CN100551588C - A kind of preparation method of hollow micro-nano-nickel powder - Google Patents
A kind of preparation method of hollow micro-nano-nickel powder Download PDFInfo
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- CN100551588C CN100551588C CNB2008100452018A CN200810045201A CN100551588C CN 100551588 C CN100551588 C CN 100551588C CN B2008100452018 A CNB2008100452018 A CN B2008100452018A CN 200810045201 A CN200810045201 A CN 200810045201A CN 100551588 C CN100551588 C CN 100551588C
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Abstract
The present invention relates to the preparation method of hollow nickel powder.Mixed liquor with deionized water and silica flour is a working solution, and tool-electrode and workpiece are made by metallic nickel, and the mixed liquor after the spark eroding processing after filtration, dry, silica removal obtains spherical hollow nickel powder.The nickel powder apparent density that makes is at 2.02～2.76g/cm
3Between, particle diameter is concentrated and to be distributed between tens nanometers to 50 micron.The purity height of nickel powder, particle hollow degree height.
Description
Technical field
The present invention relates to a kind of preparation method of hollow metal powder, be specifically related to a kind of preparation method of hollow nickel powder.
Background technology
Owing to the superfines of hollow-core construction is compared physicochemical properties such as having special mechanics, light, electricity with corresponding solid powder and is shown great application prospect, in recent years, have the preparation of superfines of hollow-core construction and application and become a focus in the investigation of materials.Extra-fine nickel powder is owing to the good and good ferromagnetism of surface-active height, electric conductivity and thermal conductivity is widely used in fields such as chemical catalyst, sintering activator, electrocondution slurry, battery, carbide alloy, ferrofluid.People such as A.E.Berkowitz (Hollow metallicmicrospheres produced by spark erosion.Appl.Phys.Lett., Vol.85, No.6, August 2004 and Spark-eroded particles:Influence of processing parameters.J.Appl.Phys., Vol.95, No.3, February 2004) method that a kind of method with spark eroding prepares the hollow nickel powder proposed, its method is in vacuum-packed vibration container device, with the liquid nitrogen is working solution, tool-electrode and workpiece material are metallic nickel, adopt the mode of tool-electrode rotation to process, the hollow nickel powder particle diameter of preparing is concentrated and is distributed between tens nanometers to 50 micron.Weak point is that device is complicated, and the use of liquid nitrogen exists potential safety hazard and cost higher.
Summary of the invention
The present invention has overcome deficiency of the prior art, provides a kind of device simple, the method for preparing the hollow nickel powder that safety and cost are low.
The method that spark eroding prepares powder is to make the spark discharge that constantly produces pulse feature between the tool-electrode that is immersed in the working solution and the workpiece, the part, the TRANSIENT HIGH TEMPERATURE that produce when relying on each the discharge, in discharge channel, produce a large amount of heat, make the instantaneous gasification of localized metallic and the fusing of electrode surface, thereby the micro-one by one ablation of metal material is got off, enter into working solution, the micro-material of these gasifications or fusing cools down in working solution and just forms particle.Because the effect of surface tension and cohesive force makes the material of dishing out have minimum surface area, forming tiny particle during condensation is ball.The part that electrode material is melted is dished out with liquid phase, after molten drop is thrown into working solution, can rapid cooling be condensed into solid sphere owing to surrounding medium conducts heat.Can dish out with gas phase in the electrode material top layer, the vapor phase metal that is thrown in the liquid medium can form the vapour bubble that contacts with the low-temperature working liquid phase.Because the result of conducting heat in the vapour bubble border, metal meeting rapid cooling, cohesion and the crystallization of boundary vicinity form a housing that is similar to the vapour bubble shape.And body in metal vapors in the phase transition process of cooling, cohesion and crystallization, volume can obviously dwindle, it is hollow causing in the metal ball body.Therefore to have part be hollow to the particle that comes out of common electrical spark erosion, but the shared ratio of hollow particle is very little.If can improve the vaporized ratio of electrode material, the ratio of hollow particle will enlarge markedly so.Mixing the spark eroding of Si powder can be so that discharging gap increases, the discharge channel chap, the energy density step-down, pit " big and shallow " in electrode surface formation, with respect to the common electrical spark erosion, the ratio that the electrode material that mixed Si powder spark eroding is dished out is dished out with vaporous form increases, and the ratio of therefore mixing the hollow particle of Si powder spark eroding preparation enlarges markedly.
The present invention is achieved by the following technical solutions: utilize the electric spark device, mixed liquor with deionized water and silica flour is a working solution, tool-electrode and workpiece are made by metallic nickel, mixed liquor after the processing after filtration, dry, remove Si and obtain spherical hollow nickel powder, the hollow nickel powder apparent density that makes is at 2.02～2.76g/cm
3Between, particle diameter is concentrated and to be distributed between tens nanometers to 50 micron.
When thick powder enters discharging gap, can be at thick powder place form and concentrate discharge or short circuit, make processing unstable, experiment shows that the silica flour particle diameter of electric spark working solution is advisable less than 45 microns.When the concentration of powder is increased to a certain degree in the working solution, the flowability of powder working solution reduces, and easily forms powder deposition at finished surface, thereby destroys the discharge condition in gap, bad phenomenon such as the generation discharge is concentrated are so the silica flour concentration of electric spark working solution is preferably 4～40g/L.
Compared with prior art, the present invention does not need the processing environment of vacuum, does not need security is low and price is higher liquid nitrogen as working solution, the deionized water that only needs to mix the Si powder gets final product as working solution, therefore apparatus of the present invention are simple, the processing safety height, and cost is low.
Description of drawings
Fig. 1 is the XRD spectrum of mixing the hollow spheres Ni powder that Si powder spark eroding method makes.
Fig. 2 is the laser particle size distribution map of the hollow nickel particle of embodiment 1 acquisition.
Fig. 3 is the stereoscan photograph of the hollow nickel particle of embodiment 1 acquisition.
Fig. 4 is the stereoscan photograph of the hollow nickel particle of embodiment 3 acquisitions.
The specific embodiment
Embodiment 1
Metal nickel plate is processed into rectangular tool-electrode and block workpiece, and tool-electrode and surface of the work are removed oxide-film and made its surfacing.Deionized water and silica flour are mixed into equally distributed suspension, and concentration is 4g/L.Install tool-electrode and workpiece, the working solution that mixes is poured in the working groove, open electric mixer.Set the discharge parameter of electric spark equipment: low-tension current is 45A, and pulse width is 90 μ s, and the pulse spacing is 15 μ s.Adding the man-hour peak point current is 6A.With working solution vacuum filtration, drying,, adopt distilled water repeatedly to wash then after the completion of processing, be drying to obtain the hollow spherical nickel powder after the washing dried powder and excess NaOH solution reaction.
The apparent density of powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition is respectively: 2.90g/cm
3And 2.02g/cm
3
Granularity is respectively smaller or equal to the accumulative perception of 51.5 μ m in the powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition: 94.53% and 91.02%.
Embodiment 2
Metal nickel plate is processed into rectangular tool-electrode and block workpiece, and tool-electrode and surface of the work are removed oxide-film and made its surfacing.Deionized water and silica flour are mixed into equally distributed suspension, and concentration is 10g/L.Install tool-electrode and workpiece, the working solution that mixes is poured in the working groove, open electric mixer.Set the discharge parameter of electric spark equipment: low-tension current is 45A, and pulse width is 120 μ s, and the pulse spacing is 15 μ s.Adding the man-hour peak point current is 12A.With working solution vacuum filtration, drying,, adopt distilled water repeatedly to wash then after the completion of processing, be drying to obtain the hollow spherical nickel powder after the washing dried powder and excess NaOH solution reaction.
The apparent density of powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition is respectively: 3.14g/cm
3And 2.21g/cm
3
Granularity is respectively smaller or equal to the accumulative perception of 51.5 μ m in the powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition: 94.72% and 94.51%.
Embodiment 3
Metal nickel plate is processed into rectangular tool-electrode and block workpiece, and tool-electrode and surface of the work are removed oxide-film and made its surfacing.Deionized water and silica flour are mixed into equally distributed suspension, and concentration is 6g/L.Install tool-electrode and workpiece, the working solution that mixes is poured in the working groove, open electric mixer.Set the discharge parameter of electric spark equipment: low-tension current is 45A, and pulse width is 200 μ s, and the pulse spacing is 15 μ s.Adding the man-hour peak point current is 20A.With working solution vacuum filtration, drying,, adopt distilled water repeatedly to wash then after the completion of processing, be drying to obtain the hollow spherical nickel powder after the washing dried powder and excess NaOH solution reaction.
The apparent density of powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition is respectively: 3.66g/cm
3And 2.76g/cm
3
Granularity is respectively smaller or equal to the accumulative perception of 51.5 μ m in the powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition: 90.85% and 94.55%.
Embodiment 4
Metal nickel plate is processed into rectangular tool-electrode and block workpiece, and tool-electrode and surface of the work are removed oxide-film and made its surfacing.Deionized water and silica flour are mixed into equally distributed suspension, and concentration is 20g/L.Install tool-electrode and workpiece, the working solution that mixes is poured in the working groove, open electric mixer.Set the discharge parameter of electric spark equipment: low-tension current is 45A, and pulse width is 200 μ s, and the pulse spacing is 15 μ s.Adding the man-hour peak point current is 20A.With working solution vacuum filtration, drying,, adopt distilled water repeatedly to wash then after the completion of processing, be drying to obtain the hollow spherical nickel powder after the washing dried powder and excess NaOH solution reaction.
The apparent density of powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition is respectively: 3.66g/cm
3And 2.49g/cm
3
Granularity is respectively smaller or equal to the accumulative perception of 51.5 μ m in the powder that common electrical spark erosion and the spark eroding of mixed Si powder make under this discharging condition: 90.85% and 94.68%.
For determining the phase composition of the powder that the present invention prepares, powder is carried out the XRD analysis of spectrum, see Fig. 1, powder is made up of metal Ni basically as shown in Figure 1, and small amount of N iO is arranged.For determining the particle size range of the powder that the present invention prepares, the powder of embodiment 1 is carried out laser particle size analysis, Fig. 2 is the laser particle size distribution map of the hollow nickel particle that obtains of embodiment 1.For observing the apparent pattern and the hollow situation of the powder that the present invention prepares, powder to embodiment 1 and embodiment 3 carries out scanning electron microscopic observation, Fig. 3 is the stereoscan photograph of the hollow nickel particle of embodiment 1 acquisition, and Fig. 4 is the stereoscan photograph of the hollow nickel particle of embodiment 3 acquisitions.
Claims (4)
1. a method that adopts spark eroding to prepare the hollow micro-nano-nickel powder is characterized in that working solution is the mixed liquor of deionized water and silica flour, and tool-electrode and workpiece are made by metallic nickel, and the apparent density of nickel powder is at 2.02～2.76g/cm
3Between.
2. employing spark eroding according to claim 1 prepares the method for hollow micro-nano-nickel powder, and the silica flour concentration that it is characterized in that described working solution is 4～40g/L.
3. employing spark eroding according to claim 1 prepares the method for hollow micro-nano-nickel powder, and the silica flour concentration that it is characterized in that described working solution is 10～20g/L.
4. employing spark eroding according to claim 1 prepares the method for hollow micro-nano-nickel powder, and the silica flour particle diameter that it is characterized in that described working solution is less than 45 microns.
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| CN100551588C true CN100551588C (en) | 2009-10-21 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011219830A (en) * | 2010-04-12 | 2011-11-04 | Jfe Mineral Co Ltd | Nickel fine particle, mixture of nickel fine particle, and conductive paste |
| CN102274975B (en) * | 2011-07-12 | 2014-02-26 | 四川大学 | Method for preparing metal micro-nano hollow spherical powder |
| CN102335749A (en) * | 2011-07-12 | 2012-02-01 | 四川大学 | Device for preparing metal micro-nano hollow sphere powder |
| CN102744477B (en) * | 2012-06-29 | 2014-04-23 | 南京航空航天大学 | Preparation method and device of nano particle by using shock wave assistant ultrashort pulse electricity discharge |
| 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 |
| CN113020613B (en) * | 2021-03-12 | 2022-06-03 | 深圳航天科创实业有限公司 | Hollow powder and method for producing same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5133800A (en) * | 1991-03-11 | 1992-07-28 | General Electric Company | Fabrication of cryogenic refrigerator regenerator materials by spark erosion |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5133800A (en) * | 1991-03-11 | 1992-07-28 | General Electric Company | Fabrication of cryogenic refrigerator regenerator materials by spark erosion |
Non-Patent Citations (2)
| Title |
|---|
| 电火花腐蚀制备Ni粉. 李忠丽，李翔龙，文玉华，李宁.微细加工技术，第无卷第2期. 2007 |
| 电火花腐蚀制备Ni粉. 李忠丽，李翔龙，文玉华，李宁.微细加工技术，第无卷第2期. 2007 * |
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