CN102274975A - Method for preparing metal micro-nano hollow spherical powder - Google Patents
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- CN102274975A CN102274975A CN2011101947630A CN201110194763A CN102274975A CN 102274975 A CN102274975 A CN 102274975A CN 2011101947630 A CN2011101947630 A CN 2011101947630A CN 201110194763 A CN201110194763 A CN 201110194763A CN 102274975 A CN102274975 A CN 102274975A
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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 say, relate to a kind of method for preparing metal micro-nano hollow ball powder.
Background technology
The hollow powder of micro-nano is owing to have special hollow-core construction, compare that ultra-fine its specific area of solid powder is big, density is little, showing special excellent properties aspect physics, chemistry, electromagnetism and the optics, especially aspect the suction ripple, the magnetic hollow powder has huge application potential.The structure of magnetic hollow powder, wall thickness not only directly influence the fluctuation of itself dielectric constant and magnetic conductivity, and then directly control its absorbing property, also directly influence it and cover the stealthy body of shielding, weight as 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, as the surface density of present extensive use at 5kg/m
2Above ferrite wave-absorbing material can increase its weight undoubtedly widely, does not reach institute's requirement.The hollow powder that shell is thin has not only alleviated it greatly and has covered the weight of the stealthy body of shielding, may solve the shortcomings such as poor, the anti-oxidant acid and alkali-resistance ability of high-temperature behavior that traditional absorbing material exists in addition, realizes the target of absorbing material " thin, light, wide, strong ".Therefore the magnetic hollow powder has caused the research boom of various countries.The common method of the hollow powder of preparation is a template at present, adopt template to prepare hollow powder, need a colloid, emulsion drop etc. and do template, assemble on its surface then, reactions such as absorption and chemical deposition, also need use methods such as dissolving, calcining, chemical reaction to remove template at last.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.
Discharge ablation processing powder, be by electrode discharge from electrode surface some electrode materials of dishing out, be metal dust after the electrode material of the being dished out cooling.This method has made polytype micro mists such as simple metal, alloy, compound, semiconductor, pottery.People such as domestic Wen Yuhua adopt mixed powder electric discharge machining method to prepare hollow powder (Wang Jing, Wen Yuhua, Li Xianglong, Li Zhongli. mix the research [J] that the spark eroding of Si powder prepares hollow Ni powder. functional material, 2008.), obtain certain effect, need carry out in specific agitating device but mix the powder spark machined, need control to mix the powder degree, device structure is complicated, and the ratio of powder hollow bulbus cordis is lower, and the hollow rate of hollow ball is also lower.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 vacuum tightness case by the polyoxymethylene resin besieged city, the employing liquid nitrogen is a working solution, two electrodes and uniform bulk material are placed on the porose polyoxymethylene resin screen cloth, whole vacuum tightness case is applied the concussion of certain frequency, utilize the spark discharge that reaches between bulk material and the bulk material between two electrodes and the bulk material to produce hollow powder, and point out that shell thickness changes with the difference of composition, the hollow Ni powder inner surface that makes is more coarse.This preparation method's processing conditions requires high, the apparatus structure complexity, and the production cost height, and do not provide concrete shell thickness.
Summary of the invention
The state of the art at prior art for preparing metal hollow powder, purpose of the present invention aims to provide a kind of new method for preparing metal micro-nano hollow ball powder, with preparation hollow ball ratio height, hollow ball hollow rate height, be regular spheroidal, the surfaces externally and internally quality is good, the thin and micro-nano hollow ball powder of wall thickness even metal of shell.
The metal micro-nano hollow ball powder that the present invention will produce is achieved through the following technical solutions:
Tool-electrode and piece pole are keeping the spark required gap of discharging to be immersed in the working solution accordingly, the make pulse power supply makes tool-electrode and piece pole spark discharge fusing, gasifies, in the spark discharge process, the working solution between tool-electrode and the piece pole is implemented the supersonic frequency vibration simultaneously, make the working solution in the gap produce microbubble, the metal material adventitious deposit of tool-electrode and piece pole fusing, gasification is on the microbubble surface, form the metal micro-nano hollow ball, promptly prepare metal micro-nano hollow ball powder through Separation of Solid and Liquid, drying then.
In technique scheme, tool-electrode and piece pole are provided with relation, it can be vertical setting, also can be that flat crouching is provided with, or be obliquely installed, preferably adopt vertical the setting, promptly tool-electrode refers to straight down facing to the piece pole that is immersed in the working solution, and tool-electrode keeps end portion to be immersed in the working solution.
In technique scheme, described ultrasonic vibration can be applied by the working solution of working liquid container body wall between tool-electrode and piece pole by ultrasonic oscillator, also can the working solution between tool-electrode and piece pole applies by tool-electrode or piece pole respectively or simultaneously.Described frequency of ultrasonic should be the frequency that is enough to produce ultrasonic cavitation and bubble crushing effect in working solution, and its frequency generally is not less than 16KHZ, is controlled at 20KHZ~200KHZ scope usually.
In technique scheme, make the pulse current of tool-electrode and piece pole spark discharge fusing, gasification, its intensity generally is not less than 20A, is controlled at 20A~60A scope usually, its pulse width generally is not more than 150 μ s, is controlled at 2 μ s~150 μ s scopes usually.
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 the metal micro-nano hollow ball powder that will prepare, and the material of electrode is exactly the material of metal micro-nano hollow ball 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 for use from kerosene and deionized water, preferably selects kerosene for use.
Metal micro-nano hollow ball powder preparation method of the present invention both applicable to continuous production, is also produced applicable to being interrupted.Producing the metal material that needs in that tool-electrode and piece pole spark discharge melt, gasify continuously is deposited in the process on microbubble surface, the limit adds working solution and the working solution that contains metal micro-nano hollow ball powder is drawn on the limit, and the liquid level of working solution is remained in certain scope.
Metal micro-nano hollow ball powder preparation method of the present invention, can utilize existing spark discharge device, with kerosene or deionized water is working solution, with the metal micro-nano hollow ball dusty material tools electrode and the piece pole that will prepare, working solution between two electrodes is applied ultrasonic vibration, adopt the electric machining parameter of the little pulsewidth of the big electric current corrosion processing of discharging, produce the metal micro-nano hollow ball, the working solution after the processing after filtration, wash, be drying to obtain hollow powder.
The present invention is to be different from traditional electrical spark-ULTRASONIC COMPLEX machining principle processing and preparing metal micro-nano hollow ball powder fully.Galvano-cautery phenomenon when the processing of traditional electrical spark-ULTRASONIC COMPLEX is based on pulse feature spark discharge between instrument and the workpiece is come the unnecessary metal of ablation, to reach the predetermined processing request of size, shape and surface quality to part.The supersonic frequency vibration acts on tool-electrode or piece pole in traditional electrical spark-ULTRASONIC COMPLEX processing, utilizes interelectrode supersonic frequency relative motion, to avoid short circuit, to open circuit and arc discharge, improves machining accuracy and efficient.Principle of the present invention is by the working solution between tool-electrode and the piece pole is applied ultrasonic vibration, utilize hyperacoustic cavitation effect and fragmentation, in working solution, produce a large amount of micro-bubbles, simultaneously by control spark discharge parameter, increase electrode gasification, fusing amount in the spark discharge process, gasification, molten metal material and bubble are met, thereby, form the thin and uniform hollow ball of wall thickness of shell attached on the minute bubbles.In addition, because action of ultrasonic waves, the bubble that the working solution cracking produces in the time of can breaking spark discharge further increases number of bubbles, reduces bubble diameter, obtain more less hollow ball, thereby prepare the metal micro-nano hollow ball powder that to 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, forms hollow ball at its surface deposition.
2, the Vltrasonic device and the spark-erosion machine tool of enforcement the inventive method are relatively independent, are independent of each other during parameter adjustment, and machined parameters is easy to control.
3, the present invention has gathered 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 ball processing of the present invention, do not need additional other equipment except that Vltrasonic device, processing conditions is simple and easy to realize.
The present invention has following beneficial technical effects compared with prior art:
1, cost is low, processing safety is high.Because it is working solution that the present invention adopts kerosene or plasma water, 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, technology is simple, contaminative is little.Hollow ball of the present invention does not need processes such as prefab-form nuclear and later stage chemical solution nuclear in spark-discharge gap moment moulding, so just makes technology simple relatively, has shortened the production cycle greatly.Owing to there is not the participation of too much chemicals in the process, reduced pollution simultaneously to environment.
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, does not need to mix powder and agitating device, and machined parameters is easy to control, and device is simple.
4, ionization puncture is easy, pulse utilization rate height, and the chip removal condition improves.Apply ultrasonic vibration in common spark machined, the advantage of integrated traditional electrical spark-ULTRASONIC COMPLEX processing makes ionization puncture easy, pulse utilization rate height.
5, the hollow degree height of powder, shell is thinner, and has surfaces externally and internally quality preferably.Hollow ball is subjected 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 surfaces externally and internally quality preferably.With respect to mixed powder electric discharge machining method, nearly one times of the ratio increase of its hollow powder.
Description of drawings
Fig. 1 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is installed in working solution casing homonymy.
Fig. 2 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is installed in working solution casing heteropleural.
Fig. 3 implements electric spark-ULTRASONIC COMPLEX processing experiment device schematic diagram that ultrasonic oscillator of the present invention is installed in 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
The present invention is described in further detail below in conjunction with embodiment; it is important to point out; following embodiment only is used for that the present invention is described further; can not be interpreted as limiting the scope of the invention; affiliated art skilled staff is according to the foregoing invention content; the present invention is made some nonessential improvement and adjustment is specifically implemented, should still belong to protection scope of the present invention.
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, tool-electrode as positive electrode is suspended in the working liquid container by the servo feeding apparatus 2 of fixed in position on the working liquid container body wall, 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 the working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in the kerosene.The supersonic generator power 100W of ultrasonic unit, frequency 20KHZ, the ultrasonic oscillator of ultrasonic unit have 6, and homogeneous phase is arranged on the working liquid container body wall facing to the gap between tool-electrode and the piece pole over the ground.Set the spark discharge parameter: low-tension current 20A, pulse width 150 μ s.Opening ultrasonic power and electric spark device processes.With dissolving remaining kerosene with petroleum ether again behind the working solution filtration drying, promptly get the hollow nickel powder after the drying after the completion of processing.7 is workbench.
Accompanying drawing 4 is sem photographs of the hollow nickel powder of present embodiment acquisition.Not adding nickel by powder that the common electrical spark erosion of ultrasonic vibration obtains under this discharging condition does not observe hollow ball and exists.
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, tool-electrode as positive electrode is suspended in the working liquid container by the servo feeding apparatus 2 of fixed in position on the working liquid container body wall, 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 the working liquid container as the plasma water of working solution 4, the end portion of tool-electrode is extend in the plasma water.The supersonic generator power 200W of ultrasonic unit, frequency 60KHZ, the ultrasonic oscillator of ultrasonic unit have 4, are arranged on the working solution casing two side walls facing to the gap between tool-electrode and the piece pole.Set the spark discharge parameter: low-tension current 60A, pulse width 2 μ s.Opening ultrasonic power and electric spark device processes.The hollow nickel powder will promptly be got after the completion of processing behind the working solution filtration drying.7 is workbench.
Accompanying drawing 5 is sem photographs of the hollow nickel powder of present embodiment acquisition.Not adding the powder observation that the common electrical spark erosion of ultrasonic vibration obtains under this discharging condition 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, tool-electrode as positive electrode is suspended in the working liquid container by the servo feeding apparatus 2 of fixed in position on the working liquid container body wall, 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 the working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in the kerosene.The supersonic generator power 400W of ultrasonic unit, frequency 100KHZ, the ultrasonic oscillator of ultrasonic unit have 2, and homogeneous phase is arranged on the working liquid container body wall facing to the gap between tool-electrode and the piece pole over the ground.Set the spark discharge parameter: low-tension current 50A, pulse width 10 μ s.Opening ultrasonic power and electric spark device processes.With dissolving remaining kerosene with petroleum ether again behind the working solution filtration drying, promptly get the hollow copper powder after the drying after the completion of processing.7 is workbench.
Fig. 6 is the ESEM picture of the hollow copper powder of present embodiment acquisition.Not adding copper powders may that the common electrical spark erosion of ultrasonic vibration obtains under this discharging condition does not observe hollow ball and exists.
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, tool-electrode as positive electrode is suspended in the working liquid container by the servo feeding apparatus 2 of fixed in position on the working liquid container body wall, 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 the working liquid container as the kerosene of working solution 4, the end portion of tool-electrode is extend in the kerosene.The supersonic generator power 500W of ultrasonic unit, frequency 200KHZ, the ultrasonic oscillator of ultrasonic unit have 2, are placed in working solution casing bottom, tool-electrode below facing to the gap between tool-electrode and the piece pole.Set the spark discharge parameter: low-tension current 60A, pulse width 100 μ s.Opening ultrasonic power and electric spark device processes.In process, the limit adds working solution kerosene limit and draws the kerosene that contains hollow powder from the working liquid container bottom.With dissolving remaining kerosene with petroleum ether again behind the working solution filtration drying, promptly get the hollow copper powder after the drying after the completion of processing.7 is workbench.
Exist to observe a large amount of hollow balls in the powder that this electric spark-ULTRASONIC COMPLEX processing obtains.
Claims (10)
1. metal micro-nano hollow ball powder preparation method, it is characterized in that: tool-electrode and piece pole are keeping the spark required gap of discharging to be immersed in the working solution accordingly, the make pulse power supply makes tool-electrode and piece pole spark discharge fusing, gasification, in the spark discharge process, the working solution between tool-electrode and the piece pole is implemented the supersonic frequency vibration simultaneously, make the working solution in the gap produce microbubble, tool-electrode and piece pole fusing, the metal material adventitious deposit of gasification is on the microbubble surface, form the metal micro-nano hollow ball, then through Separation of Solid and Liquid, drying promptly prepares metal micro-nano hollow ball powder.
2. metal micro-nano hollow ball powder preparation method according to claim 1 is characterized in that: tool-electrode refers to straight down facing to piece pole, and keeps the tool-electrode end portion to be immersed in the working solution.
3. metal micro-nano hollow ball powder preparation method according to claim 2, it is characterized in that: described ultrasonic vibration is applied by the working solution of working liquid container body wall between tool-electrode and piece pole by ultrasonic oscillator, or the working solution between tool-electrode and piece pole applies by tool-electrode or piece pole respectively or simultaneously.
4. metal micro-nano hollow ball powder preparation method according to claim 3 is characterized in that: the ultrasonic frequency that the working solution between tool-electrode and piece pole applies is the frequency that is enough to produce ultrasonic cavitation and bubble crushing effect in working solution.
5. metal micro-nano hollow ball powder preparation method according to claim 3, it is characterized in that: the ultrasonic frequency that the working solution between tool-electrode and piece pole applies is not less than 16KHZ.
6. metal micro-nano hollow ball powder preparation method according to claim 3 is characterized in that: make the pulse current of tool-electrode and piece pole spark discharge fusing, gasification, its intensity is not less than 20A, and its pulse width is not more than 150 μ s.
7. according to the described metal micro-nano hollow ball of one of claim 1 to 6 powder preparation method, it is characterized in that: tool-electrode is made by the identical metal material of the metal micro-nano hollow ball powder that will prepare with piece pole.
8. metal micro-nano hollow ball powder preparation method according to claim 7, it is characterized in that: electrode was removed surface film oxide before coming into operation.
9. according to the described metal micro-nano hollow ball of one of claim 1 to 6 powder preparation method, it is characterized in that: described working solution is selected from kerosene and deionized water.
10. according to the described metal micro-nano hollow ball of one of claim 1 to 6 powder preparation method, 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 the limit adds working solution and the working solution that contains metal micro-nano hollow ball powder is drawn on the limit.
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CN102910859A (en) * | 2012-09-28 | 2013-02-06 | 成都新柯力化工科技有限公司 | Preparation method for low-density stone paper |
CN104551274A (en) * | 2015-01-21 | 2015-04-29 | 合肥工业大学 | Preparation method of novel electric spark working solution |
CN105834449A (en) * | 2016-05-04 | 2016-08-10 | 苏州思美特表面材料科技有限公司 | Preparation method for inductively producing silver powder by using micro-nano bubbles as crystal seeds |
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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 |
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