CN114850422B - Method for preparing metal micro-nano fibers through centrifugal melt electrostatic spinning - Google Patents
Method for preparing metal micro-nano fibers through centrifugal melt electrostatic spinning Download PDFInfo
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- CN114850422B CN114850422B CN202210533834.3A CN202210533834A CN114850422B CN 114850422 B CN114850422 B CN 114850422B CN 202210533834 A CN202210533834 A CN 202210533834A CN 114850422 B CN114850422 B CN 114850422B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/005—Continuous casting of metals, i.e. casting in indefinite lengths of wire
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
- B22D13/02—Centrifugal casting; Casting by using centrifugal force of elongated solid or hollow bodies, e.g. pipes, in moulds rotating around their longitudinal axis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
- B22D13/10—Accessories for centrifugal casting apparatus, e.g. moulds, linings therefor, means for feeding molten metal, cleansing moulds, removing castings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention belongs to the field of electrostatic spinning, and particularly relates to a novel method for preparing metal micro-nano fibers by centrifugal melt electrostatic spinning. The method comprises the following steps: 1) Putting a pure metal block with certain mass into a customized crucible, covering an end cover, installing a thermocouple, starting a power supply of a comprehensive control console, turning on an electromagnetic induction coil heating switch, and heating the customized crucible until the metal block is completely melted; 2) Starting a high-voltage power supply and a high-speed motor, driving the customized crucible to rotate to provide centrifugal force under the action of a rotating shaft, and uniformly dropping the metal melt in the customized crucible onto a collecting plate in a fiber form through a porous spray head under the dual action of the centrifugal force and high-voltage electrostatic force to obtain the long metal fiber with the advantages of small fiber diameter, wide application range and the like. The method for preparing the metal fiber is simple and convenient, has low production cost and high spinning efficiency, and can produce finer and longer micro-nano metal fiber.
Description
Technical Field
The invention relates to a method for preparing metal micro-nano fibers by adopting a centrifugal melt electrostatic spinning process, and belongs to the field of electrostatic spinning.
Background
The micro-nano metal fiber felt prepared by electrostatic spinning has a porous structure, a large number of mutually communicated pores are formed in the micro-nano metal fiber felt, so that sound waves can be diffused and consumed in the material, and the high specific surface area of the micro-nano metal fiber felt is favorable for collision consumption of the sound waves in medium and low frequency bands and the surface of the fiber. Therefore, the micro-nano metal fiber prepared by electrostatic spinning has obvious advantages in the aspect of absorbing medium and low frequency sound waves. In addition, the metal fiber also has the advantages of good mechanical strength, high temperature resistance, impact resistance and the like, and has wider application range. The metal fiber with the fiber diameter of micro-nano level can absorb sound and reduce noise in various extreme environments. The development of light-weight, highly durable metal fiber-based sound absorbers is a necessary trend for future development.
The preparation of the metal fiber at present mainly comprises a drawing method, a cutting method, a grinding method, a metal plating sintering method and the like. The fiber prepared by the drawing method has smooth surface and accurate size, but has low production efficiency, high mold cost, high price and larger fiber diameter. Although the cutting method is simple, short in production period and low in cost, it is difficult to obtain fibers with uniform and smooth sections, and the cutting method is mainly used for producing short metal fibers. The grinding method can produce metal short fibers with a desired diameter, but the fiber diameter is seriously affected by various factors, such as the coarser the abrasive particle size, the coarser the diameter of the produced metal fiber. The metal fiber prepared by the plating metal sintering method has the problems of large investment, high process cost and the like. These methods of preparing metal fibers all have their disadvantages.
Zhang Tongling and the like adopt a melt drawing method to prepare the titanium-based metal fiber with the diameter of 20-50 mu m. The fiber has the advantages of uniform diameter, smooth surface, maximum length of 20cm, amorphous structure, good thermal stability and excellent mechanical property, but has the defects of more complex preparation process and higher cost. The permissive drug and the like adopts an electroplating method to deposit an iron-plated layer on the surface of a 316L stainless steel wire, and the stainless steel fiber with the diameter of 12 mu m is prepared through the working procedures of pipe penetration, drawing, annealing, electrolysis and the like. However, the surface quality of the fiber is poor, obvious precipitates and grooves exist, the breaking strength and the elongation rate of the fiber are low, and measures such as annealing treatment of the electroplated wire and annealing by using a continuous annealing furnace with a water cooling device are needed to improve.
The present invention provides a method for preparing metal fiber, which solves the problems of low production efficiency, high cost, large diameter and insufficient length of the produced fiber. The electrostatic spinning process can be used for efficiently preparing the micro-nano metal fibers and producing long fibers, and compared with short fibers produced by a mechanical force or gas pressure spinning method and a cutting method, the long fibers have more complicated entanglement structures, the complex entanglement enables the void structures among the fibers to be more diversified, and the effective absorption of sound waves with different wavelengths can be realized; compared with the metal plating sintering method, the electrostatic spinning process does not need complex physical and chemical treatment, and has simpler process and relatively lower cost. Meanwhile, the fiber produced by the electrostatic spinning method has the advantage of small fiber diameter (the diameter of the melt electrostatic spinning fiber is generally hundreds of nanometers to several micrometers), and thinner fiber can effectively absorb low-frequency sound waves with longer wavelength which are difficult to eliminate, so that the research on the electrostatic spinning process suitable for spinning the micro-nano metal fiber to prepare the sound-absorbing material has great application prospect.
Disclosure of Invention
The invention provides a method for preparing metal micro-nanofibers through centrifugal melt electrostatic spinning, and aims to produce long metal fibers with the advantages of small fiber diameter, wide application range and the like and reduce production cost.
The method adopts a novel centrifugal melt electrostatic spinning device to prepare the metal micro-nano fiber, and the device comprises a spinning system, an electromagnetic heating system, a collecting system, a transmission system, a rack and a high-voltage power supply, wherein the spinning system consists of a customized crucible, a heat-insulating sleeve, an end cover and a porous spray head, the customized crucible is made of graphite serving as a main material, not only has good electromagnetic induction capability, but also has smooth inner wall, the molten metal liquid in the customized crucible is not easy to leak and adhere to the inner wall of the crucible, so that the molten metal liquid has good fluidity and castability, meanwhile, the corrosion resistance of the graphite crucible is excellent, metal residues possibly existing after spinning is finished can be cleaned by nitric acid or hydrochloric acid and lightly ground by fine sand, and the device is very convenient and can not damage the crucible; the heat-insulating sleeve is used for preventing the customized crucible wall from radiating too fast, so that the temperature difference of each part of the crucible is reduced, and the spinning process of the porous nozzle is prevented from being influenced; the end cover is provided with an observation port for checking the melting condition of the metal block in the customized crucible, the middle part of the end cover is provided with a small hole, so that the K-type thermocouple can pass through and extend into the metal melt, and meanwhile, the end cover can reduce the heat loss, thereby reducing the temperature difference between the upper part and the bottom of the customized crucible; the bottom of the customized crucible is provided with a boss and is provided with a hole, the customized crucible is connected with the rotating shaft through a threaded joint, the rising direction of the thread is the same as the rotating direction of the rotating shaft, and the customized crucible is ensured to be connected with the rotating shaft more and more firmly and cannot be thrown away in the rotating process; a hole for melt flowing is formed in the side face of the customized crucible at the position of 3/5 of the height, the capacity of raw materials is increased under the condition that the rotating speed can be adjusted in a large range, and the raw materials are connected with a multi-hole nozzle in a threaded connection mode to realize spinning; the porous nozzle is divided by last module, lower module, position circle and fixed end cover four bibliographic categories and forms, and the top of going up the module is processed into the form of screw thread and is linked to each other with the customization crucible, and upper and lower module combination forms the runner, and the sprue diameter is by thin to thick, and the reposition of redundant personnel position sets up to circular-arc arch to reduce the impact pressure of metal melt to each part. The porous nozzle uses a positioning ring to position each part, and then 12 set screws are adopted to be connected with other three parts through a fixed end cover so as to play a role in fixing the whole body. All parts of the nozzle are made of stainless steel, so that the nozzle has the advantages of difficult material accumulation and impurity adhesion, and is convenient to disassemble and replace at any time. The electromagnetic heating system consists of an electromagnetic induction coil, a K-type thermocouple and a comprehensive console. Wherein the electromagnetic induction coil passes through the screw thread and links to each other with the support, and the support passes through the fix with screw in the frame, and the K type thermocouple directly stretches into the metal melt in the customization crucible, carries out real-time temperature monitoring to it to feed back to the integrated control platform, through instrument demonstration, record, thereby be convenient for control whether heating of electromagnetic induction coil is according to real-time temperature, realize heating and temperature control to the metal melt in the customization crucible. The metal protection tube is equipped with in K type thermocouple outside, when convenient maintenance and change, can play the fixed action and avoid high temperature metal melt to bond, guarantees that the thermocouple does not receive the destruction of high temperature metal melt. The collecting system comprises collecting plate and alumina baffle, between collecting plate and the alumina baffle, links to each other fixedly through the screw between alumina baffle and the frame respectively, and the alumina baffle does not possess the conducting property, and the melting point is high again, when the fixed collecting plate of support that can be fine, can not destroyed by the metal melt spill again. The transmission system consists of a high-speed motor and a rotating shaft, the high-speed motor is fixed on the ground and is perpendicular to the rack, the rotating speed is 0-3000 r/min, the starting and the adjustment of the working frequency are controlled by the comprehensive control console, and the customized crucible is driven to rotate to provide the spinning centrifugal force by driving the rotating shaft to rotate. The rotating shaft is connected with the customized crucible through a threaded joint and is fixed on the frame through a bearing. The frame supports the whole device and is protected with earth, the positive pole of the high-voltage power supply is connected with the collecting plate, and the negative pole is grounded, so that a high-voltage electrostatic field is formed between the customized crucible and the collecting plate, and electrostatic spinning is realized. The whole centrifugal melt electrostatic spinning device is horizontally arranged, the rotating shaft is respectively connected with the customized crucible and the rack, and the customized crucible, the rack and the rack have good conductivity and are protected by grounding of the rack. The porous spray head and the collecting plate have a certain distance, and the voltage is controlled within a certain range, so that the short circuit cannot be broken down between the porous spray head and the collecting plate, and the spinning process is not influenced.
The invention adopts the following steps to prepare the superfine metal fiber:
the method comprises the following steps: putting a pure metal block with certain mass into a customized crucible, covering an end cover, and installing and fixing a K-type thermocouple;
step two: starting a power supply of the comprehensive control console, turning on an electromagnetic induction heating switch, and heating the customized crucible through an electromagnetic induction coil;
step three: observing through an observation port until the metal block is heated to be completely melted and then preserving heat for a certain time;
step four: starting a high-voltage power supply and a high-speed motor, wherein the high-voltage power supply provides high-voltage electrostatic force, the high-speed motor is set to have a certain rotating speed, and the customized crucible is driven to rotate under the action of a rotating shaft so as to provide spinning centrifugal force;
step five: the metal melt in the customized crucible uniformly falls onto the collecting plate in a fiber form through the porous spray head under the dual action of centrifugal force and high-pressure electrostatic force, and the long metal fiber with the advantages of small fiber diameter, wide application range and the like is obtained.
Further, the mass of the metal block in the first step is 10-50g.
Further, the heat preservation time in the third step is 10-30min.
Further, the rotating speed interval in the fourth step is 1000r/min-2000r/min.
The beneficial effects of the invention are as follows:
(1) The customized crucible is made of graphite as a main material, not only has good electromagnetic induction capability, electric conduction capability and corrosion resistance, but also has smooth inner wall and is not easy to adhere to metal melt.
(2) The electromagnetic induction coil heating mode belongs to non-contact heating and has the advantages of high heating temperature, high heating efficiency, high heating speed, easy temperature control and the like.
(3) The method of contact temperature measurement is adopted, the K-type thermocouple is in direct contact with the metal melt, the true temperature of the metal melt can be reflected, meanwhile, the metal protection tube is arranged outside, the service life of the thermocouple is prolonged while the maintenance and the replacement are convenient, and the method has the advantages of high measurement precision, wide measurement range, simple structure, convenience in use, low price and the like.
(4) The switch that is provided with the heating of control electromagnetic induction coil simultaneously on the integrated control platform, the switch that controls high speed motor start-up and adjustment rotational speed and with the supporting display instrument, record instrument and the electronic regulator who uses of K type thermocouple, the fuse-element temperature can transmit in real time to the display instrument to more conveniently realize interrupting the heating of electromagnetic induction coil, guaranteed that the fuse-element temperature is in certain within range all the time, be favorable to the stability of spinning process to go on.
(5) Adopt self-control porous shower nozzle, by last module, lower module, position circle, fixed end cover four bibliographic categories divide to constitute, upper and lower module combination forms the runner, and the sprue diameter is by thin to thick, and the reposition of redundant personnel position sets up to circular-arc arch, can effectively reduce the impact pressure of metal melt to each part. Each part of the spray head is connected by a set screw, so that the spray head is convenient to disassemble and replace, and is made of stainless steel, so that the spray head is not easy to accumulate materials and adhere impurities, and has a higher melting point and good conductivity, and metal fibers which are thinner and longer can be spun under the dual action of centrifugal force and high-voltage electrostatic force, and the spinning efficiency is effectively improved.
(6) The spinning device can freely change the spinning mode, not only can realize centrifugal melt electrostatic spinning, but also can carry out solution centrifugal electrostatic spinning at room temperature when the temperature control device is not started, and can also carry out centrifugal spinning without electrostatic effect when a high-voltage power supply is not switched on.
(7) The method for preparing the metal micro-nano fibers has the advantages that the production efficiency is high, the cost is low, the prepared metal fibers are thinner and longer, the long fibers have more complex entanglement structures, the complex entanglement enables the gap structures among the fibers to be more diversified, the effective absorption of sound waves with different wavelengths is facilitated, the thinner fibers can effectively absorb low-frequency sound waves which are difficult to eliminate, and the method has important significance for preparing sound-absorbing materials with excellent sound absorption and noise reduction performance.
Description of the drawings:
fig. 1 is a schematic diagram of an apparatus for preparing micro-nano metal fibers by centrifugal melt electrostatic spinning. Fig. 2 is a schematic structural view of the porous spray head, and fig. 3 is a plan view of the porous spray head.
In the figure: 1-collecting plate, 2-electromagnetic induction coil, 3-customized crucible, 4-heat preservation sleeve, 5-end cover, 6-metal protection tube, 7-K type thermocouple, 8-viewing port, 9-porous nozzle, 10-metal fiber, 11-high voltage power supply, 12-rotating shaft, 13-high speed motor, 14-bracket, 15-frame, 16-alumina partition plate, 17-comprehensive console, 18-upper module, 19-lower module, 20-locating ring and 21-fixed end cover.
The spinning system comprises a customized crucible 3, a heat-insulating sleeve 4, an end cover 5 and a porous spray head 9, the porous spray head 9 comprises an upper module 18, a lower module 19, a positioning ring 20 and a fixed end cover 21, the electromagnetic heating system comprises an electromagnetic induction coil 2, a K-type thermocouple 7 and a comprehensive control console 17, the collecting system comprises a collecting plate 1 and an alumina partition plate 16, the transmission system comprises a rotating shaft 12 and a high-speed motor 13, a rack 15 is used for supporting the whole device, and a support 14 is used for supporting the electromagnetic induction coil 2.
Detailed Description
Example 1:
in the device shown in figure 1, 30g of metal blocks are added into a customized crucible 3, an end cover 5 is covered, a K-type thermocouple 7 is installed and fixed, then a power supply of a comprehensive control console 17 is switched on, the metal blocks in the customized crucible 3 are heated through an electromagnetic induction coil 2, real-time temperature monitoring is carried out on the metal blocks through the K-type thermocouple 7, signals are fed back to the comprehensive control console 17, observation is carried out through an observation port in the end cover 5 until all the pure metal blocks are melted into a melt, heat preservation is carried out for 10min, then a high-voltage power supply 11 and a high-speed motor 13 are started, the set rotating speed is 1000r/min, the customized crucible 3 is driven to rotate through a rotating shaft 12, and finally the metal melt uniformly falls onto a collecting plate 1 in a fiber form through a porous nozzle 9 on the customized crucible 3 under the dual effects of centrifugal force and high-voltage electrostatic force, so that long metal fibers 10 with multiple advantages of small fiber diameter, wide application range and the like are obtained.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. A method for preparing metal micro-nanofibers through centrifugal melt electrostatic spinning is characterized in that a centrifugal melt electrostatic spinning device is adopted to prepare the metal micro-nanofibers, the device comprises a spinning system, an electromagnetic heating system, a collecting system, a transmission system, a rack and a high-voltage power supply, wherein the spinning system consists of a customized crucible, a heat-insulating sleeve, an end cover and a porous nozzle, the customized crucible is made of graphite serving as a main material, the inner wall of the customized crucible is smooth, and metal residues possibly existing after spinning can be cleaned by nitric acid or hydrochloric acid and subjected to fine sand light grinding treatment; the heat-insulating sleeve is used for preventing the wall of the customized crucible from radiating too fast and reducing the temperature difference of each part of the customized crucible; the end cover is provided with an observation port for checking the melting condition of the metal block in the customized crucible, and the middle part of the end cover is provided with a small hole for enabling the K-type thermocouple to pass through and extend into the metal melt; the bottom of the customized crucible is provided with a boss and a hole, the customized crucible is connected with the rotating shaft through a threaded joint, the rising direction of the thread is the same as the rotating direction of the rotating shaft, and the customized crucible is ensured to be connected with the rotating shaft more and more firmly in the rotating process and cannot be thrown away; a hole for melt flowing is formed in the side face of the customized crucible at the position of 3/5 of the height, the capacity of raw materials is increased under the condition that the rotating speed can be adjusted in a large range, and the raw materials are connected with a multi-hole spray head in a threaded connection mode to realize spinning; the multi-hole spray head is composed of an upper module, a lower module, a locating ring and a fixed end cover, wherein the top end of the upper module is processed into a thread form and is connected with the customized crucible, the upper module and the lower module are combined to form a flow channel, the diameter of the main flow channel is from thin to thick, and the flow distribution position is provided with an arc-shaped bulge, so that the impact pressure of the metal melt on each part is reduced; the porous nozzle uses a positioning ring to position each part, and then 12 set screws are connected with other three parts through a fixed end cover to play a role in fixing the whole; all parts of the porous spray head are made of stainless steel, so that the porous spray head is convenient to disassemble and replace at any time; the electromagnetic heating system consists of an electromagnetic induction coil, a K-type thermocouple and a comprehensive console; the electromagnetic induction coil is connected with the support through threads, the support is fixed on the rack through screws, the K-type thermocouple directly extends into the metal melt in the customized crucible, real-time temperature monitoring is carried out on the metal melt, the metal melt is fed back to the comprehensive control console, and the metal melt is displayed and recorded through the instrument, so that whether the electromagnetic induction coil is heated or not is controlled according to the real-time temperature, and the heating and the temperature control of the metal melt in the customized crucible are realized; a metal protection tube is arranged outside the K-type thermocouple; the collecting system consists of a collecting plate and an alumina clapboard, wherein the collecting plate is connected and fixed with the alumina clapboard and the alumina clapboard is connected and fixed with the rack through screws; the transmission system consists of a high-speed motor and a rotating shaft, the high-speed motor is fixed on the ground and is vertical to the rack, the starting and the adjustment of the working frequency are controlled by the comprehensive control console, and the customized crucible is driven to rotate by driving the rotating shaft to provide the spinning centrifugal force; the rotating shaft is connected with the customized crucible through a threaded joint and is fixed on the rack through a bearing; the frame supports the whole device and is protected in parallel, the positive pole of the high-voltage power supply is connected with the collecting plate, and the negative pole is grounded, so that a high-voltage electrostatic field is formed between the customized crucible and the collecting plate, and electrostatic spinning is realized; the whole centrifugal melt electrostatic spinning device is horizontally placed, the rotating shaft is respectively connected with the customized crucible and the rack, the customized crucible, the rack and the rack have good conductivity, and the centrifugal melt electrostatic spinning device is protected by grounding of the rack; the porous spray head and the collecting plate have a certain distance, and the voltage is controlled within a certain range, so that the short circuit caused by breakdown can be avoided between the porous spray head and the collecting plate, and the spinning process is not influenced.
2. The method for preparing the metal micro-nano fiber by centrifugal melt electrospinning according to claim 1, characterized by comprising the following steps:
the method comprises the following steps: putting a pure metal block with certain mass into a customized crucible, covering an end cover, and installing and fixing a K-type thermocouple;
step two: starting a power supply of the comprehensive control console, turning on an electromagnetic induction heating switch, and heating the customized crucible through an electromagnetic induction coil;
step three: observing through an observation port until the metal block is heated to be completely melted and then preserving heat for a certain time;
step four: starting a high-voltage power supply and a high-speed motor, wherein the high-voltage power supply provides high-voltage electrostatic force, the high-speed motor is set to have a certain rotating speed, and the customized crucible is driven to rotate under the action of a rotating shaft so as to provide spinning centrifugal force;
step five: the metal melt in the customized crucible uniformly falls onto a collecting plate in a fiber form through a porous spray head under the double actions of centrifugal force and high-pressure electrostatic force to obtain long metal fibers.
3. The method for preparing the metal micro-nano fiber through centrifugal melt electrospinning according to claim 2, wherein the mass of the metal block in the first step is 10-50g.
4. The method for preparing the metal micro-nano fiber through centrifugal melt electrospinning according to claim 2, wherein the heat preservation time in the third step is 10-30min.
5. The method for preparing the metal micro-nano fibers through centrifugal melt electrospinning according to claim 2, wherein the rotating speed interval in the fourth step is 800r/min-2000r/min.
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