CN115467035A - Conductive yarn and preparation method thereof - Google Patents
Conductive yarn and preparation method thereof Download PDFInfo
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- CN115467035A CN115467035A CN202211087302.8A CN202211087302A CN115467035A CN 115467035 A CN115467035 A CN 115467035A CN 202211087302 A CN202211087302 A CN 202211087302A CN 115467035 A CN115467035 A CN 115467035A
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- 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
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- 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
- D01D11/00—Other features of manufacture
- D01D11/06—Coating with spinning solutions or melts
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- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- Textile Engineering (AREA)
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- General Chemical & Material Sciences (AREA)
- Multicomponent Fibers (AREA)
Abstract
The invention discloses a conductive yarn and a preparation method thereof. The conductive yarn comprises a skin layer and a core layer; the skin layer comprises a spun polymer and a conductive material; the spinning polymer comprises at least one of polyurethane, polyacrylonitrile, polylactic acid, polyvinyl alcohol, polycaprolactone, polyaniline, polyvinyl alcohol, polysulfone, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, styrene-butadiene-styrene block copolymer, hydrogenated styrene-butadiene block copolymer or derivatives thereof; the conductive material comprises at least one of carbon black, carbon fiber, carbon nano tube, graphite particle, graphene and metal powder; the conductive core layer comprises conductive fibers; the conductive fibers include at least one of metal-based conductive fibers, nanocarbon conductive fibers, and polymer conductive fibers. The conductive yarn has the advantages of high conductivity, water washing resistance, sweat immersion resistance, weaving capability and high biological safety.
Description
Technical Field
The invention relates to the technical field of conductive materials, in particular to a conductive yarn and a preparation method thereof.
Background
Along with the development of science and technology, the continuous innovation of technique, wearable fabrics of intelligence receives popular liking more and more, and in intelligent textiles, conductive fiber, yarn play vital function as the important basic material of intelligent textiles.
Most of the traditional yarns are made of insulating materials, and common fibers and yarns can also be changed into wires by using a plurality of new technologies. At present, the materials commonly used in the market for preparing conductive fibers or yarns include metal materials, conductive polymers, nanocarbon materials, and the like. In metal materials, silver-plated conductive yarns have the advantages of simple and stable preparation process, high conductivity, water washing, weaving and the like, and are widely used in the field of intelligent textile conductive yarns, but the silver is easily corroded due to long-term immersion of sweat, the conductivity is greatly reduced, and the risk of skin allergy is caused due to long-term contact, so that the silver-plated conductive yarns cannot be attached to the skin for a long time.
In conclusion, there is still a need to develop a new conductive yarn that combines the properties of high conductivity, water washing resistance, sweat immersion resistance, weaving ability, high biosafety and the like.
Disclosure of Invention
The first technical problem to be solved by the invention is as follows:
an electrically conductive yarn is provided. The conductive yarn has the advantages of high conductivity, water washing resistance, sweat immersion resistance, weaving capability and high biological safety.
The second technical problem to be solved by the invention is:
provides a preparation method of the conductive yarn.
In order to solve the first technical problem, the invention adopts the technical scheme that:
a conductive yarn comprises conductive fibers and a conductive skin layer coated on the outer surfaces of the conductive fibers;
the conductive skin layer comprises the following raw materials: spun polymers and conductive materials.
According to an embodiment of the invention, the spinning polymer comprises at least one of polyurethane, polyacrylonitrile, polylactic acid, polyvinyl alcohol, polycaprolactone, polyaniline, polyvinyl alcohol, polysulfone, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, styrene-butadiene-styrene block copolymer, hydrogenated styrene-butadiene block copolymer or a derivative thereof.
According to an embodiment of the present invention, the conductive material includes at least one of carbon black, carbon fiber, carbon nanotube, graphite particle, graphene, metal powder.
According to one embodiment of the present invention, the conductive fibers include at least one of metal-based conductive fibers, nanocarbon conductive fibers and polymer conductive fibers.
According to one embodiment of the invention, the diameter of the conductive yarn is 1-10000 μm. The diameter of the conductive yarn can be adjusted by adjusting the preparation parameters of the conductive yarn.
According to one embodiment of the invention, the diameter of the conductive yarn is 10 to 1000 μm.
According to one embodiment of the invention, the skin layer has a thickness of 1 to 10000 μm.
According to one embodiment of the invention, the thickness of the skin layer is 1-1000 μm.
According to one embodiment of the invention, the thickness of the skin layer is 100-500 μm.
Too low a thickness of the sheath results in a sheath-core yarn that does not have sweat-leaching resistance, and a high thickness improves sweat-leaching resistance.
According to one embodiment of the present invention, the mass ratio of the spinning polymer to the conductive material is 1.
According to one embodiment of the invention, the metal-based conductive fibers comprise at least one of copper-based fibers, nickel-based fibers, tungsten-based fibers, silver-based fibers, platinum-based fibers, stainless steel-based fibers, and iron-based fibers.
According to an embodiment of the present invention, the nano carbon conductive fiber includes at least one of a carbon nanotube conductive fiber, a graphene conductive fiber, and an acetylene black conductive fiber. The mass percentage of carbon in the nanocarbon conductive fibers is 100%.
According to one embodiment of the present invention, the polymer conductive fibers include at least one of polyacetylene fibers, polyaniline fibers, polythiophene fibers, and polypyrrole fibers.
According to one embodiment of the invention, the conductive yarn has at least one of the following advantages or benefits:
the conductive fibers are selected to have good conductivity; the skin layer is prepared from the following raw materials: the spinning polymer and the conductive material enable the cortex to have good biological safety and excellent mechanical property; the cortex cladding electrically conducts the sandwich layer, forms the skin core structure, avoids electrically conducting the sandwich layer and external environment contact, thereby makes electrically conducting yarn possesses high conductivity, can wash, can weave, resistant sweat soaks, biosecurity advantage such as.
In order to solve the second technical problem, the invention adopts the technical scheme that:
a method of making the conductive yarn comprising the steps of:
s1, mixing a spinning polymer and a conductive material in a solvent to obtain a spinning solution;
and S2, wrapping the spinning solution on the outer layer of the conductive fiber by adopting a wet spinning process to obtain the conductive yarn.
After the spinning polymer is dissolved in the solvent, the solvent firstly permeates into the high polymer, so that the distance between macromolecules is continuously increased, the spinning polymer is firstly swelled before being dissolved, and then is dissolved to form a uniform solution after being swelled. The swelling speed and the dissolving speed have a relationship with the viscosity of the spinning solution, which affects the wet spinning process, so in an embodiment of the present invention, the spinning polymer selected comprises at least one of polyurethane, polyacrylonitrile, polylactic acid, polyvinyl alcohol, polycaprolactone, polyaniline, polyvinyl alcohol, polysulfone, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, styrene-butadiene-styrene block copolymer, hydrogenated styrene-butadiene block copolymer or derivatives thereof, so as to adapt to the wet spinning process.
According to an embodiment of the present invention, the method for preparing the conductive yarn further comprises a step of dispersing the spinning solution through a magnetic stirrer, an ultrasonic cleaning machine and a three-roll machine. By dispersing the spinning solution, the properties of the spinning solution are uniform, gel blocks and impurities entrained therein are removed, and air bubbles in the spinning solution are removed.
According to an embodiment of the present invention, in the method for preparing the conductive yarn, the wet spinning process in step S2 specifically includes the following steps:
after the conductive fibers pass through the inner phase channel of the two-channel spinning needle head, winding is carried out;
in the winding process, the spinning solution flows out through the two-channel spinning needle head external phase channel and then wraps the outer surface of the conductive fiber, and the conductive yarn is obtained after solidification.
According to one embodiment of the invention, the curing is water bath curing.
According to one embodiment of the invention, the solvent of the spinning solution comprises at least one of N, N-dimethylformamide, N-dimethylacetamide.
According to one embodiment of the invention, the drawing speed of the conductive fibers is 0.01 to 10000m/min.
According to one embodiment of the invention, the drawing speed of the conductive fibers is 1 to 1000m/min.
According to one embodiment of the invention, the collection speed of the conductive yarn is 0.01-10000m/min. The higher the collection speed of the winder, the smaller the fiber diameter in the conductive skin. It will be appreciated that the collection speed of the conductive yarn is the collection speed of the winder.
According to one embodiment of the invention, the collection speed of the conductive yarn is 1-1000m/min.
According to one embodiment of the invention, the spinning polymer has a mass concentration of 0.1 to 50% in the spinning solution. The concentration of the spinning solution is in the range, so that the thickness of the conductive skin layer obtained by spinning is uniform.
According to one embodiment of the invention, the spinning polymer has a mass concentration of 1 to 30% in the spinning solution.
According to one embodiment of the present invention, the mass concentration of the conductive material in the spinning solution is 0.1 to 50%.
According to one embodiment of the present invention, the mass concentration of the conductive material in the spinning solution is 1 to 30%.
According to one embodiment of the present invention, the mass ratio of the spinning polymer to the conductive material in the spinning solution is 1:0.01 to 1. Outside the range, the prepared conductive yarn cannot have the performances of good conductivity, washability, knittability, sweat-immersion resistance and the like.
According to one embodiment of the present invention, the spinning solution has a mass ratio of the spinning polymer to the conductive material of 1:0.1 to 0.5.
According to one embodiment of the present invention, in the wet spinning process, the flow rate of the spinning solution is 0.01 to 10000ml/min. The invention adjusts the flow speed of the spinning solution within the range, so that the conductive sheath obtained by spinning has higher mechanical property and stronger waterproofness.
According to one embodiment of the present invention, in the wet spinning process, the flow rate of the spinning solution is 1 to 1000ml/min.
One of the technical solutions has at least one of the following advantages or beneficial effects:
the preparation method of the embodiment has the advantages of simple process, low cost, easy realization and low requirement on technical personnel.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic view of an apparatus used in wet spinning in examples 1 to 8.
Fig. 2 is an electron microscope image of the outer surface of the conductive yarn prepared in example 1.
Fig. 3 is a cross-sectional electron microscope image of the conductive yarn prepared in example 1.
FIG. 4 shows the effect of the conductive yarn prepared in example 1 on cell proliferation.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 scope of the present invention.
Example 1
A method of making an electrically conductive yarn comprising the steps of:
s1, preparing a spinning solution:
(1) Preparing a polymer solution: weighing 10ml of N, N-dimethylformamide solution and 2.581g of Polyurethane (PU), mixing the two solutions, and stirring by using a magnetic stirrer until the PU is fully dissolved;
(2) Preparing a spinning solution: weighing 0.323g of carbon black, pouring the carbon black into the polymer solution prepared in the early stage for dissolving, stirring the carbon black serving as a conductive material in the solution for 4min by using a glass rod, and then dispersing the solution for 2h by using an ultrasonic cleaning machine; further dispersing the solution by using a three-roller machine, standing the dispersed solution for half an hour, observing whether the solution is precipitated, and continuing dispersing the solution if the solution is precipitated until no precipitate is observed visually.
S2, preparing the conductive yarn by adopting a wet spinning process:
the apparatus for making the conductive yarn is shown in fig. 1;
(1) The inner phase channel of the two-channel needle head is communicated with the injector A to build an assembly device and is fixed in the water tank. The silver-plated conductive yarn sequentially passes through the injector A and the inner phase channel of the two-channel needle, and the outer phase channel of the two-channel needle is communicated with the injector B filled with the spinning solution through a polyethylene plastic pipe;
(2) The combination device, the winding rod and the winding machine are sequentially arranged at intervals in a straight line, and the silver-plated conductive yarns are drawn and wound by the winding rod and the winding machine;
(3) Opening a propeller for driving the injector B, extruding the spinning solution, stretching the inner core while propelling the spinning solution, and ensuring that the spinning solution is wrapped on the outer layer of the inner core, thereby forming a skin-core structure; the flow rate of the spinning solution is 200ml/min;
(4) And after the spinning is observed to be stable, opening a winding machine to collect the conductive yarn. The collection speed of the winder was 10m/min.
The conductive yarn prepared in example 1 had a diameter of 380 μm.
The scanning electron microscope image of the outer surface of the conductive yarn prepared in example 1 is shown in fig. 2.
A cross-sectional scanning electron micrograph of the conductive yarn prepared in example 1 is shown in fig. 3.
Example 2
Example 2 a method of preparing an electrically conductive yarn, differing from example 1 only in that: polyurethane was replaced with polyacrylonitrile.
Example 3
Example 3 a process for preparing an electrically conductive yarn, differing from example 1 only in that: polyurethane was replaced with polyvinylidene fluoride and N, N-dimethylformamide solution was replaced with N, N-dimethylacetamide.
Example 4
Example 4 a method of preparing an electrically conductive yarn, differing from example 1 only in that: the polyurethane was replaced with a styrene-butadiene-styrene block copolymer.
Example 5
Example 5 a method of preparing an electrically conductive yarn, differing from example 1 only in that: carbon black is replaced with carbon nanotubes.
Example 6
Example 6 a method of preparing an electrically conductive yarn, differing from example 1 only in that: replacing carbon black with metal powder, wherein the metal powder is mixed powder of copper, nickel, tungsten, silver, platinum and iron, and the mass ratio of the copper, the nickel, the tungsten, the silver, the platinum and the iron is 1:1:1:1:1:1.
example 7
Example 7 a method of making an electrically conductive yarn, differing from example 1 only in that: and replacing the silver-plated conductive yarn with graphene conductive fiber.
Example 8
Example 8 a method of making an electrically conductive yarn, differing from example 1 only in that: the silver-plated conductive yarn is replaced by polyacetylene conductive yarn.
And (4) performance testing:
1. sweat soak resistance test:
(1) The silver-plated yarns and the conductive yarns prepared in the embodiment 1 are divided into 5 independent groups, the length of each group of yarns is 20cm, and the yarns are marked to ensure that the resistance measured at each time is at the same position;
(2) Taking 10 parts of beakers, pouring 10ml of acidic artificial sweat (pH = 4.2) into 5 parts of beakers, pouring 10ml of alkaline artificial sweat (pH = 8.0) into the other 5 parts of beakers, respectively, soaking the silvered yarns and the conductive yarns prepared in the example 1 in the acidic artificial sweat or the alkaline artificial sweat respectively in a whole piece, stirring by using a glass rod, ensuring complete soaking, and keeping the soaking time for 30min;
(3) Taking out the yarns, and fully and naturally airing the yarns in a constant temperature and humidity chamber (the airing time is 24 hours);
(4) And (3) after the yarn is dried, observing the change of the resistance at the mark position of the yarn by using a digital source meter, and observing the change of the outer surface of the yarn. Three experiments were repeated.
The test results are shown in Table 1.
TABLE 1
2. And (3) water washing test:
a water wash was performed using the silver plated yarn and the conductive yarn prepared in example 1. The yarn appearance was observed using a microscope and resistance tested with a multimeter prior to washing. The yarn is washed with water according to the national standard of the people's republic of China, textile trial family washing and drying procedure (standard number: GB/T8629-2017), and the specific washing conditions are as follows:
(1) Washing machine specification and washing program: refer to the standard washing machine of type A2 and the washing program of program number 4H; immediately after completion of the washing procedure and carefully taking out the sample, taking care not to stretch or twist, the sample was laid flat on a horizontal screen drying rack (16 mesh, made of plastic) and dried in the shade in a static atmosphere;
(2) Specification of washing accompanying articles: reference 100% polyester fiber;
(3) Total wash load (total mass of sample and corresponding wash load): (2.0 +/-0.1) kg;
(4) Test water: the hardness of water is lower than 0.7mmol/L, which is measured according to the national standard GB/T7477 and expressed by calcium carbonate; the water supply pressure at the water filling port of the washing machine is higher than 150kPa, and the water filling temperature of the washing machine is (20 +/-5 ℃);
(5) A detergent: standard detergent 3; washing requires the addition of (20 + -1) g of standard detergent;
the one-time water washing procedure comprises one-time washing and airing. After repeating the complete washing procedure 10, 50 and 100 times, the appearance and the resistance of the two yarns were checked and tested.
The test results are shown in Table 2.
TABLE 2
3. And (3) biological safety test:
3.1 biosafety evaluations were performed on the conductive yarn prepared in example 1. The conductive yarn prepared in example 1 was not dyed, and therefore, the color fastness, the forbidden dye, and the sensitizing dye were not examined.
The specific detection items and methods are as follows:
(1) And (3) detecting the content of formaldehyde: national basic safety technical Specification for textiles (Standard No. GB/T18401-2010);
(2) The pH value; national basic safety technical Specification for textiles (Standard No.: GB/T18401-2010);
(3) Peculiar smell: national basic safety technical Specification for textiles (Standard number: GB/T18401-2010). If the peculiar smell exists, the excessive chemical substance residue is indicated on the fiber;
(4) Heavy metal content: conducting detection analysis on the conductive yarn prepared in the example 1 by using a Fourier infrared spectrometer;
(5) The fabric combustion performance: according to the American Standard ASTM D1230-94, the flame off time of plain cloth fabrics should be greater than 3.5 seconds and the flame off time of terry cloth fabrics should be greater than 7 seconds.
The test results are shown in Table 3.
TABLE 3
3.2 cell proliferation assay was performed on the conductive yarn prepared in example 1 using the CKK-8 test method.
The specific test method is as follows:
(1) Making a standard curve
1) Cell suspensions (100. Mu.L/well) were seeded in 96-well plates. A cell concentration gradient is made according to the proportion of 500, 1000, 2000, 4000, 6000 and 8000, and each group has 3-6 compound holes. The plates were incubated in an incubator (5% CO at 37% 2 Conditions) until cell adherence is complete (typically 24 hours).
2) Add 10. Mu.l of CCK-8 solution to each well (taking care not to create air bubbles in the wells which would affect the OD readings)
3) The plates were then assayed for absorbance at each cell concentration for different incubation times. The culture is generally incubated for 0h,0.5h,1h,2h,3h and 4h in an incubator for 1-4 hours.
4) Absorbance at 450nm was measured with a microplate reader, and a standard curve was drawn.
(2) Cell proliferation-toxicity assay
1) Cell suspensions (100. Mu.l/well) were seeded in 96-well plates. Placing the mating plates in an incubator for pre-incubation (5% CO at 37 ℃% 2 Conditions) until cell adherence is complete (typically 24 hours).
2) Conductive yarns (experimental material group) prepared in example 1 of different thickness were put into the culture plate to have no conductive yarn added as a blank control group. The plates were incubated in an incubator for an appropriate period of time.
3) Add 10. Mu.l of CCK-8 solution to each well (taking care not to generate bubbles in the wells which would affect the OD reading).
4) The plates were incubated for an incubation time according to a standard curve.
5) Absorbance at 450nm was measured with a microplate reader.
The test results are shown in fig. 4.
As can be seen from fig. 4, the cells grew well in the presence of the conductive yarn of example 1 over the test time range, with no significant difference from the blank control. The conductive yarn of example 1 was not cytotoxic.
The results of examples 2 to 8 are similar to example 1 and are not shown one by one to avoid redundancy.
The above description is only an example of the present invention and is not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention as described in the specification of the present invention or directly or indirectly applied to the related technical fields are included in the scope of the present invention.
Claims (10)
1. An electrically conductive yarn characterized by: the conductive fiber comprises conductive fibers and a conductive skin layer coated on the outer surfaces of the conductive fibers;
the conductive skin layer comprises the following raw materials: spun polymers and conductive materials.
2. An electrically conductive yarn as in claim 1, wherein: the spinning polymer comprises at least one of polyurethane, polyacrylonitrile, polylactic acid, polyvinyl alcohol, polycaprolactone, polyaniline, polyvinyl alcohol, polysulfone, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, styrene-butadiene-styrene block copolymer, hydrogenated styrene-butadiene block copolymer or derivatives thereof;
preferably, the conductive material comprises at least one of carbon black, carbon fiber, carbon nanotube, graphite particle, graphene, metal powder;
preferably, the mass ratio of the spinning polymer to the conductive material is 1.
3. An electrically conductive yarn as in claim 1, wherein: the conductive fibers comprise at least one of metal-based conductive fibers, nanocarbon conductive fibers and polymer conductive fibers;
preferably, the metal-based conductive fibers include at least one of copper-based fibers, nickel-based fibers, tungsten-based fibers, silver-based fibers, platinum-based fibers, stainless steel-based fibers, and iron-based fibers;
preferably, the nano carbon conductive fiber comprises at least one of a carbon nanotube conductive fiber, a graphene conductive fiber and an acetylene black conductive fiber;
preferably, the polymer conductive fibers include at least one of polyacetylene fibers, polyaniline fibers, polythiophene fibers, and polypyrrole fibers.
4. An electrically conductive yarn according to any one of claims 1 to 3, wherein: the thickness of the skin layer is 1-10000 μm.
5. An electrically conductive yarn as in any one of claims 1 to 3, wherein: the diameter of the conductive yarn is 1-10000 μm.
6. A method of making an electrically conductive yarn as claimed in claim 2 or 4 or 5, wherein: the method comprises the following steps:
s1, preparing a spinning solution containing the spinning polymer and the conductive material;
and S2, wrapping the conductive skin layer on the outer layer of the conductive fiber by adopting a wet spinning process to obtain the conductive yarn.
7. The method of claim 6, wherein: in the spinning solution, the mass ratio of the spinning polymer to the conductive material is 1:0.01 to 1.
8. The method of claim 6, wherein: in the wet spinning process, the flow rate of the spinning solution is 0.01-10000ml/min.
9. The method of claim 6, wherein: in the wet spinning process, the drafting speed of the conductive fiber is 0.01-10000m/min.
10. The method of claim 6, wherein: the collection speed of the conductive yarn is 0.01-10000m/min.
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