CN115233335A - Flexible liquid metal/seaweed composite fiber and preparation method thereof - Google Patents
Flexible liquid metal/seaweed composite fiber and preparation method thereof Download PDFInfo
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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
-
- 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
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of liquid metal composite fiber preparation, and relates to a flexible liquid metal/seaweed composite fiber and a preparation method thereof, wherein liquid metal or liquid metal of composite magnetic particles is dispersed into an alginate aqueous solution to prepare a spinning solution; then spinning the spinning solution by a wet spinning technology to obtain flexible liquid metal/seaweed composite fibers; magnetic particles and liquid metal are uniformly distributed in the alginate fibers in a micro-nano level, the content is adjustable, and the stability is good; the flexible liquid metal/seaweed composite fiber has the advantages of ingenious overall idea design, simplicity in operation and low operation cost, is suitable for large-scale production, has magnetism, electromagnetic shielding performance and flame retardant performance, and is suitable for being used in the aspects of electromagnetic radiation resistant clothing and fabrics, particularly military clothes and the like.
Description
The technical field is as follows:
the invention belongs to the technical field of liquid metal composite fiber preparation, and relates to a flexible liquid metal/seaweed composite fiber and a preparation method thereof.
Background art:
with the development of 5G technology, the number of electronic devices is increasing, and the problem of electromagnetic pollution is becoming more and more serious. Electromagnetic pollution not only interferes electronic equipment and easily causes accidents, but also damages the reproductive system, the immune system and the nervous system of a human body, and can directly influence the development of brain tissues and even induce serious diseases such as cancers and the like in severe cases. The liquid metal is used as a good conductor material, has flexibility and high electromagnetic shielding performance, and has wide market prospect in the field of flexible wearable intelligent materials. The fiber with electromagnetic shielding performance prepared by using the liquid metal has important theoretical significance and practical value.
The liquid metal has good fluidity and higher surface tension (for example, the surface tension of the gallium-indium alloy is 624mN m -1 ) Which makes it difficult to attach or to complex with the fibers on the fiber fabric to achieve the preparation of the functionalized liquid metal fibers. The processing performance of the fiber material is generally improved by filler doping or structural design, so that the liquid metal-based fiber material is constructed. For example in literature (ACS Applied Materials)&Interfaces,2020 12 (5), 6112-6118) use high viscosity polymethacrylate as a binder for connecting liquid metal and polyurethane fibers to construct liquid metal coated fibers, although the attachment of the liquid metal to the fibers is achieved, the liquid metal coating is easily adhered to any other contacted object, which results in the contamination of adjacent objects, and the liquid metal is easily peeled off, which is poor in stability. Literature (Advanced Functional Materials,2013,23, 2308-2314) injecting liquid metal into the thermoplastic elastomer hollow fiber formed by melt processing to obtain conductive liquid metal elastic fiber, but the conductive fiber can cause uneven distribution of the liquid metal due to the stretching and rebounding of the material, and the liquid metal is easy to leak; the literature (Science Advances,2021, 2027 eabg 4041) prepares a liquid metal sheath-core composite fiber by using a coaxial wet spinning method, the sheath of the fiber mainly comprises a fluorine-containing elastomer with good elasticity, the core is a composite material of the fluorine elastomer and liquid metal nanoparticles, although the liquid metal and the fiber are compounded, the fiber has poor comfort and is difficult to biodegrade, and the problems of complex operation, complex process, high cost and the like exist, so the fiber has certain limitation in the application process.
The patent document No. CN 113527733A published Japanese 2021-10-22 discloses a liquid metal fiber/elastomer flexible composite material, a preparation method and application thereof, the invention directly adds liquid metal (pure metal or metal alloy with the melting point lower than 30 ℃) into elastomer solution, the liquid metal forms strip-shaped fiber to be distributed in the elastomer through magnetic stirring, and the composite material is obtained through heating and curing, but the preparation process of the invention is complex, and the used solvent has toxicity.
At present, in the prior art, no method for directly preparing liquid metal composite fibers by using liquid metal or liquid metal of composite magnetic particles and a single high polymer material exists.
The invention content is as follows:
in order to overcome the defects of the prior art, the invention provides the flexible liquid metal/seaweed composite fiber which is simple to operate and the preparation method thereof.
In order to achieve the above objects, the present invention provides a flexible liquid metal/seaweed composite fiber, the main structure of which is that liquid metal and/or magnetic particles are uniformly distributed inside and on the surface of the seaweed fiber.
The invention also provides a preparation method of the flexible liquid metal/seaweed composite fiber, which comprises the steps of firstly dispersing the liquid metal or the liquid metal of the composite magnetic particles into alginate solution to prepare spinning solution; and spinning the spinning solution by a wet spinning technology, feeding the spinning solution into a coagulating bath for forming after spinning, and then sequentially drawing, washing and drying to obtain the flexible liquid metal/seaweed composite fiber.
The preparation method comprises the following specific steps:
(1) Dispersing liquid metal or liquid metal of the composite magnetic particles into an alginate solution to obtain liquid metal dispersion liquid serving as a wet spinning solution;
(2) Spinning the spinning solution obtained in the step (1), and then entering a coagulating bath for forming to obtain nascent fiber;
(3) And (3) drafting, washing and drying the nascent fiber to obtain the flexible liquid metal/seaweed composite fiber with magnetism and electromagnetic shielding performance.
The alginate is sodium alginate, and the mass percentage concentration of the sodium alginate aqueous solution is 1-8%.
The liquid metal is selected from gallium (Ga) or low melting point alloys of Ga with other metals (In, sn, zn, bi, etc.), preferably gallium indium alloy (Ga 75wt%, in 25wt%, melting point 15.9 ℃).
The preparation method of the liquid metal of the composite magnetic particle comprises the following steps: adding magnetic particles such as iron, nickel or ferric oxide into liquid metal, preferably nickel particles; uniformly mixing in a vortex manner, wherein the mixing speed is preferably 2000-2500 rpm, and the mixing time is more than 3min, preferably 5-20min; and preparing the liquid metal of the composite magnetic particles.
The content of the magnetic particles in the liquid metal of the composite magnetic particles is preferably 50wt%.
The method for dispersing the liquid metal into the solution in the step (1) is an existing method such as ultrasonic crushing, mechanical stirring, grinding or microchannel extrusion, and the like, and the method for dispersing the liquid metal by ultrasonic is preferred.
The content of liquid metal in the spinning solution is preferably 1wt% to 6wt%.
The specific steps of the step (1) are as follows: ultrasonically dispersing liquid metal or liquid metal of the composite magnetic particles into a sodium alginate solution to obtain a liquid metal dispersion solution, and ultrasonically dispersing in an ice-water bath at low temperature (0-50 ℃) for more than 2min, preferably 10-60min.
In the method, the step (2) comprises the following specific steps: injecting the spinning solution into a coagulating bath through a needle tube injector or a wet spinning machine to obtain nascent fibers; the extrusion speed of the nascent fiber is 1.8-5.3m/min, and the draft ratio is 120-200%; the coagulating bath is calcium chloride water solution, and the concentration of the calcium chloride water solution is 1-5 wt%, and the preferred concentration is 4wt%.
The nascent fiber obtained by the invention is washed and dried after being soaked in deionized water or ethanol (50-95%) for 30min, wherein the drying method comprises the following steps: natural drying, heat drying, vacuum freeze drying, etc., preferably freeze drying.
In the present invention, wt% means mass%.
Compared with the prior art, the invention has the following advantages:
(1) According to the invention, sodium alginate is used as a liquid metal dispersing agent, so that the effect of solvent dispersion and the protective effect of microgel shell layer formation are achieved, and the liquid metal dispersion liquid with controllable metal particles and good stability is obtained by dispersion, so that the uniformly distributed liquid metal-sodium alginate spinning solution is obtained, and the flexible liquid metal/seaweed composite fiber is obtained;
(2) Compared with the method of directly coating on the surface of the fiber, the method has the advantages that liquid metal drops are uniformly dispersed in the fiber, the stability is high, and the like;
(3) Compared with the liquid metal fiber prepared by using the liquid metal encapsulated in the elastomer and the coaxial wet spinning, the invention has the characteristics of strong wearing comfort, biodegradability, environment-friendly and pollution-free used materials and the like.
In conclusion, the metal is uniformly distributed in the alginate fibers in a micro-nano level, the content is adjustable, and the stability is good; the flexible liquid metal/seaweed composite fiber has the advantages of ingenious overall concept design, simple operation and low operation cost, is suitable for large-scale production, has magnetism, electromagnetic shielding performance and flame retardant performance, and is suitable for being used in the aspects of electromagnetic radiation resistant clothes and fabrics, particularly military clothes and the like; can also be used as medical material.
Description of the drawings:
FIG. 1 is a surface SEM representation of the composite fiber obtained in example 1 according to the present invention.
FIG. 2 is a schematic cross-sectional SEM representation of the composite fiber obtained in example 2 according to the present invention.
FIG. 3 is a schematic diagram of the apparent morphology of the composite fiber obtained in example 3 according to the present invention.
FIG. 4 is a schematic diagram showing the results of the electromagnetic shielding performance test of the composite fiber obtained in example 3 and the pure alginate fiber according to the present invention.
FIG. 5 is a graph showing the results of the flame retardant property test of the composite fiber obtained in example 3 according to the present invention.
FIG. 6 is a schematic diagram of the apparent morphology of the composite fiber obtained in example 4 according to the present invention.
FIG. 7 is a graph showing the results of magnetic characterization of the composite fiber obtained in example 4 according to the present invention.
The specific implementation mode is as follows:
the invention is further illustrated by the following specific examples in combination with the accompanying drawings.
Example 1:
the embodiment relates to a preparation method of a flexible liquid metal/seaweed composite fiber with electromagnetic shielding performance, which specifically comprises the following steps:
(1) Adding 6g of sodium alginate into 300mL of deionized water, mechanically stirring for 1h at the speed of 500 revolutions/min to obtain a uniform 2wt% sodium alginate solution, taking out 10mL of sodium alginate solution, and placing the solution into a 20mL sample bottle for later use;
(2) Adding 150mg of gallium-indium alloy into 10mL of 2wt% sodium alginate solution obtained in the step (1), and performing ultrasonic treatment for 15min by using an ultrasonic crushing instrument with the power of 900W under the condition of ice-water bath to obtain a liquid metal-sodium alginate dispersion spinning solution; in the gallium-indium alloy, the mass percent content of gallium (Ga) is 75%, the mass percent content of indium (In) is 25%, and the melting point of the gallium-indium alloy is 15.9 ℃;
(3) 2mL of the spinning solution is extracted by using a 2.5mL needle tube, a 0.5mm needle head is used for uniformly and rapidly injecting a 3wt% calcium chloride aqueous solution to form fibers, the fibers are crosslinked and formed in the calcium chloride solution for 10min to obtain nascent fibers, the nascent fibers are placed into deionized water for soaking for 10min for washing, and the nascent fibers are taken out and wound on a bobbin or a glass rod bracket to obtain formed fibers;
(4) And (4) naturally drying the formed fiber obtained in the step (3) at room temperature to obtain the seaweed composite fiber with uniformly dispersed liquid metal, namely the flexible liquid metal/seaweed composite fiber.
In this example, the surface morphology of the obtained composite fiber is characterized by SEM, and as shown in fig. 1, the liquid metal particles dispersed by ultrasound are uniformly distributed on the surface of the fiber, and the result shows that the liquid metal/seaweed composite fiber is successfully prepared in this example.
Example 2:
the embodiment relates to a preparation method of a flexible liquid metal/seaweed composite fiber, which specifically comprises the following steps:
(1) Adding 18g of sodium alginate into 300mL of deionized water, mechanically stirring for 3h at the speed of 500 r/min to obtain a uniform 6wt% sodium alginate solution, and respectively taking out 7mL of sodium alginate solution and 21mL of sodium alginate solution for later use;
(2) Adding 840mg gallium indium alloy into 7mL 6wt% sodium alginate solution, and then carrying out ultrasonic treatment for 25min by using an ultrasonic crusher with power of 900W under the condition of ice water bath to obtain liquid metal dispersion liquid; in the gallium-indium alloy, the mass percent content of gallium (Ga) is 75%, the mass percent content of indium (In) is 25%, and the melting point of the gallium-indium alloy is 15.9 ℃;
(3) Mixing the sodium alginate solution of the step (1) with the liquid metal dispersion liquid obtained in the step (2) in a 50mL beaker, and magnetically stirring for 10min at the speed of 800 revolutions per minute to obtain a liquid metal-sodium alginate spinning solution;
(4) 2mL of spinning solution is extracted by a 2.5mL needle tube, a 0.5mm needle head is used for uniformly and rapidly injecting 3.5wt% calcium chloride aqueous solution to form fibers, the fibers are crosslinked and formed in the calcium chloride solution for 10min to obtain nascent fibers, then the nascent fibers are put into deionized water for soaking for 10min for washing, and the nascent fibers are taken out and wound on a bobbin or a glass rod bracket to obtain formed fibers;
(5) And (4) freezing the molded fiber obtained in the step (4) and then carrying out freeze drying by using a freeze dryer to obtain the seaweed composite fiber with uniformly dispersed liquid metal, namely the flexible liquid metal/seaweed composite fiber.
In this example, SEM characterization of the cross section of the obtained composite fiber was performed, and as shown in FIG. 2, the liquid metal particles dispersed by ultrasound were embedded in the fiber, which indicates that this example successfully produces the liquid metal/seaweed composite fiber.
Example 3:
the embodiment relates to a preparation method of flexible liquid metal/seaweed composite fibers, which specifically comprises the following steps:
(1) Adding 24g of sodium alginate into 400mL of deionized water, mechanically stirring for 3h at the speed of 500 r/min to obtain uniform 6wt% sodium alginate solution, and respectively taking out 100mL of sodium alginate solution and 300mL of sodium alginate solution for later use;
(2) Taking 100mL of a sodium alginate solution of 6wt% in the step (1), equally dividing into 6 parts, adding 2g of gallium-indium alloy into each part, carrying out ultrasonic treatment on each part for 30min under the condition of ice-water bath by using an ultrasonic crusher with the power of 900W, and finally mixing 6 parts completely to obtain a liquid metal dispersion liquid;
(3) Mixing the 300mL of sodium alginate solution obtained in the step (1) and the liquid metal dispersion liquid obtained in the step 2) in a 500mL beaker, and mechanically stirring at the speed of 800 revolutions per minute for 30min to obtain a liquid metal-sodium alginate spinning solution;
(4) Placing the liquid metal-sodium alginate spinning solution obtained in the step (3) into a spinning tank, standing and defoaming for 12h, taking 3000mL of 4wt% calcium chloride aqueous solution as a coagulation bath, taking 3000mL of deionized water as a stretching bath, feeding the spinning solution into a wet spinning machine through a spinning nozzle, solidifying in the calcium chloride coagulation bath, and stretching in the deionized water stretching bath to obtain nascent fibers;
(5) Freezing the fiber obtained in the step 4), and drying by using a freeze dryer to obtain the flexible liquid metal/seaweed composite fiber.
The results of the electromagnetic radiation resistance test of the seaweed composite fiber and the pure seaweed fiber are shown in fig. 4, the EMI SE of the seaweed composite fiber under the frequency of 8GHz-18GHz exceeds 17dB, and the EMI SE of the pure seaweed fiber under the frequency of 8GHz-18GHz does not exceed 2dB, which indicates that the seaweed fiber has excellent electromagnetic shielding performance due to the addition of the liquid metal.
The obtained seaweed composite fiber is subjected to a combustion test, the test result is shown in figure 5, only a small amount of sparks are generated after flame is removed after 7s of ignition, and the flame is completely extinguished after 0.3s, and the test result shows that the seaweed fiber obtained by the invention has a flame retardant property.
Example 4:
the embodiment relates to a preparation method of flexible liquid metal/seaweed composite fibers, which specifically comprises the following steps:
(1) Adding 24g of sodium alginate into 400mL of deionized water, mechanically stirring for 3h at the speed of 500 r/min to obtain uniform 6wt% sodium alginate solution, and respectively taking out 100mL of sodium alginate solution and 300mL of sodium alginate solution for later use;
(2) Mixing 6.5g of gallium-indium alloy and 6.5g of nickel particles in a centrifugal tube, and mixing for 20min at the speed of 2500 rpm by using a vortex mixer to obtain composite liquid metal;
(3) Taking 100mL of a 6wt% sodium alginate solution obtained in the step (1), equally dividing into 6 parts, adding 2g of the composite liquid metal obtained in the step (2) into each part, carrying out ultrasonic treatment on each part for 30min under the condition of ice-water bath by using an ultrasonic crusher with the power of 900W, and finally completely mixing to obtain a liquid metal dispersion liquid;
(4) Mixing the 300mL of sodium alginate solution obtained in the step (1) and the liquid metal dispersion liquid obtained in the step (3) in a 500mL beaker, and magnetically stirring for 30min at the speed of 800 revolutions per minute to obtain a liquid metal-sodium alginate spinning solution;
(5) Placing the liquid metal-sodium alginate spinning solution obtained in the step (4) into a spinning tank, standing and defoaming for 12h, taking 3000mL of 4wt% calcium chloride aqueous solution as a coagulating bath and 3000mL of deionized water as a stretching bath, and allowing the spinning solution to enter room temperature through a wet spinning machine through a spinning jet, solidifying in the calcium chloride coagulating bath and stretching in the deionized water stretching bath to obtain nascent fiber;
6) Freezing the fiber obtained in the step 5), and drying by using a freeze dryer to obtain the final flexible liquid metal/seaweed composite fiber.
The obtained composite fiber is subjected to magnetic characterization, and the result is shown in fig. 7, the obtained flexible liquid metal/seaweed composite fiber can be woven into a certain shape and can be stably attracted to a magnet under both vertical and horizontal conditions, and the test result shows that the seaweed fiber obtained in the embodiment has good magnetism.
Claims (9)
1. The flexible liquid metal/seaweed composite fiber is characterized in that the main structure of the flexible liquid metal/seaweed composite fiber is that liquid metal and/or magnetic particles are uniformly distributed in the seaweed fiber and on the surface of the seaweed fiber.
2. A method for preparing flexible liquid metal/seaweed composite fiber is characterized in that liquid metal or liquid metal of composite magnetic particles is dispersed into alginate aqueous solution to prepare spinning solution; and spinning the spinning solution by a wet spinning technology to obtain the flexible liquid metal/seaweed composite fiber.
3. The method for preparing the flexible liquid metal/seaweed composite fiber according to claim 2, characterized in that the method comprises the following steps:
(1) Dispersing liquid metal or liquid metal of the composite magnetic particles into an alginate aqueous solution to obtain liquid metal dispersion liquid serving as a wet spinning solution;
(2) Spinning the spinning solution obtained in the step (1), and then entering a coagulating bath for forming to obtain nascent fiber;
(3) And (3) drafting, washing and drying the nascent fiber to obtain the flexible liquid metal/seaweed composite fiber with magnetism and electromagnetic shielding performance.
4. The method for preparing the flexible liquid metal/seaweed composite fiber according to claim 2, wherein the alginate is sodium alginate, and the mass percentage concentration of the sodium alginate aqueous solution is 1% -8%.
5. The method as claimed in claim 2, wherein the liquid metal is gallium or a low melting point alloy containing gallium.
6. The method for preparing the flexible liquid metal/seaweed composite fiber according to claim 5, wherein the low melting point alloy is gallium indium alloy, wherein gallium accounts for 75% by mass, indium accounts for 25% by mass, and the melting point of the gallium indium alloy is 15.9 ℃.
7. The method for preparing flexible liquid metal/seaweed composite fiber according to claim 2, wherein the method for preparing the liquid metal of the composite magnetic particle comprises: adding magnetic particles into liquid metal, and mixing uniformly by vortex at a mixing speed of 2000-2500 rpm for 5-20min; the magnetic particles are iron, nickel or iron oxide.
8. The method of claim 2, wherein the spinning dope contains liquid metal in an amount of 1wt% to 6wt%.
9. The method of claim 3, wherein the extrusion speed of the nascent fiber in step (2) is 1.8-5.3m/min, and the draw ratio is 120-200%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115976689A (en) * | 2023-01-03 | 2023-04-18 | 青岛大学 | Preparation method of algal polysaccharide composite functional fiber |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624833A (en) * | 2016-03-03 | 2016-06-01 | 青岛大学 | Preparation method of magnetic alginate fiber |
| CN109338716A (en) * | 2018-09-28 | 2019-02-15 | 成都新柯力化工科技有限公司 | A kind of fibrous composite and preparation method for robot electronic skin |
| CN112647156A (en) * | 2020-12-21 | 2021-04-13 | 苏州菲拓生物科技有限公司 | Method for electrochemically assisting preparation of liquid metal hydrogel fiber |
| CN113584723A (en) * | 2021-08-02 | 2021-11-02 | 岭南师范学院 | Liquid metal nanoparticle composite nanofiber membrane and preparation method and application thereof |
| CN114703555A (en) * | 2022-03-07 | 2022-07-05 | 西安工程大学 | One-step forming batch preparation method of core-shell structure liquid metal conductive fiber |
-
2022
- 2022-09-01 CN CN202211063172.4A patent/CN115233335B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624833A (en) * | 2016-03-03 | 2016-06-01 | 青岛大学 | Preparation method of magnetic alginate fiber |
| CN109338716A (en) * | 2018-09-28 | 2019-02-15 | 成都新柯力化工科技有限公司 | A kind of fibrous composite and preparation method for robot electronic skin |
| CN112647156A (en) * | 2020-12-21 | 2021-04-13 | 苏州菲拓生物科技有限公司 | Method for electrochemically assisting preparation of liquid metal hydrogel fiber |
| CN113584723A (en) * | 2021-08-02 | 2021-11-02 | 岭南师范学院 | Liquid metal nanoparticle composite nanofiber membrane and preparation method and application thereof |
| CN114703555A (en) * | 2022-03-07 | 2022-07-05 | 西安工程大学 | One-step forming batch preparation method of core-shell structure liquid metal conductive fiber |
Non-Patent Citations (1)
| Title |
|---|
| 薛超: "聚氨酯基碳纳米管－液态金属导电纤维的制备及其性能", 《纺织学报》, vol. 43, no. 7, pages 29 - 35 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115976689A (en) * | 2023-01-03 | 2023-04-18 | 青岛大学 | Preparation method of algal polysaccharide composite functional fiber |
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