CN102274975B - Method for preparing metal micro-nano hollow spherical powder - Google Patents
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Abstract
The invention discloses a method for preparing metal micro-nano hollow spherical powder. The method comprises the main contents of: correspondingly immersing a tool electrode and a workpiece electrode into a working fluid, wherein a gap required by spark discharge is kept between the tool electrode and workpiece electrode; and switching on a pulse power supply to enable the tool electrode and the workpiece electrode to generate spark discharge to be molten and gasified, and meanwhile implementing supersonic vibration on the working fluid between the tool electrode and the workpiece electrode during the spark discharge process, so that the working fluid in the gap generates micro-bubbles, and molten and gasified metal materials of the tool electrode and the workpiece electrode are attached and sedimentated on the surfaces of the micro-bubbles to form metal micro-nano hollow spheres. By adopting the method disclosed by the invention, the prepared metal micro-nano hollow spherical powder has high degree of hollowness, the particle diameter ranges from 20 nanometers to 100 micrometers, the wall surface is not larger than 1 micrometer, and the proportion of the hollow spheres is high. The micro-nano hollow sphere exhibits special outstanding performances in terms of physics, chemistry, electromagnetics and photology, and can be widely applied to the fields of chemistry, metallurgy, material, aerospace and the like.
Description
Technical field
The present invention relates to metal hollow powder preparation technology, more specifically, relate to a kind of method of preparing metal micro-nano hollow sphere powder.
Background technology
The hollow powder of micro-nano is owing to having special hollow-core construction, compare that ultra-fine its specific area of solid powder is large, density is little, aspect physics, chemistry, electromagnetism and optics, showing special excellent properties, especially, aspect suction ripple, magnetic hollow powder has huge application potential.The structure of magnetic hollow powder, wall thickness not only directly affect the fluctuation of itself dielectric constant and magnetic conductivity, and then directly control its absorbing property, also directly affect it and cover the stealthy body of shielding, as the weight of aircraft, guided missile etc., and weight is extremely important to aircraft, guided missile etc., require very harshly, general wave-absorbing and camouflage material covers on its surface, if the surface density of current extensive use is at 5kg/m
2above ferrite wave-absorbing material, can increase its weight undoubtedly widely, do not reach requirement.The hollow powder that shell is thin has not only greatly alleviated it and has covered the weight of the stealthy body of shielding, may solve in addition the shortcomings such as poor, the anti-oxidant acid and alkali-resistance ability of high-temperature behavior that traditional absorbing material exists, and realizes the target of absorbing material " thin, light, wide, strong ".Therefore magnetic hollow powder has caused the research boom of various countries.The common method of the hollow powder of preparation is template at present, adopt the hollow powder of template synthesis, need to there be a colloid, emulsion drop etc. to do template, then on its surface, assemble, the reaction such as absorption and chemical deposition, finally also need to remove template by methods such as dissolving, calcining, chemical reactions.The place of this preparation method's deficiency is that complex process, production efficiency are low, production cost is high, template is difficult for removal and totally and easily causes environmental pollution.
Electric discharge removal processing powder, be by electrode discharge from electrode surface some electrode materials of dishing out, after the electrode material of being dished out is cooling, be metal dust.The method has made polytype micro mists such as simple metal, alloy, compound, semiconductor, pottery.The people such as domestic Wen Yuhua adopt Powder-mixed EDM processing method to prepare hollow powder (Wang Jing, Wen Yuhua, Li Xianglong, Li Zhongli. the research [J] of hollow Ni powder is prepared in mixed Si powder spark eroding. functional material, 2008.), obtain certain effect, but Powder-mixed EDM processing need to be carried out in specific agitating device, needs to control mixed Powder Particle Size, and device structure is more complicated, and the ratio of powder hollow bulbus cordis is lower, and the hollow rate of hollow ball is also lower.The people such as A.E.Berkowitz (A.E.Berkowitz, M.F.Hansen, F.T.Parker, K.S.Vecchio.Amorphous soft magnetic particles produced by spark erosion[J] Journal of Magnetismand Magnetic Materials, 2003, 1 (6): 254-255.) in the vacuum tightness case of being encircled a city by polyoxymethylene resin, employing liquid nitrogen is working solution, two electrodes and uniform bulk material are placed on porose polyoxymethylene resin screen cloth, whole vacuum tightness case is applied to the concussion of certain frequency, utilize the spark discharge between two electrodes and bulk material and between bulk material and bulk material to produce hollow powder, and point out that shell thickness changes with the difference of composition, the hollow Ni powder inner surface making is more coarse.This preparation method's processing conditions requires high, and apparatus structure is complicated, and production cost is high, and does not provide concrete shell thickness.
Summary of the invention
The state of the art of preparing metal hollow powder for prior art, object of the present invention aims to provide a kind of new method of preparing metal micro-nano hollow sphere powder, high to prepare hollow ball ratio, hollow ball hollow rate is high, be regular spheroidal, surfaces externally and internally quality is good, the thin and uniform metal micro-nano hollow sphere powder of wall thickness of shell.
The metal micro-nano hollow sphere powder that the present invention will produce is achieved through the following technical solutions:
Tool-electrode and piece pole are keeping the required gap of spark discharge to be immersed in accordingly in working solution, make pulse power supply makes tool-electrode and piece pole spark discharge fusing, gasifies, in spark discharge process, the working solution between tool-electrode and piece pole is implemented to supersonic frequency vibration simultaneously, make the working solution in gap produce microbubble, the metal material adventitious deposit of tool-electrode and piece pole fusing, gasification is on microbubble surface, form metal micro-nano hollow sphere, then through Separation of Solid and Liquid, the dry metal micro-nano hollow sphere powder that prepares.
In technique scheme, tool-electrode and piece pole arrange relation, it can be vertical setting, also can be flat sleeping setting, or be obliquely installed, preferably adopt vertical setting, tool-electrode refers to straight down facing to being immersed in the piece pole in working solution, and tool-electrode keeps end portion to be immersed in working solution.
In technique scheme, described ultrasonic vibration can be applied to the working solution between tool-electrode and piece pole by working liquid container body wall by ultrasonic oscillator, also can by tool-electrode or piece pole, to the working solution between tool-electrode and piece pole, apply respectively or simultaneously.Described hyperacoustic frequency, should be the frequency that is enough to produce ultrasonic cavitation and bubble crushing effect in working solution, and its frequency is generally not less than 16KHZ, is conventionally controlled at 20KHZ～200KHZ scope.
In technique scheme, the pulse current that makes tool-electrode and piece pole spark discharge fusing, gasification, its intensity is generally not less than 20A, is conventionally controlled at 20A～60A scope, its pulse width is generally not more than 150 μ s, is conventionally controlled at 2 μ s～150 μ s scopes.
In technique scheme, tool-electrode can be made by identical metal material with piece pole, also can be made by different metal materials.Concrete what metal material that adopts, depends on metal micro-nano hollow sphere powder to be prepared, and the material of electrode is exactly the material of metal micro-nano hollow sphere powder.No matter be tool-electrode or piece pole, before coming into operation, preferably carry out surface treatment, remove surface film oxide.
In technique scheme, described working solution is selected from kerosene and deionized water, preferably selects kerosene.
Method for preparing metal micro-nano hollow spherical powder of the present invention, both applicable to continuous production, also produces applicable to being interrupted.The metal material that production need be melted, gasify at tool-electrode and piece pole spark discharge is continuously deposited in the process on microbubble surface, limit adds working solution and limit to draw the working solution that contains metal micro-nano hollow sphere powder, and the liquid level of working solution is remained in certain scope.
Method for preparing metal micro-nano hollow spherical powder of the present invention, can utilize existing spark discharge device, take kerosene or deionized water as working solution, with metal micro-nano hollow sphere powder material tools electrode and the piece pole that will prepare, working solution between two electrodes is applied to ultrasonic vibration, adopt the electric machining parameter of the little pulsewidth of the large electric current corrosion processing of discharging, produce metal micro-nano hollow sphere, the working solution after processing after filtration, wash, be drying to obtain hollow powder.
The present invention is that metal micro-nano hollow sphere powder is prepared in the principle processing that is different from the processing of traditional electrical spark-ULTRASONIC COMPLEX completely.The processing of traditional electrical spark-ULTRASONIC COMPLEX is to carry out the unnecessary metal of ablation based on galvano-cautery phenomenon during pulse feature spark discharge between instrument and workpiece, to reach the predetermined processing request of size, shape and surface quality to part.In the processing of traditional electrical spark-ULTRASONIC COMPLEX, supersonic frequency effect of vibration, in tool-electrode or piece pole, utilizes interelectrode supersonic frequency relative motion, to avoid short circuit, to open circuit and arc discharge, improves machining accuracy and efficiency.Principle of the present invention is to apply ultrasonic vibration by the working solution between tool-electrode and piece pole, utilize hyperacoustic cavitation effect and fragmentation, in working solution, produce a large amount of micro-bubbles, simultaneously by controlling spark discharge parameter, increase electrode gasification, fusing amount in spark discharge process, gasification, molten metal material and bubble are met, thereby be attached on minute bubbles, the thin and uniform hollow ball of wall thickness of formation shell.In addition, due to hyperacoustic effect, the bubble that in the time of can breaking spark discharge, working solution cracking produces, further increases number of bubbles, reduces bubble diameter, obtain more less hollow ball, thereby prepare the metal micro-nano hollow sphere powder that will produce.
Compared with the prior art the present invention has following very outstanding technical characterstic:
1, the present invention is incorporated into the effect of hyperacoustic cavitation effect and bubble crushing in traditional spark machined, and the microvesicle that utilizes ultrasonic cavitation effect and fragmentation to produce is template core, at its surface deposition, forms hollow ball.
2, Vltrasonic device and the spark-erosion machine tool of enforcement the inventive method are relatively independent, during parameter adjustment, are independent of each other, and machined parameters is easy to control.
3, set of the present invention the advantage of traditional electrical spark-ultrasonic wave Compound Machining, and process principle is different from traditional electrical spark-ultrasonic wave Compound Machining.
4, adopt common spark-erosion machine tool just can realize metal micro-nano hollow sphere processing of the present invention, do not need additional other equipment except Vltrasonic device, processing conditions is simple and easy to realize.
The present invention compared with prior art, has following useful technique effect:
1, cost is low, processing safety is high.Because the present invention adopts kerosene or plasma water, be working solution, on common spark-erosion machine tool, realize processing, do not need vacuum environment and liquid nitrogen working solution, reduced processing cost, improved the security of processing simultaneously.
2, the production cycle shortens greatly, technique is simple, contaminative is little.Hollow ball of the present invention, in spark-discharge gap moment moulding, does not need the processes such as prefab-form core and later stage chemical solution core, so just makes technique relatively simple, has greatly shortened the production cycle.Owing to there is no the participation of too much chemicals in process, reduced the pollution to environment simultaneously.
3, simple, the machined parameters of device is easy to control.The present invention only needs common electric spark machine tool and Vltrasonic device just can realize, and does not need mixed powder and agitating device, and machined parameters is easy to control, and device is simple.
4, ionization puncture is easy, and pulse utilization rate is high, and chip removal condition improves.In common spark machined, apply ultrasonic vibration, the advantage of integrated traditional electrical spark-ULTRASONIC COMPLEX processing, makes ionization puncture easy, and pulse utilization rate is high.
5, the hollow degree of powder is high, and shell is thinner, and has good surfaces externally and internally quality.Hollow ball is subject to the effect of surface tension and cohesive force in forming process, deposition modeling on microvesicle again, and the hollow ball external diameter of formation is between 20 nanometers to 50 micron, and wall thickness is not more than 1 micron, and not only shell is thin, and has good surfaces externally and internally quality.With respect to Powder-mixed EDM processing method, nearly one times of the ratio increase of its hollow powder.
Accompanying drawing explanation
Fig. 1 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is arranged on working solution casing homonymy.
Fig. 2 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is arranged on working solution casing heteropleural.
Fig. 3 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is arranged on working solution casing bottom.
The ESEM picture of the hollow nickel powder that Fig. 4 embodiment 1 obtains.
The ESEM picture of the hollow nickel powder that Fig. 5 embodiment 2 obtains.
The ESEM picture of the hollow copper powder that Fig. 6 embodiment 3 obtains.
Above-mentioned each attached picture in picture is known the sign of label to liking: 1 pulse power; 2 servo feeding apparatus; 3 tool-electrodes; 4 working solutions; 5 ultrasonic oscillators; 6 piece poles; 7 workbench; 8 working liquid containers.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail; it is important to point out; following embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; affiliated art skilled staff is according to foregoing invention content; the present invention is made to some nonessential improvement and adjustment is specifically implemented, should still belong to protection scope of the present invention.
Embodiment 1
Metal nickel plate is processed into rectangular tool-electrode 3 and piece pole 6, electrode surface deoxidation film and equating is whole.At the bottom of being placed on cylindrical shape working liquid container 8 casees as the piece pole of negative electrode, as the tool-electrode of positive electrode, by fixed in position, the servo feeding apparatus on working liquid container body wall 2 is suspended in working liquid container, refer to downwards facing to piece pole, process is to keep the required gap of spark discharge, tool-electrode is connected with the both positive and negative polarity interface of Pulased power supply unit 1 with piece pole, to pour in working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in kerosene.The supersonic generator power 100W of ultrasonic unit, frequency 20KHZ, the ultrasonic oscillator of ultrasonic unit has 6, and homogeneous phase is arranged on working liquid container body wall facing to the gap between tool-electrode and piece pole over the ground.Set spark discharge parameter: low-tension current 20A, pulse width 150 μ s.Opening ultrasonic power and electro-discharge device processes.After completion of processing, will after working solution filtration drying, by petroleum ether, dissolve remaining kerosene again, after being dried, obtain hollow nickel powder.7 is workbench.
Accompanying drawing 4 is scanning electron microscope (SEM) photographs of the hollow nickel powder of the present embodiment acquisition.Under this discharging condition, not adding nickel by powder that the common spark eroding of ultrasonic vibration obtains does not observe hollow ball and exists.
Embodiment 2
Metal nickel plate is processed into rectangular tool-electrode 3 and piece pole 6, electrode surface deoxidation film and equating is whole.At the bottom of being placed on square working liquid container 8 casees as the piece pole of negative electrode, as the tool-electrode of positive electrode, by fixed in position, the servo feeding apparatus on working liquid container body wall 2 is suspended in working liquid container, refer to downwards facing to piece pole, process is to keep the required gap of spark discharge, tool-electrode is connected with the both positive and negative polarity interface of Pulased power supply unit 1 with piece pole, to pour in working liquid container as the plasma water of working solution 4, the end portion of tool-electrode is extend in plasma water.The supersonic generator power 200W of ultrasonic unit, frequency 60KHZ, the ultrasonic oscillator of ultrasonic unit has 4, facing to the gap between tool-electrode and piece pole, is arranged in working solution casing two side walls.Set spark discharge parameter: low-tension current 60A, pulse width 2 μ s.Opening ultrasonic power and electro-discharge device processes.After completion of processing, hollow nickel powder will be obtained after working solution filtration drying.7 is workbench.
Accompanying drawing 5 is scanning electron microscope (SEM) photographs of the hollow nickel powder of the present embodiment acquisition.Under this discharging condition, not adding the powder observation that the common spark eroding of ultrasonic vibration obtains exists less than hollow ball.
Metal copper plate is processed into rectangular tool-electrode 3 and piece pole 6, electrode surface deoxidation film and equating is whole.At the bottom of being placed on cylindrical shape working liquid container 8 casees as the piece pole of negative electrode, as the tool-electrode of positive electrode, by fixed in position, the servo feeding apparatus on working liquid container body wall 2 is suspended in working liquid container, refer to downwards facing to piece pole, process is to keep the required gap of spark discharge, tool-electrode is connected with the both positive and negative polarity interface of Pulased power supply unit 1 with piece pole, to pour in working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in kerosene.The supersonic generator power 400W of ultrasonic unit, frequency 100KHZ, the ultrasonic oscillator of ultrasonic unit has 2, and homogeneous phase is arranged on working liquid container body wall facing to the gap between tool-electrode and piece pole over the ground.Set spark discharge parameter: low-tension current 50A, pulse width 10 μ s.Opening ultrasonic power and electro-discharge device processes.After completion of processing, will after working solution filtration drying, by petroleum ether, dissolve remaining kerosene again, after being dried, obtain hollow copper powder.7 is workbench.
Fig. 6 is the ESEM picture of the hollow copper powder of the present embodiment acquisition.Under this discharging condition, not adding copper powders that the common spark eroding of ultrasonic vibration obtains does not observe hollow ball and exists.
Embodiment 4
Metal copper plate is processed into rectangular tool-electrode 3 and piece pole 6, electrode surface deoxidation film and equating is whole.At the bottom of being placed on cylindrical shape working liquid container 8 casees as the piece pole of negative electrode, as the tool-electrode of positive electrode, by fixed in position, the servo feeding apparatus on working liquid container body wall 2 is suspended in working liquid container, refer to downwards facing to piece pole, process is to keep the required gap of spark discharge, tool-electrode is connected with the both positive and negative polarity interface of Pulased power supply unit 1 with piece pole, to pour in working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in kerosene.The supersonic generator power 500W of ultrasonic unit, frequency 200KHZ, the ultrasonic oscillator of ultrasonic unit has 2, facing to the gap between tool-electrode and piece pole, is placed in working solution casing bottom, tool-electrode below.Set spark discharge parameter: low-tension current 60A, pulse width 100 μ s.Opening ultrasonic power and electro-discharge device processes.In process, limit adds working solution kerosene limit to draw from working liquid container bottom the kerosene that contains hollow powder.After completion of processing, will after working solution filtration drying, by petroleum ether, dissolve remaining kerosene again, after being dried, obtain hollow copper powder.7 is workbench.
In the powder obtaining with the processing of this electric spark-ULTRASONIC COMPLEX, observing a large amount of hollow balls exists.
Claims (7)
1. a method for preparing metal micro-nano hollow spherical powder, it is characterized in that: tool-electrode and piece pole are keeping the required gap of spark discharge to be immersed in accordingly in working solution, make pulse power supply makes tool-electrode and piece pole spark discharge fusing, gasification, in spark discharge process, the working solution between tool-electrode and piece pole is implemented to ultrasonic vibration simultaneously, make the working solution in gap produce microbubble, tool-electrode and piece pole fusing, the metal material adventitious deposit of gasification is on microbubble surface, form metal micro-nano hollow sphere, then through Separation of Solid and Liquid, the dry metal micro-nano hollow sphere powder that prepares, described ultrasonic frequency vibratory is not less than 16KHZ, describedly make tool-electrode and piece pole spark discharge fusing, the pulse current intensity of gasification is not less than 20A, pulse width is not more than 150 μ s.
2. method for preparing metal micro-nano hollow spherical powder according to claim 1, is characterized in that: tool-electrode refers to straight down facing to piece pole, and retaining tool electrode end portion is immersed in working solution.
3. method for preparing metal micro-nano hollow spherical powder according to claim 2, it is characterized in that: described ultrasonic vibration is applied to the working solution between tool-electrode and piece pole by working liquid container body wall by ultrasonic oscillator, or by tool-electrode or piece pole, to the working solution between tool-electrode and piece pole, apply respectively or simultaneously.
4. according to the method for preparing metal micro-nano hollow spherical powder one of claims 1 to 3 Suo Shu, it is characterized in that: tool-electrode is made by the identical metal material of the metal micro-nano hollow sphere powder that will prepare with piece pole.
5. method for preparing metal micro-nano hollow spherical powder according to claim 4, is characterized in that: electrode was removed surface film oxide before coming into operation.
6. according to the method for preparing metal micro-nano hollow spherical powder one of claims 1 to 3 Suo Shu, it is characterized in that: described working solution is selected from kerosene and deionized water.
7. according to the method for preparing metal micro-nano hollow spherical powder one of claims 1 to 3 Suo Shu, it is characterized in that: the metal material that melts, gasifies at tool-electrode and piece pole spark discharge is deposited in the process on microbubble surface, and limit adds working solution and limit to draw the working solution that contains metal micro-nano hollow sphere powder.
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| CN102623273B (en) * | 2012-04-13 | 2015-02-18 | 苏州晶讯科技股份有限公司 | Miniature fuse |
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| CN105834449B (en) | 2016-05-04 | 2017-09-22 | 苏州思美特表面材料科技有限公司 | It is a kind of that the preparation method for producing silver powder is induced by the use of micro-nano bubble as crystal seed |
| CN108856703B (en) * | 2018-06-29 | 2021-02-19 | 中国电子科技集团公司第二十六研究所 | Two-phase spherical material, manufacturing device and manufacturing method thereof, and manufacturing method of plate |
| CN108480653A (en) * | 2018-06-29 | 2018-09-04 | 中国科学院上海光学精密机械研究所 | The device and method of hollow over spherical powder is prepared based on femtosecond laser |
| CN108580916A (en) * | 2018-08-01 | 2018-09-28 | 重庆国际复合材料股份有限公司 | A kind of electric spark corrode prepares the reaction unit of metal powder |
| CN111172381A (en) * | 2020-01-20 | 2020-05-19 | 重庆医科大学 | Method and device for changing performance of metal material by utilizing strong cavitation |
| CN113070481B (en) * | 2021-03-30 | 2023-06-27 | 深圳航科新材料有限公司 | Method for preparing metal powder by cavitation jet assisted arc micro-explosion and metal powder |
| CN113976900B (en) * | 2021-11-01 | 2022-10-28 | 电子科技大学 | Equipment for preparing ultrafine powder by batch electric spark and ultrafine powder production system |
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