CN114703555A - One-step forming batch preparation method of core-shell structure liquid metal conductive fiber - Google Patents
One-step forming batch preparation method of core-shell structure liquid metal conductive fiber Download PDFInfo
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- CN114703555A CN114703555A CN202210217600.8A CN202210217600A CN114703555A CN 114703555 A CN114703555 A CN 114703555A CN 202210217600 A CN202210217600 A CN 202210217600A CN 114703555 A CN114703555 A CN 114703555A
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
- 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
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
Abstract
The invention discloses a one-step molding batch preparation method of core-shell structure liquid metal conductive fibers, which adopts a coaxial wet spinning technology, a shell layer injector is used for extracting a polyurethane solution, and a core layer injector is used for extracting gallium-based liquid metal; starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; and starting the core layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer, thereby preparing the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane. The invention overcomes the large surface tension of the liquid metal, the prepared liquid metal conductive fiber has excellent stretchability and conductivity, the strain and the temperature can be monitored through the change of the resistance, and the human body touch sensing capability can be simulated through the change of the capacitance. Meanwhile, the conductive fiber has good electrothermal and photothermal properties and can be used as a wearable heater.
Description
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to a one-step forming batch preparation method of core-shell structure liquid metal conductive fibers.
Background
As an indispensable component in intelligent wearable electronic products, the stretchable electronic conductor has the characteristics of excellent flexibility, stretchability, light weight and the like, so that the wearable electronic products can be applied to the aspects of medical care, artificial skin, flexible sensors and the like, which cannot be realized by the current commercial wires. Unlike current rigid commercial metal wires, stretchable conductors do not restrict human activity and do not damage wearable electronics due to good stretch recovery, and therefore are receiving increasing attention.
The conductive fiber prepared by using the conductive materials such as graphene and the like has overlarge initial resistance, high energy loss and single function, and is not suitable for flexible wearable devices. Different from the traditional rigid conductive material, the emerging gallium-based liquid metal has good fluidity, lower viscosity and excellent mechanical properties, and simultaneously retains the good conductivity and heat conductivity of the metal. In addition, the gallium-based liquid metal has biocompatibility, and the direct contact with the gallium-based liquid metal does not affect health.
However, the conductive fibers prepared by using liquid metal at present all adopt unstable processes such as multi-step preparation or impregnation, for example, a hollow stretchable fiber is prepared first, then the liquid metal is injected into the fiber by injection or the like to prepare the liquid metal conductive fiber, or the surface of the stretchable fiber is treated and then the liquid metal is impregnated, the methods are often complex and cannot be formed at one time, and the prepared liquid metal still has the problem of low conductivity. Meanwhile, because the liquid metal has large surface tension, the liquid metal cannot be continuously prepared in large batch by methods such as injection and the like, because the large surface tension can make the liquid metal granular in the fiber, and the conductive layer is discontinuous.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the technical problem of providing a one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber.
The technical scheme for solving the technical problem is to provide a one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber, which is characterized by comprising the following steps of:
Compared with the prior art, the invention has the beneficial effects that:
(1) the liquid metal conductive fiber is prepared by a one-step method through a coaxial wet spinning process based on excellent fluidity and conductivity of liquid metal and high elasticity of spandex, the production process is simple and convenient, parameters are easy to control, the production rate reaches 1m/min under laboratory conditions, the requirements of industrial continuous mass production can be met, and the liquid metal conductive fiber is used for flexible intelligent wearable equipment.
(2) The invention improves the concentration of polyurethane in the spinning process, so that the shell layer has stronger mechanical property and completely wraps the liquid metal without leakage. The liquid metal in the core layer is pressed by the polyurethane from the shell layer by combining with the higher drafting speed in the preparation process, so that the higher surface tension of the liquid metal is overcome, the liquid metal is always continuous in the conductive fibers in the preparation process, and the continuous mass production of the conductive fibers is realized.
(3) The conductive fiber prepared by the invention has excellent conductivity (even if the stretching exceeds 350 percent, the conductivity can reach 3.4 multiplied by 10)4S/cm) is equivalent to the conductivity of metal, shows excellent tensile property (the maximum strain reaches 373 percent, and the maximum tensile strength reaches 5.5MPa), still has stable performance after multiple times of tensile recovery, and has good durability.
(4) The conductive fiber prepared by the invention has multiple functions, can monitor strain and temperature change, and responds to a tiny force of 0.001 cN. In the non-contact mode, the fiber can also sense objects within 40 centimeters. And has waterproof property, and can detect the movement of underwater marine fishes.
(5) The conductive fiber prepared by the method has the tensile strength of 3.6-5.5 MPa, the elongation at break of 373 percent and the conductivity of 3.4 multiplied by 104S/cm, and the response time of the sensor is 20 ms. The conductive fiber can be rapidly heated from 27.3 ℃ to 39.2 ℃ under the voltage of 0.1V, and the energy loss is small. Can release a large amount of joule heat under low voltage condition and is used as a wearable heater. Meanwhile, the temperature rise rate is obviously faster than the ambient temperature rise rate under the illumination condition.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic diagram of the process of the present invention;
FIG. 3 is a cross-sectional view of a conductive fiber prepared in example 3 of the present invention;
FIG. 4 is a graph of tensile properties of conductive fibers prepared in example 3 of the present invention;
FIG. 5 is a graph showing the electrothermal properties of the conductive fiber prepared in example 3 of the present invention;
FIG. 6 is a graph of photothermal performance of conductive fibers prepared in example 3 of the present invention;
FIG. 7 is a graph showing the temperature response of the conductive fiber prepared in example 3 of the present invention;
FIG. 8 is a graph showing the durability against resistance change of the conductive fiber prepared in example 3 of the present invention;
FIG. 9 is a graph of pressure sensor performance for conductive fibers prepared in example 3 of the present invention;
FIG. 10 is a graph of the distance sensor performance of the conductive fibers prepared in example 3 of the present invention.
Detailed Description
Specific examples of the present invention are given below. The specific examples are only intended to illustrate the invention in further detail and do not limit the scope of protection of the claims of the present application.
The invention provides a one-step forming batch preparation method (method for short) of core-shell structure liquid metal conductive fibers, which is characterized by comprising the following steps:
preferably, step 1 is specifically: adding polyurethane particles and a solvent into a reaction container, putting magnetons into the reaction container for sealing treatment, then placing the sealed reaction container into a water bath kettle at 50-80 ℃ for slowly heating, and stirring for 4-6 hours by using a magneton stirring device to form a uniform solution, thereby obtaining a polyurethane solution;
preferably, in step 1, the solvent is a solvent capable of dissolving polyurethane, specifically N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), or Dimethylsulfoxide (DMSO).
Preferably, in step 1, the concentration of the polyurethane solution is 10 to 30 wt% (preferably 20 to 30 wt%).
Preferably, in step 2, the coagulation bath is deionized water; the gallium-based liquid metal is gallium indium tin liquid metal.
Preferably, in step 2, the parameters of the wet spinning are as follows: the extrusion speed of the polyurethane solution is 15-60 ml/h, the extrusion speed of the gallium-based liquid metal is 10-30 ml/h, and the ratio of the extrusion speeds of the polyurethane solution and the gallium-based liquid metal meets 1.5-2: 1; the drafting speed of the collecting roller is 15-40 mm/s, the drafting speed of the stretching roller is 10-20 mm/s, and the ratio of the drafting speeds of the collecting roller and the stretching roller satisfies 1.3-2: 1.
Preferably, the method further comprises step 3, post-processing: and (3) naturally airing the conductive fiber prepared in the step (2) or putting the conductive fiber into an oven for drying to remove the coagulating bath on the surface of the polyurethane shell layer and the solvent possibly remained in the polyurethane shell layer.
Preferably, in the step 3, the natural drying time is 6-12 h; the drying temperature of the drying oven is 30-40 ℃, and the drying time is 1-3 h.
In the following examples, the electrical conductivity of the conductive fibers was calculated by measuring the resistance of the conductive fibers using an LCR digital bridge. The method for testing the strength and the elongation at break is a universal tester tensile test, the gauge length is 15cm, and the tensile speed is 50 mm/min.
Example 1
adjusting spinning parameters of wet spinning equipment, wherein the extrusion speeds of the polyurethane solution and the liquid metal are respectively 30ml/h and 15ml/h, the drafting speed of a drawing roller is 10mm/s, and the drafting speed of a collecting roller is 15 mm/s;
starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; then starting the nuclear layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer; the two injection pumps extrude the polyurethane solution and the liquid metal through the coaxial spinning needle at the same time by using different pushing speeds, and the polyurethane solution and the liquid metal are finally collected by a winding roller through a deionized water coagulating bath and a stretching roller to prepare the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane.
And step 3, post-treatment: and (3) naturally airing the conductive fibers prepared in the step (2).
The prepared conductive fiber is of a core-shell structure, the durability is good, the stability is good, the maximum strain can reach 365%, and the tensile strength can reach 5.1 MPa. Meanwhile, the conductive fiber has multiple functions, has excellent electrothermal and photothermal properties and can respond to temperature, pressure and the distance between adjacent conductors.
Example 2
adjusting spinning parameters of wet spinning equipment, wherein the extrusion speeds of the polyurethane solution and the liquid metal are respectively 30ml/h and 15ml/h, the drafting speed of a drawing roller is 10mm/s, and the drafting speed of a collecting roller is 15 mm/s;
starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; then starting the nuclear layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer; the two injection pumps extrude the polyurethane solution and the liquid metal through the coaxial spinning needle at the same time by using different pushing speeds, and the polyurethane solution and the liquid metal are finally collected by a winding roller through a deionized water coagulating bath and a stretching roller to prepare the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane.
And step 3, post-treatment: and (3) naturally airing the conductive fibers prepared in the step (2).
The prepared conductive fiber is of a core-shell structure, the durability is good, the stability is good, the maximum strain can reach 347%, and the tensile strength can reach 4.2 MPa. Meanwhile, the conductive fiber has multiple functions, has excellent electrothermal and photothermal properties and can respond to temperature, pressure and the distance between adjacent conductors.
Example 3
adjusting spinning parameters of wet spinning equipment, wherein the extrusion speeds of the polyurethane solution and the liquid metal are respectively 50ml/h and 25ml/h, the drafting speed of a drawing roller is 15mm/s, and the drafting speed of a collecting roller is 20 mm/s;
starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; then starting the nuclear layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer; the two injection pumps extrude the polyurethane solution and the liquid metal through the coaxial spinning needle at the same time by using different pushing speeds, and the polyurethane solution and the liquid metal are finally collected by a winding roller through a deionized water coagulating bath and a stretching roller to prepare the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane.
And step 3, post-treatment: and (3) naturally airing the conductive fibers prepared in the step (2).
As can be seen from FIG. 3, the prepared liquid metal conductive fiber is coaxially placed in the core-shell structure, and the polyurethane of the shell layer completely wraps and protects the liquid metal of the core layer from leakage, so that high stretchability and recoverability are provided for the conductive fiber. The liquid metal of the core layer provides the conductive fibers with extremely high electrical conductivity.
As can be seen from FIG. 4, the prepared liquid metal conductive fiber has excellent mechanical properties, the maximum strain of the prepared liquid metal conductive fiber can reach 373%, and meanwhile, the tensile strength of the prepared liquid metal conductive fiber can reach 5.5 MPa.
As can be seen from fig. 5, the prepared liquid metal conductive fiber has excellent electrothermal performance, and the temperature of the conductive fiber increases with the increase of the applied direct current voltage, and reaches 85.2 ℃ when the applied voltage is 0.6V. The temperature of the conductive fiber can be increased to 39.2 ℃ at an ambient temperature of 27.1 ℃ even at a voltage of 0.1V, and good heating performance is shown at low power consumption.
As can be seen from FIG. 6, the prepared liquid metal conductive fiber has excellent photo-thermal performance, and the temperature is rapidly increased under the irradiation of an infrared lamp, and the temperature increase rate is faster than the temperature increase of the environment.
As can be seen from FIG. 7, the prepared liquid metal conductive fiber has good response to temperature change, the temperature change at 30-60 ℃ can be monitored, and the resistance of the conductive fiber is increased along with the temperature increase.
As can be seen from FIG. 8, the prepared liquid metal conductive fiber has good durability and good stability, and the electrical signal output is still stable after more than 5000 times of cycle tests at the frequency of 3 Hz.
As can be seen from fig. 9, the prepared liquid metal conductive fiber has good response to pressure changes, and the capacitance formed by the conductive fiber gradually increases as the pressure increases.
As can be seen from fig. 10, the prepared liquid metal conductive fiber has good response to the conductor within the distance range of 40cm, and the capacitance gradually increases as the capacitance distance formed by the conductor from the liquid metal conductive fiber increases. In the non-contact mode, the fiber can also sense objects within 40 centimeters.
Example 4
adjusting spinning parameters of wet spinning equipment, wherein the extrusion speeds of the polyurethane solution and the liquid metal are respectively 30ml/h and 15ml/h, the drafting speed of a drawing roller is 10mm/s, and the drafting speed of a collecting roller is 20 mm/s;
starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; then starting the nuclear layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer; the two injection pumps extrude the polyurethane solution and the liquid metal through the coaxial spinning needle at the same time by using different pushing speeds, and the polyurethane solution and the liquid metal are finally collected by a winding roller through a deionized water coagulating bath and a stretching roller to prepare the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane.
And step 3, post-treatment: and (3) naturally airing the conductive fibers prepared in the step (2).
The prepared liquid metal conductive fiber is of a core-shell structure, the durability is good, the stability is good, the maximum strain can reach 356%, and the tensile strength can reach 4.4 MPa. Meanwhile, the conductive fiber has multiple functions, has excellent electrothermal and photothermal properties and can respond to temperature, pressure and the distance between adjacent conductors.
TABLE 1 Properties of conductive fibers prepared in examples 1-4
| Examples | Conductivity of conductive fiber | Elongation of conductive fiber | Tensile strength of conductive fiber |
| Example 1 | 2.7×104S/cm | 365％ | 5.1MPa |
| Example 2 | 3×104S/cm | 347％ | 4.2MPa |
| Example 3 | 2.5×104S/cm | 373％ | 5.5MPa |
| Example 4 | 3.4×104S/cm | 356％ | 4.4MPa |
Nothing in this specification is said to apply to the prior art.
Claims (10)
1. A one-step forming batch preparation method of core-shell structure liquid metal conductive fibers is characterized by comprising the following steps:
step 1, adding polyurethane into a solvent, sealing and magnetically stirring until a uniform solution is formed, and obtaining a polyurethane solution;
step 2, adopting a coaxial wet spinning technology, extracting the polyurethane solution obtained in the step 1 by using a shell layer injector, and extracting gallium-based liquid metal by using a core layer injector; respectively and correspondingly connecting the shell layer injector and the nuclear layer injector with an outer layer needle head and an inner layer needle head of the coaxial spinning needle head and respectively fixing the shell layer injector and the nuclear layer injector in respective injection pumps; starting spinning, starting a shell injection pump, extruding a polyurethane solution through the injection pump, and solidifying the polyurethane solution through a coagulating bath; then starting the nuclear layer injection pump to ensure that the liquid metal is hermetically wrapped in the polyurethane shell layer; the two injection pumps extrude the polyurethane solution and the liquid metal through the coaxial spinning needle at the same time by using different pushing speeds, and the polyurethane solution and the liquid metal are finally collected by a winding roller through a coagulating bath and a drawing roller to prepare the core-shell structure liquid metal conductive fiber with the core layer of the liquid metal and the shell layer of the polyurethane.
2. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, wherein in the step 1, the concentration of the polyurethane solution is 10-30 wt%.
3. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1 or 2, wherein in the step 1, the concentration of the polyurethane solution is 20-30 wt%.
4. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, wherein in the step 1, the temperature of sealing and magnetic stirring is 50-80 ℃ for 4-6 h; the solvent is a solvent capable of dissolving the polyurethane.
5. The one-step forming batch preparation method of core-shell structure liquid metal conductive fibers according to claim 1, wherein in step 2, the coagulation bath is deionized water.
6. The one-step forming batch preparation method of core-shell structure liquid metal conductive fibers according to claim 1, wherein in the step 2, the gallium-based liquid metal is gallium indium tin liquid metal.
7. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, wherein in the step 2, parameters of wet spinning are as follows: the extrusion speed of the polyurethane solution is 15-60 ml/h, the extrusion speed of the gallium-based liquid metal is 10-30 ml/h, and the ratio of the extrusion speeds of the polyurethane solution and the gallium-based liquid metal meets 1.5-2: 1.
8. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, wherein in the step 2, parameters of wet spinning are as follows: the drawing speed of the collecting roller is 15-40 mm/s, the drawing speed of the drawing roller is 10-20 mm/s, and the ratio of the drawing speeds of the collecting roller and the drawing roller satisfies 1.3-2: 1.
9. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, characterized by further comprising the following steps of 3, post-treatment: and (3) naturally airing the conductive fiber prepared in the step (2) or putting the conductive fiber into an oven for drying to remove the coagulating bath on the surface of the polyurethane shell layer and the solvent possibly remained in the polyurethane shell layer.
10. The one-step forming batch preparation method of the core-shell structure liquid metal conductive fiber according to claim 1, wherein in the step 3, the natural air drying time is 6-12 hours; the drying temperature of the drying oven is 30-40 ℃, and the drying time is 1-3 h.
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| CN115522280A (en) * | 2022-09-05 | 2022-12-27 | 东华大学 | Method for preparing fiber with liquid metal core by utilizing melt spinning |
| CN115559019A (en) * | 2022-09-30 | 2023-01-03 | 苏州大学 | Elastic piezoresistive strain sensing fiber and preparation method and application thereof |
| CN115613346A (en) * | 2022-11-25 | 2023-01-17 | 吴江福华织造有限公司 | Functional fiber with ultraviolet resistance and antibacterial performance, and preparation method and application thereof |
| CN115652624A (en) * | 2022-11-17 | 2023-01-31 | 四川大学 | Preparation method of conductive fabric of high-voltage electrostatic protective clothing |
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| CN115233335A (en) * | 2022-09-01 | 2022-10-25 | 青岛大学 | Flexible liquid metal/seaweed composite fiber and preparation method thereof |
| CN115233335B (en) * | 2022-09-01 | 2024-01-26 | 青岛大学 | Flexible liquid metal/seaweed composite fiber and preparation method thereof |
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| CN116905118B (en) * | 2022-11-25 | 2024-04-26 | 吴江福华织造有限公司 | Preparation method of functional fiber |
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