu m.
8. The one-dimensional nanomaterial multilayer coated continuous high-conductivity organic fiber of claim 7, characterized in that: the composite functional cladding further includes an infrared emission characteristic layer and a magnetic layer.
9. Electrically conductive yarn, its characterized in that: comprising a one-dimensional nanomaterial of claims 7-8 in the form of a multilayer coated continuous highly conductive organic fiber.
10. A conductive fiber structure characterized by: comprising the conductive yarn of claim 9.
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