WO2021088217A1 - 新型球形粉末及其制备方法 - Google Patents

新型球形粉末及其制备方法 Download PDF

Info

Publication number
WO2021088217A1
WO2021088217A1 PCT/CN2019/126466 CN2019126466W WO2021088217A1 WO 2021088217 A1 WO2021088217 A1 WO 2021088217A1 CN 2019126466 W CN2019126466 W CN 2019126466W WO 2021088217 A1 WO2021088217 A1 WO 2021088217A1
Authority
WO
WIPO (PCT)
Prior art keywords
electrode
workpiece
spherical powder
powder
preparing
Prior art date
Application number
PCT/CN2019/126466
Other languages
English (en)
French (fr)
Inventor
徐辉
姚青
Original Assignee
深圳航科新材料有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CN201911082147.9A external-priority patent/CN110961644B/zh
Priority claimed from CN201911082177.XA external-priority patent/CN110961646B/zh
Application filed by 深圳航科新材料有限公司 filed Critical 深圳航科新材料有限公司
Priority to US17/775,192 priority Critical patent/US20220395899A1/en
Priority to EP19951796.2A priority patent/EP4056301A4/en
Priority to JP2022526418A priority patent/JP7407927B2/ja
Priority to CA3163929A priority patent/CA3163929C/en
Publication of WO2021088217A1 publication Critical patent/WO2021088217A1/zh

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/13—Use of plasma
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/10—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/15—Millimeter size particles, i.e. above 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • 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
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the invention relates to the field of preparation of metal powders, in particular to a novel spherical powder and a preparation method thereof.
  • the processes for preparing spherical metal powder mainly include gas atomization and rotating electrodes.
  • Scholars at home and abroad have conducted a lot of research on the structure and properties of the metal powder printed parts prepared by the above process.
  • Some researchers have compared the performance of gas atomization and rotating electrode powder used in 3D printing to manufacture parts.
  • the porosity of the nickel-based superalloy powder molded parts prepared by the gas atomization method is the rotating electrode method. 25 times, this is mainly due to the fluidity of metal powder and hollow powder and other factors that caused micro-cracks and holes in the molding process of parts.
  • the advantages of aerosolized powder used in additive manufacturing of parts are mature and stable technology, small powder particle size, fine structure, and less element segregation, which is conducive to improving the mechanical properties of parts and reducing the cost of powder used in the laser melting process of selected areas; but hollow Factors such as powder and satellite powder increase the risk of increased pore content and micro-cracks in parts; the advantage of rotating electrode powder for additive manufacturing of parts is that there are very few hollow powder and satellite spheres, and the parts are compactly formed and the surface roughness is small. , Is beneficial to fracture and fatigue performance, but the powder preparation cost is high, the particle size range is narrow, and the powder particle size is larger, which is difficult to use in 3D printing technology.
  • the present invention provides a method for preparing a novel spherical powder.
  • the prepared metal powder has small particle size, regular particle shape, good sphericity, and low content of hollow powder and satellite powder.
  • a method for preparing a novel spherical powder includes the following steps:
  • the electrode and the workpiece are placed at the two poles of the power supply, and the discharge gap between the electrode and the workpiece is adjusted by the motion control system to generate arc plasma.
  • the arc plasma acts on the surface of the electrode and the workpiece, the electrode and the workpiece surface are promoted Melting to form a molten zone.
  • a fluid medium is introduced into the discharge gap.
  • the arc plasma working form is changed, and the molten zone is promoted.
  • Produce a small explosion, crush and throw away the material located in the melting zone the crushed molten material is condensed in the fluid medium, and the condensed fine spherical powder is collected;
  • the electrode is provided with a hollow cavity and/or the workpiece is provided with a hollow cavity.
  • the present invention has the following beneficial effects:
  • the preparation method of the novel spherical powder of the present invention places the electrode and the workpiece on the two poles of the power supply, and uses the arc plasma as a high-density energy heat source to act on the surface of the electrode and the workpiece to melt the surface of the electrode and the workpiece to form tiny particles. Melt pit is the melting zone. At the same time, a fluid medium is passed between the electrode and the workpiece. Through the relative displacement of the electrode and the workpiece and the arc-shifting coupling effect of the fluid medium, the material in the molten zone is continuously thrown away from the pit. , Improve the discharge rate of particles and improve production efficiency.
  • controlling the rotating speed of the electrode or the rotating speed of the workpiece, and controlling the flow rate of the fluid medium can change the working state of the arc plasma, cause a small explosion in the melting zone, crush and throw away the material in the melting zone, and further refine the material.
  • the crushed and thrown material in the molten zone is rapidly cooled in the fluid medium, and the fine particles are solidified into spherical powder due to the shrinkage of surface tension during the condensation process, and the cooled fine spherical powder is collected.
  • the pulverized fine particles are rapidly condensed in the fluid medium, and the resulting fine spherical powder has good sphericity.
  • the spherical powder produced has a small particle size, a uniform particle size, and a particle shape Regularity, good sphericity, low content of hollow powder and satellites.
  • the fine spherical powder can also be cleaned, dried and sieved, and spherical powder with a particle size of 10 ⁇ m-250 ⁇ m can be collected to give the powder better fluidity.
  • the flow rate is in the range of 0.5L/min-500L/min, which is beneficial to increase the yield of fine powder and collect more spherical powders with particle diameters of 10 ⁇ m-250 ⁇ m.
  • a horn-shaped buffer part and a stepped multi-stage powder collecting device are used to collect the fine spherical powder in the fluid medium.
  • the fine spherical powder in the fluid medium The powder can also be deposited to avoid the loss or splashing of the fine spherical powder with the fluid medium, and further achieve the purpose of improving the yield of the fine powder.
  • Figure 1 is a schematic diagram of the principle of powder production by arc micro-explosion technology
  • Example 2 is a schematic diagram of the spherical metal powder of Example 1;
  • Example 3 is a schematic diagram of the spherical metal powder of Example 2.
  • Example 4 is a schematic diagram of the spherical metal powder of Example 3.
  • Example 5 is a schematic diagram of the spherical metal powder of Example 4.
  • FIG. 6 is a schematic diagram of the spherical metal powder of Example 5.
  • a method for preparing a novel spherical powder includes the following steps:
  • the electrode and the workpiece are placed at the two poles of the power supply, and the discharge gap between the electrode and the workpiece is adjusted by the motion control system to generate arc plasma.
  • the arc plasma acts on the surface of the electrode and the workpiece, the electrode and the workpiece surface are promoted Melting to form a molten zone.
  • a fluid medium is introduced into the discharge gap.
  • the arc plasma working form is changed, and the molten zone is promoted.
  • Produce a small explosion, crush and throw away the material located in the melting zone the crushed molten material is condensed in the fluid medium, and the condensed fine spherical powder is collected;
  • the electrode is provided with a hollow cavity and/or the workpiece is provided with a hollow cavity.
  • placing the electrode and the workpiece on the two poles of the power source can be understood as connecting the electrode to the anode of the power source and connecting the workpiece to the cathode of the power source. It can also be understood that the electrode is connected to the cathode of the power source, and the workpiece is connected to the anode of the power source.
  • This method breaks through the limitation that the workpiece can only be connected to the cathode of the power supply in the existing process, and there is no special restriction on the appearance of the workpiece.
  • by changing the polarity of the electrode and the workpiece by changing the electrode and the electrode of the workpiece. It can also improve the efficiency of the spherical powder preparation process and the yield of fine powder.
  • the power source drives the electrode to rotate.
  • the electrode is provided with a hollow cavity.
  • the electrode provided with a hollow cavity is an electrode provided with a single tube, multiple tubes and hollow nests.
  • the electrode is an electrode provided with a single tube, and its partial structure is shown on the left side of FIG. 1.
  • the single tube electrode is provided with an electrode assembly 110 and a channel tube 120 located between the electrode assemblies.
  • the channel tube is provided with an inlet and an outlet, and the fluid medium can enter from the inlet in the channel tube and flow out from the outlet in the channel tube.
  • the outlet of the channel pipe faces the workpiece, so that the fluid medium can flow to the workpiece.
  • the fluid medium can also enter from the outside 130 of the channel tube, flow along the outer surface of the electrode assembly to the workpiece.
  • the fluid medium can be introduced separately from the hollow cavity or outside the hollow cavity of the electrode, or can also be introduced from the hollow cavity and outside the hollow cavity of the electrode at the same time.
  • the fluid medium flowing in from the hollow cavity and the outside of the hollow cavity may be the same fluid medium or different fluid medium.
  • the fluid medium introduced into the hollow cavity and outside the hollow cavity is independently selected from a water-based medium and/or an inert gas, and the inert gas includes nitrogen.
  • the water-based medium is preferably distilled water.
  • the power source drives the workpiece to rotate.
  • the workpiece is provided with a hollow cavity.
  • the fluid medium can be separately introduced from the hollow cavity or outside of the hollow cavity of the workpiece, or can also be introduced from the hollow cavity and outside the hollow cavity of the workpiece at the same time.
  • the introduction of the fluid medium from the hollow cavity of the workpiece can be understood as: the fluid medium flows to the electrode along the outer surface of the workpiece.
  • the fluid medium flowing in from the hollow cavity and the outside of the hollow cavity may be the same fluid medium or different fluid medium.
  • the fluid medium introduced into the hollow cavity and outside the hollow cavity is independently selected from a water-based medium and/or an inert gas, and the inert gas includes nitrogen.
  • the water-based medium is preferably distilled water.
  • the power supply is a DC pulse power supply, a DC constant current power supply, an AC pulse power supply or an AC constant current power supply.
  • the power source is a pulsed power source
  • the pulse width is 2 ⁇ s to 200,000 ⁇ s
  • the pulse interval is 2 ⁇ s to 200,000 ⁇ s.
  • the relative position of the electrode and the workpiece is adjusted by the motion control system to obtain an arc plasma in an ideal discharge state.
  • the discharge gap between the electrode and the workpiece is adjusted to generate arc plasma.
  • the discharge gap that is, the distance between the discharge end of the electrode and the surface of the workpiece, is 0.1mm-100mm. This distance enables the arc plasma to act on the electrode and the workpiece, and can ensure that the fluid medium has a large pressure when it passes through.
  • the center temperature of the arc plasma is as high as 10000K, which can melt most of the conductive materials. Under its action, the surface of the workpiece melts, forming a small molten pit with a radius of 0.5mm-2mm, that is, the melting zone. At this time, the electrodes face each other. For high-speed rotating mechanical movement of the workpiece.
  • the power supply parameters of the power supply further include: the gap voltage is 10-160V, and the discharge current is 5A-1000A.
  • the electrode is a copper electrode or a graphite electrode.
  • Fig. 1 shows a preferred embodiment of introducing a fluid medium.
  • the arrow in 1 indicates the flow direction of the fluid medium.
  • An enlarged view of the discharge gap on the right side of FIG. 1, 210 is an arc plasma, and 220 is a molten pit.
  • controlling the rotating speed of the electrode or the rotating speed of the workpiece, and controlling the flow rate of the fluid medium can change the working state of the arc plasma, cause a small explosion in the melting zone, crush the material in the melting zone, and further refine the material.
  • powders with different particle size distributions can be obtained by controlling the motion control system, power supply parameters, rotation speed, and flow rate.
  • the rotation speed of the electrode is 100r/min-60000r/min, more preferably 3000r/min-60000r/min.
  • the rotation speed of the workpiece is 100 r/min-60000 r/min, more preferably 3000 r/min-60000 r/min.
  • the flow rate when the fluid medium is initially introduced is 0.5L/min-500L/min.
  • Controlling the rotation speed of the electrode or metal workpiece within the above range, and controlling the flow rate of the fluid medium at the time of initial introduction within the above range, is beneficial to increase the yield of fine powder and collect more metals with a particle size of 10 ⁇ m-250 ⁇ m powder.
  • the electrode and the workpiece are both conductive materials or weakly conductive materials, and the material of the electrode and the workpiece may be the same or different.
  • the above method is suitable for the preparation of a variety of conductive powders.
  • the above method does not make too many requirements on the shape of the workpiece, and the workpiece can be in a regular or irregular shape such as a rod shape or a block shape.
  • the pulverized material is rapidly cooled in a fluid medium, and the pulverized fine particles are solidified into fine spherical powder due to the shrinkage of surface tension during the condensation process, and the condensed fine spherical powder is collected.
  • the device used to collect the above-mentioned fine spherical powder in a fluid medium is a multi-stage powder collecting device
  • the multi-stage powder collecting device is provided with a horn-shaped buffer part and is not smoothly connected to the horn-shaped buffer
  • the ladder-shaped collection platform, each level of ladder corresponds to a collection platform.
  • the condensed fine spherical powder flows out of the multi-stage powder collecting device along with the fluid medium.
  • the fine spherical powder can be deposited on the steps to prevent the fluid medium from being directly washed into the powder collecting box. In this way, the fine spherical powder is lost or splashed along with the fluid medium to ensure the integrity of powder collection and achieve the purpose of improving the yield of fine powder.
  • the condensed fine spherical powder can also be cleaned, dried and sieved.
  • the cleaning agent can be selected from carbonic acid cleaning agent, alcohol cleaning agent or ether cleaning agent, to clean the oil stains in the powder.
  • the carbonic acid cleaning agent, alcohol cleaning agent, or ether cleaning agent has a low melting point, is easy to volatile, and is convenient for subsequent drying.
  • the cleaned powder is dried in a vacuum drying box or a resistance box. After drying, the powder is sieved in a grading sieve to collect particles with a particle size of 10 ⁇ m-250 ⁇ m. Preferably, particles with a particle size of 10 ⁇ m-103 ⁇ m are collected.
  • the pulverized fine particles are rapidly condensed in the fluid medium, and the obtained primary powder has good sphericity, which gives the powder better fluidity.
  • the novel spherical powder prepared by the above method has small particle size, high fine powder yield, regular particle shape, good sphericity, low content of hollow powder and satellite powder, and good fluidity.
  • This embodiment provides a method for preparing a novel spherical powder, which includes the following steps:
  • the size is 100mm*100mm*20mm, after cleaning it and decontamination, connect the cathode of the power supply. Connect the graphite electrode with the single tube to the positive pole of the power supply. The distance between the discharge end of the electrode and the workpiece is 0.5 mm.
  • the multi-tube refers to a plurality of channel tubes located between the electrode assemblies, and the outlet of the channel tube faces the block 304 stainless steel.
  • the power supply parameters are set as follows: the gap voltage is 45V-55V, the discharge current is 500A, the pulse width is 2000 ⁇ s, the pulse interval is 200 ⁇ s, the power is turned on, and the rotation speed of the electrode is controlled to 5000 r/min.
  • distilled water was introduced into a number of the channel tubes, and the flow rate was 50 L/min.
  • the arc plasma acts on the graphite electrode and the surface of the workpiece, and the molten material is continuously discharged with distilled water, exploded and crushed, and finally condensed into fine spherical powder in the distilled water, which is a new type of spherical powder.
  • This embodiment provides a method for preparing a novel spherical powder, which includes the following steps:
  • the rod-shaped TC4 (titanium alloy) is used as a workpiece for processing, and the outer diameter is The inner diameter is The length is 100mm. After cleaning and decontamination, connect the anode of the power supply. Connect the TC4 electrode to the cathode of the power supply, the distance between the discharge end of the electrode and the workpiece is 1 mm, the rod-shaped TC4 is provided with a channel tube, and the outlet of the channel tube faces the TC4 electrode.
  • the power supply parameters are set as follows: the gap voltage is 45V-55V, the discharge current is 500A, the pulse width is 2000 ⁇ s, the pulse interval is 200 ⁇ s, the power is turned on, and the rotation speed of the tube rotating electrode is controlled to 3000 r/min.
  • distilled water is introduced into the channel tube and the channel tube, and the flow rate of the channel tube is 50 L/min.
  • the arc plasma acts on the surface of the electrode and the workpiece, and the molten material is continuously discharged with distilled water, exploded and crushed, and finally condensed into fine spherical powder in the distilled water, which is a new type of spherical powder.
  • the weight of the metal workpiece is determined to be reduced by 850g, that is, the processing efficiency of the above method reaches 1700g/h.
  • the obtained new spherical powder is shown in Figure 3.
  • the obtained spherical powder has a small particle size, a regular particle shape, a good sphericity, and a low content of hollow powder and satellite powder.
  • This embodiment provides a method for preparing a novel spherical powder, which includes the following steps:
  • a massive nickel alloy is used as a metal workpiece with a size of 100mm*100mm*20mm. After cleaning and decontamination, connect the cathode of the power supply. Connect the graphite electrode of the tube to the positive electrode of the tube. The distance between the discharge end of the electrode and the workpiece is 0.5 mm.
  • the multi-tube refers to a plurality of channel tubes located between the electrode assemblies, and the outlet of the channel tube faces the massive nickel alloy.
  • the power supply parameters are set as follows: the gap voltage is 45V-55V, the discharge current is 500A, the pulse width is 2000 ⁇ s, the pulse interval is 200 ⁇ s, the power is turned on, and the rotation speed of the electrode is controlled to 3000 r/min.
  • distilled water is introduced into a number of the channel tubes, and the flow rate is 20 L/min when passing in.
  • the arc plasma acts on the surface of the graphite electrode and the nickel alloy workpiece.
  • the molten material is continuously discharged with distilled water, exploded and crushed, and finally condensed into fine spherical powder in the distilled water, followed by the distilled water into the stepped multi-stage Powder collection device.
  • the above-mentioned fine spherical powder is cleaned with a carbonic acid cleaning agent, dried after cleaning, and sieved after drying to collect particles with a particle size of 10 ⁇ m-250 ⁇ m, which is a new type of spherical powder, as shown in Figure 4.
  • This embodiment provides a method for preparing a novel spherical powder, which includes the following steps:
  • the rod-shaped copper alloy is used as the metal workpiece, and the outer diameter is The inner diameter is The length is 100mm. After cleaning and decontamination, connect the anode of the power supply.
  • the copper electrode is connected to the cathode of the power supply, the distance between the discharge end of the electrode and the workpiece is 1 mm, the rod-shaped copper alloy is provided with a channel tube, and the outlet of the channel tube faces the copper electrode.
  • the power supply parameters are set as follows: the gap voltage is 45V-55V, the discharge current is 500A, the pulse width is 2000 ⁇ s, the pulse interval is 200 ⁇ s, the power is turned on, and the rotation speed of the electrode is controlled to 3000 r/min.
  • distilled water is introduced into the channel tube and outside the channel tube, and the flow rate is 20 L/min when it is introduced.
  • the arc plasma acts on the surface of the copper electrode and the copper alloy workpiece.
  • the molten material is continuously discharged with distilled water, exploded and crushed, and finally condensed into fine spherical powder in the distilled water, followed by the distilled water into the stepped multi-stage Powder collection device.
  • the above-mentioned fine spherical powder is cleaned with a carbonic acid cleaning agent, dried after cleaning, and then sieved after drying to collect particles with a particle size of 10 ⁇ m-250 ⁇ m, which is a new type of spherical powder, as shown in Figure 5.
  • the obtained spherical powder with a particle size of 10 ⁇ m-250 ⁇ m is calculated as the ratio of the collected powder weight to the total weight of the workpiece, that is, the yield of fine powder reaches 86.1%.
  • This embodiment provides a method for preparing a novel spherical powder, which is basically the same as the preparation method of Example 1, except that the rotation speed of the electrode and the flow rate of distilled water are different. It includes the following steps:
  • a massive nickel alloy is used as a metal workpiece with a size of 100mm*100mm*20mm. After cleaning and decontamination, connect the cathode of the power supply. Connect the graphite tube to the anode of the electric tube. The distance between the discharge end of the electrode and the workpiece is 0.5 mm.
  • the multi-tube refers to a plurality of channel tubes located between the electrode assemblies, and the outlet of the channel tube faces the massive nickel alloy.
  • the power supply parameters are set as follows: the gap voltage is 45V-55V, the discharge current is 500A, the pulse width is 2000 ⁇ s, the pulse interval is 200 ⁇ s, the power is turned on, and the rotation speed of the electrode is controlled to 1000 r/min.
  • distilled water is introduced into a number of the channel tubes, and the flow rate is 20 L/min when passing in.
  • the arc plasma acts on the surface of the graphite electrode and the nickel alloy workpiece.
  • the molten material is continuously discharged with distilled water, exploded and crushed, and finally condensed into fine spherical powder in the distilled water, followed by the distilled water into the stepped multi-stage Powder collection device.
  • the above-mentioned fine spherical powder is cleaned with a carbonic acid cleaning agent, dried after cleaning, and sieved after drying to collect particles with a particle size of 10 ⁇ m-250 ⁇ m, which is a new type of spherical powder, as shown in FIG. 6.
  • the powder fluidity is to measure the time required for 50g of powder to flow through the standard size funnel hole. Take the arithmetic average of three times.
  • Measurement procedure Block the outlet of the funnel with your fingers, and put the sample into the funnel. Make sure to fill the bottom of the funnel with powder. When the hole of the funnel is opened, start the stopwatch. When the powder in the funnel is all out, stop the stopwatch. Record time, accurate to 0.1s.
  • Example 3 The powder fluidity of Example 3 was 21.57s; the powder fluidity of Example 4 was 22.88s; the powder fluidity of Example 5 was 25.34s.
  • Example 3-5 has a high yield, uniform particle size distribution, good fluidity, good sphericity, hollow powder and satellite powder The content is low.
  • Example 5 changing the rotation speed of the electrode and the initial flow rate of the fluid medium has an effect on the yield of fine powder. Under the process parameters of Example 3, the fine powder is recovered The rate is higher.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

一种球形粉末及其制备方法。步骤如下：将电极和工件置于电源的两极，通过运动控制系统调整所述电极和工件的放电间隙产生电弧等离子体，所述电弧等离子体作用于所述电极和工件表面，使所述电极和工件表面熔融，形成熔融区，同时，在所述放电间隙引入流体介质，控制所述流体介质的流速，控制所述电极或工件的相对转速，引起电弧等离子体工作形态的改变，使所述熔融区产生微小爆炸，抛离并粉碎位于所述熔融区的材料，粉碎后的所述材料在所述流体介质中冷凝，收集冷凝后的微细球形粉末；所述电极设置有中空腔或所述工件设置有中空腔。上述方法制得的球形粉末粒径小、颗粒形状规则、球形度好、空心粉和卫星粉含量低。

Description

新型球形粉末及其制备方法 技术领域
本发明涉及金属粉末的制备领域，特别是涉及一种新型球形粉末及其制备方法。
背景技术
随着工业技术的不断发展，新型材料和成型技术不断推陈出新，并广泛应用在国防和民用核心设备上，而这些设备普遍要面对复杂恶劣的工作环境，这就要求新材料应当具有非常高的强度和韧性，以及非常高的抗蠕变、抗疲劳、抗氧化和抗腐蚀的能力。伴随着对新材料性能上的高要求，也带来了这类材料的制备变得非常困难的问题。目前，这类材料的产品和零件大多选择近净成型技术来制备，例如：粉末冶金法、增材制造(3D打印技术)和注射成型。金属粉末是这些成型技术中最重要的原材料之一，金属粉末的稳定性、球形度、纯度，对采用上述成型技术制备新材料的加工性能具有非常重要的影响。
传统工艺中，制备球形金属粉末的工艺主要有气雾化类和旋转电极类。国内外学者对上述工艺制备的金属粉末打印工件的组织性能进行了大量研究。有研究者对比了气雾化和旋转电极粉末用于3D打印制造零部件的性能，在同一工艺条件下，使用气雾化法制备的镍基高温合金粉末成型零部件的孔隙率是旋转电极法的25倍，这主要是由于金属粉末流动性以及空心粉等因素造成零部件成型过程中的产生了微裂纹和孔洞。Arash等人采用3D打印技术制备零部件对比结果表明，使用气雾化粉末成型的零部件孔隙数量是相同工艺下旋转电极粉末 成型零部件的3倍；但气雾化粉末成型零部件的平均晶粒尺寸更细小。目前气雾化粉末用于增材制造零部件的优势在于工艺成熟稳定，粉末粒径小，组织细小、元素偏析少，有利于提高零部件力学性能，降低选区激光熔化工艺用粉成本；但空心粉和卫星粉等因素增加了零部件内孔隙含量和微裂纹增多的风险；旋转电极粉末用于增材制造零部件的优势在于空心粉和卫星球极少，零部件成型致密，表面粗糙度小，对断裂及疲劳性能有利，但粉末制备成本高，粒度范围分布较窄，粉末粒径较大，用于3D打印技术比较困难。
发明内容
基于此，本发明提供一种新型球形粉末的制备方法，制得的金属粉末粒径较小、颗粒形状规则、球形度好、空心粉和卫星粉含量低。
具体技术方案为：
一种新型球形粉末的制备方法，包括以下步骤：
将电极和工件置于电源的两极，通过运动控制系统调整所述电极和工件的放电间隙产生电弧等离子体，所述电弧等离子体作用于所述电极和工件表面时，促使所述电极和工件表面熔融，形成熔融区，同时，在所述放电间隙引入流体介质，通过控制所述流体介质的流速，以及所述电极或工件的相对转速，引起电弧等离子体工作形态的改变，促使所述熔融区产生微小爆炸，粉碎并抛离位于所述熔融区的材料，粉碎后的所述熔融材料在所述流体介质中冷凝，收集冷凝后的微细球形粉末；
所述电极设置有中空腔和/或所述工件设置有中空腔。
与现有技术相比，本发明具有以下有益效果：
本发明所述的新型球形粉末的制备方法将电极和工件分别置于电源的两 极，以电弧等离子体作为高密度的能量热源，作用于电极和工件表面，使电极和工件表面熔融，形成微小的熔坑，即熔融区，同时，在电极和工件之间通入流体介质，通过电极和工件的相对移位和流体介质的移弧耦合作用，将熔融区的材料连续的从熔坑中抛离，提高颗粒的排出率，提高生产效率。同时，控制电极的转速或工件的转速、控制流体介质的流速，能够改变电弧等离子体的工作状态，使熔融区产生微小爆炸，粉碎并抛离位于熔融区的材料，将材料进一步细化，然后，粉碎抛离的熔融区材料在流体介质中急速冷却，细小颗粒在冷凝过程中因表面张力的收缩作用固化成球形的粉末，收集冷却后的微细球形粉末。其中，粉碎后的细小颗粒在流体介质中迅速冷凝，得到的微细球形粉末具有好的球形度。通过上述方法，解决了目前雾化制粉技术空心球和卫星粉多，旋转电极制粉技术效率低、粉末粒径大等诸多问题，制得的球形粉末粒径较小、粒度均匀、颗粒形状规则、球形度好、空心粉和卫星份含量低。
进一步地，还可以对微细球形粉末进行清洗、烘干和筛分，收集粒径在10μm-250μm的球形粉末，赋予粉末更好的流动性。控制所述运动控制系统调整所述电极和工件的相对位置在0.1mm-100mm内，控制所述电极或工件的转速在100r/min-60000r/min范围内，控制所述流体介质初始通入时的流速在0.5L/min-500L/min范围内，有利于提高细粉收得率，收集到更多的粒径在10μm-250μm的球形粉末。
进一步地，采用喇叭状的缓冲部和阶梯状的多级收粉装置，对流体介质中的微细球形粉末进行收集，随着流体介质流经缓冲部和每一级阶梯，流体介质中的微细球形粉末也可以沉积下来，避免微细球形粉末随着流体介质流失或飞溅，进一步实现提高细粉收得率的目的。
附图说明
图1为电弧微爆技术生产粉末的原理示意图；
图2为实施例1的球形金属粉末示意图；
图3为实施例2的球形金属粉末示意图；
图4为实施例3的球形金属粉末示意图；
图5为实施例4的球形金属粉末示意图；
图6为实施例5的球形金属粉末示意图。
具体实施方式
以下结合具体实施例对本发明作进一步详细的说明。本发明可以以许多不同的形式来实现，并不限于本文所描述的实施方式。相反地，提供这些实施方式的目的是使对本发明公开内容理解更加透彻全面。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。
一种新型球形粉末的制备方法，包括以下步骤：
将电极和工件置于电源的两极，通过运动控制系统调整所述电极和工件的放电间隙产生电弧等离子体，所述电弧等离子体作用于所述电极和工件表面时，促使所述电极和工件表面熔融，形成熔融区，同时，在所述放电间隙引入流体介质，通过控制所述流体介质的流速，以及所述电极或工件的相对转速，引起电弧等离子体工作形态的改变，促使所述熔融区产生微小爆炸，粉碎并抛离位于所述熔融区的材料，粉碎后的所述熔融材料在所述流体介质中冷凝，收集冷 凝后的微细球形粉末；
所述电极设置有中空腔和/或所述工件设置有中空腔。
其中，将电极和工件置于电源的两极，可以理解为：将所述电极连接到所述电源的阳极，将所述工件连接到所述电源的阴极。也可以理解为，将所述电极连接到所述电源的阴极，将所述工件连接到所述电源的阳极。这种方法突破了现有工艺中，一般只能将工件连接在电源阴极的限制，对工件的外型没有特别的限定，同时，通过调换电极和工件的极性，通过调换电极和工件的极性，也可以提高球形粉末制备过程中的效率以及细粉收得率。
当所述电极连接到电源的阳极时，电源驱动电极旋转，此时，电极设置有中空腔。可以理解地，设置有中空腔的电极为设置有单管、多管和中空嵌套的电极。
在一些优选的实施例中，电极为设置有单管的电极，其局部结构如图1左侧所示，所述单管电极设置有电极组件110以及位于所述电极组件之间的通道管120。通道管设置有一个进口，以及一个出口，流体介质可以从通道管中的进口进入，从通道管中的出口流出。通道管的出口朝向工件，这样可以使流体介质流向工件。此外，流体介质也可以从通道管外130进入，顺着电极组件外表面，流向工件。
可以理解地，流体介质可以分别单独地从电极的中空腔内或中空腔外引入，也可以同时从电极的中空腔内和中空腔外引入。从中空腔内和中空腔外流入的流体介质可以是相同的流体介质也可以是不同流体介质。中空腔内和中空腔外引入的流体介质分别独立地选自水基介质和/或惰性气体，所述惰性气体包括氮气。
水基介质优选为蒸馏水。
当所述工件连接到电源的阳极时，电源驱动工件旋转。此时，工件设置有中空腔。流体介质可以分别单独地从工件的中空腔内或中空腔外引入，也可以同时从工件的中空腔内和中空腔外引入。流体介质从工件的中空腔外引入可以理解为：流体介质顺着工件外表面流向电极。从中空腔内和中空腔外流入的流体介质可以是相同的流体介质也可以是不同流体介质。中空腔内和中空腔外引入的流体介质分别独立地选自水基介质和/或惰性气体，所述惰性气体包括氮气。
水基介质优选为蒸馏水。
所述电源为直流脉冲电源、直流恒流电源，交流脉冲电源或交流恒流电源。
优选地，所述电源为脉冲电源，脉冲宽度为2μs-200000μs，脉冲间隔为2μs-200000μs。
通过所述运动控制系统调整所述电极和工件的相对位置，得到理想放电状态的电弧等离子体。
可以理解地，调整所述电极和工件的放电间隙产生电弧等离子体，优选地，所述放电间隙，即所述电极的放电端与所述工件的表面的距离，为0.1mm-100mm。该距离可使电弧等离子体能够作用于电极和工件，并能保证流体介质通过时，具有很大的压力。所述电弧等离子体的中心温度高达10000K，可熔化绝大多数的导电材料，工件表面在其作用下熔融，形成半径范围在0.5mm-2mm的微小熔坑，即熔融区，此时，电极相对于工件作高速旋转的机械运动。
优选地，电源的供电参数还包括：间隙电压为10-160V，放电电流为5A-1000A。
优选地，所述电极为铜电极或石墨电极。
启动电源的同时，于所述电极和工件之间通入流体介质。图1展示了一个 优选的通入流体介质的实施方式，如1中箭头表示流体介质的流动方向。图1右侧放电间隙的放大图，210为电弧等离子体，220为熔坑。通过电极/工件的相对移位和流体介质的移弧耦合作用，将熔融区的材料连续的从熔坑中抛离，提高颗粒的排出率，提高加工效率。同时，控制电极的转速或工件的转速、控制流体介质的流速，能够改变电弧等离子体的工作状态，使熔融区产生微小爆炸，粉碎位于熔融区的材料，将材料进一步细化。
可以理解地，通过控制所述运动控制系统、电源参数、转速以及流速，可获得不同粒径分布的粉末。
当电极连接电源阳极时，优选地，所述电极的转速为100r/min-60000r/min，更优选为3000r/min-60000r/min。同理，当工件连接电源阳极时，优选地，所述工件的转速为100r/min-60000r/min，更优选为3000r/min-60000r/min。
优选地，流体介质初始通入时的流速为0.5L/min-500L/min。
将电极或金属工件的转速控制在上述范围内，将流体介质初始通入时的流速控制在上述范围内，有利于提高细粉收得率，收集到更多的粒径在10μm-250μm的金属粉末。
可以理解地，所述电极和工件均为导体材料或弱导电材料，所述电极的材料和工件的材料可以是相同的，也可以是不同的。
由于电弧等离子体的中心温度高达10000K，熔化绝大多数的导电材料，因此上述方法适用于多种导电粉末的制备。
而且，上述方法对工件的外形不做过多要求，工件可以是棒状、块状等规则或不规则的形态。
微爆粉碎后的材料在流体介质中急速冷却，粉碎的细小颗粒在冷凝过程中因表面张力的收缩作用固化成微细球形的粉末，收集冷凝后的微细球形粉末。
具体的，在流体介质中收集上述微细球形粉末的所采用的装置为多级收粉装置，所述多级收粉装置设置有呈喇叭状的缓冲部以及与所述喇叭状的缓冲不平滑连接的阶梯状收集平台，每一级阶梯，均对应为一个收集平台。冷凝后的微细球形粉末随着流体介质流出多级收粉装置中，然后，随着流体介质流经每一级阶梯，微细球形粉末可以沉积在阶梯上，避免出现流体介质直接冲刷到收粉箱中造成微细球形粉末随着流体介质流失或飞溅现象，保证粉末收集的完整性，实现提高细粉收得率的目的。
还可对冷凝后的所述微细球形粉末进行清洗、烘干和筛分。其中，清洗剂可选自碳酸清洗剂、醇类清洗剂或醚类清洗剂，清洗掉粉末中的油污。所述碳酸清洗剂或、醇类清洗剂或醚类清洗剂熔点低，易挥发，便于后续干燥。
将清洗后的粉末置于真空干燥箱或电阻箱内烘干，烘干后，将粉末在分级筛中过筛，收集粒径在10μm-250μm的颗粒。优选地，收集粒径在10μm-103μm的颗粒。
粉碎后的细小颗粒在流体介质中迅速冷凝，得到的初级粉末具有好的球形度，赋予粉末更好的流动性。
通过上述方法制得的新型球形粉末粒径较小、细粉收得率高、颗粒形状规则、球形度好、空心粉和卫星粉含量低、流动性好。
以下结合具体实施例进行说明。
实施例1
本实施例提供一种新型球形粉末的制备方法，包括以下步骤：
以块状304不锈钢作为工件，尺寸为100mm*100mm*20mm，将其清洗去污后，连接电源的阴极。将设置有单管的石墨电极连接电源的正极。所述电极的放电端与所述工件之间的距离为0.5mm。所述多管即指位于电极组件之间的 若干个通道管，所述通道管的出口朝向该块状304不锈钢。
设置供电参数为：间隙电压为45V-55V，放电电流为500A，脉冲宽度2000μs，脉冲间隔200μs，启动电源，控制所述电极的转速为5000r/min。同时，于若干个所述通道管中通入蒸馏水，通入时，其流速为50L/min。在上述工艺条件下，电弧等离子体作用于石墨电极和工件表面，熔融的材料随着蒸馏水连续排出，爆炸粉碎，最后在蒸馏水中冷凝成微细球形粉末，即为新型球形粉末。
加工0.1h后，称量知金属工件减重290g，即上述方法的加工效率达到2900g/h。获得的新型球形粉末如图2所示。
实施例2
本实施例提供一种新型球形粉末的制备方法，包括以下步骤：
以棒状TC4(钛合金)作为工件进行加工，外径为
Figure PCTCN2019126466-appb-000001
内径为
Figure PCTCN2019126466-appb-000002
长度为100mm，将其清洗去污后，连接电源的阳极。将TC4电极连接电源的阴极，所述电极的放电端与所述工件之间的距离为1mm，所述棒状TC4设置有一个通道管，所述通道管的出口朝向TC4电极。
设置供电参数为：间隙电压为45V-55V，放电电流为500A，脉冲宽度2000μs，脉冲间隔200μs，启动电源，控制所述管旋转电极的转速为3000r/min。同时，于所述通道管中和通道管为通入蒸馏水，通入时，其流速为50L/min。在上述工艺条件下，电弧等离子体作用于电极和工件表面，熔融的材料随着蒸馏水连续排出，爆炸粉碎，最后在蒸馏水中冷凝成微细球形粉末，即为新型球形粉末。
加工0.5h后，称量知金属工件减重850g，即上述方法的加工效率达到1700g/h。获得的新型球形粉末如图3所示。
由图2和图3可知，采用实施例1和实施例2的制备方法，得到的球形粉末粒径较小、颗粒形状规则、球形度好、空心粉和卫星粉含量低。
实施例3
本实施例提供一种新型球形粉末的制备方法，包括以下步骤：
以块状镍合金作为金属工件，尺寸为100mm*100mm*20mm，将其清洗去污后，连接电源的阴极。将管石墨电极连接电管的正极。所述电极的放电端与所述工件之间的距离为0.5mm。所述多管即指位于电极组件之间的若干个通道管，所述通道管的出口朝向该块状镍合金。
设置供电参数为：间隙电压为45V-55V，放电电流为500A，脉冲宽度2000μs，脉冲间隔200μs，启动电源，控制所述电极的转速为3000r/min。同时，于若干个所述通道管中通入蒸馏水，通入时，其流速为20L/min。在上述工艺条件下，电弧等离子体作用于石墨电极和镍合金工件表面，熔融的材料随着蒸馏水连续排出，爆炸粉碎，最后在蒸馏水中冷凝成微细球形粉末，跟随蒸馏水进入呈阶梯状的多级收粉装置。
采用碳酸清洗剂对上述微细球形粉末进行清洗，清洗后烘干，烘干后过筛，收集粒径在10μm-250μm的颗粒，即为新型球形粉末，如图4所示。
加工1h后，称量所得粒径在10μm-250μm的球形粉末，计算收集得到的粉末重量占工件减重的总质量的比例，即细粉收得率达到88.3％。
实施例4
本实施例提供一种新型球形粉末的制备方法，包括以下步骤：
以棒状铜合金作为金属工件，外径为
Figure PCTCN2019126466-appb-000003
内径为
Figure PCTCN2019126466-appb-000004
长度为100mm，将其清洗去污后，连接电源的阳极。将铜电极连接电源的阴极，所述电极的放电端与所述工件之间的距离为1mm，所述棒状铜合金设置有一个通道管，所述通道管的出口朝向铜电极。
设置供电参数为：间隙电压为45V-55V，放电电流为500A，脉冲宽度2000μs， 脉冲间隔200μs，启动电源，控制所述电极的转速为3000r/min。同时，于所述通道管中和通道管外通入蒸馏水，通入时，其流速为20L/min。在上述工艺条件下，电弧等离子体作用于铜电极和铜合金工件表面，熔融的材料随着蒸馏水连续排出，爆炸粉碎，最后在蒸馏水中冷凝成微细球形粉末，跟随蒸馏水进入呈阶梯状的多级收粉装置。
采用碳酸清洗剂对上述微细球形粉末进行清洗，清洗后烘干，烘干后过筛，收集粒径在10μm-250μm的颗粒，即为新型球形粉末，如图5所示。
加工0.5h后，所得粒径在10μm-250μm的球形粉末，计算收集得到的粉末重量占工件减重的总质量的比例，即细粉收得率达到86.1％。
实施例5
本实施例提供一种新型球形粉末的制备方法，与实施例1的制备方法基本相同，区别在于，电极的转速和蒸馏水的流速不同。具体包括以下步骤：
以块状镍合金作为金属工件，尺寸为100mm*100mm*20mm，将其清洗去污后，连接电源的阴极。将管石墨连接电管的正极。所述电极的放电端与所述工件之间的距离为0.5mm。所述多管即指位于电极组件之间的若干个通道管，所述通道管的出口朝向该块状镍合金。
设置供电参数为：间隙电压为45V-55V，放电电流为500A，脉冲宽度2000μs，脉冲间隔200μs，启动电源，控制所述电极的转速为1000r/min。同时，于若干个所述通道管中通入蒸馏水，通入时，其流速为20L/min。在上述工艺条件下，电弧等离子体作用于石墨电极和镍合金工件表面，熔融的材料随着蒸馏水连续排出，爆炸粉碎，最后在蒸馏水中冷凝成微细球形粉末，跟随蒸馏水进入呈阶梯状的多级收粉装置。
采用碳酸清洗剂对上述微细球形粉末进行清洗，清洗后烘干，烘干后过筛， 收集粒径在10μm-250μm的颗粒，即为新型球形粉末，如图6所示。
加工1h后，称量所得粒径在10μm-250μm的球形粉末，计算收集得到的粉末重量占工件减重的总质量的比例，即细粉收得率达到79.6％。
测定实施例3-5的球形粉末的流动性，测定方法和结果如下：
根据GB/T 1482-2010/ISO 4490:2001金属粉末流动性的测定标准漏斗法(霍尔流速计)中规定，粉末流动性，即测量50g粉末流过标准尺寸漏斗孔所需的时间，测量三次取算数平均值。
测定步骤：用手指堵住漏斗出口，将试料放入漏斗。要确保将粉末充满漏斗底部，当打开漏斗的孔时，启动秒表，当漏斗中的粉末全部流尽，终止秒表。记录时间，精确到0.1s。
实施例3的粉末流动性21.57s；实施例4的粉末流动性22.88s；实施例5的粉末流动性25.34s。
由图2-图4和上述流动性的测试结果可知，实施例3-5制备的粉末细粉收得率高，颗粒的粒径分布均匀，流动性好，球形度好，空心粉和卫星粉含量低，与实施例3相比，实施例5中，改变电极的转速和流体介质的初始流速，对粉末的细粉收得率有影响，在实施例3的工艺参数下，细粉收得率较高。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和 改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (17)

  1. 一种新型球形粉末的制备方法，其特征在于，包括以下步骤：
    将电极和工件置于电源的两极，通过运动控制系统调整所述电极和工件的放电间隙产生电弧等离子体，所述电弧等离子体作用于所述电极和工件表面时，促使所述电极和工件表面熔融，形成熔融区，同时，在所述放电间隙引入流体介质，通过控制所述流体介质的流速，以及所述电极或工件的相对转速，引起电弧等离子体工作形态的改变，促使所述熔融区产生微小爆炸，粉碎并抛离位于所述熔融区的材料，粉碎后的所述熔融材料在所述流体介质中冷凝，收集冷凝后的微细球形粉末；
    所述电极设置有中空腔和/或所述工件设置有中空腔。
  2. 根据权利要求1所述的新型球形粉末的制备方法，其特征在于，通过所述运动控制系统调整所述电极和工件的相对位置，得到理想放电状态的电弧等离子体。
  3. 根据权利要求2所述的新型球形粉末的制备方法，其特征在于，所述电极的放电端与所述工件之间的距离为0.1mm-100mm。
  4. 根据权利要求1所述的新型球形粉末的制备方法，其特征在于，所述电极连接所述电源的阳极，所述工件连接所述电源的阴极，所述设置有中空腔的电极为设置有单管、多管或中空嵌套的电极。
  5. 根据权利要求4所述的新型球形粉末的制备方法，其特征在于，所述流体介质从所述电极的管内和/或管外引入。
  6. 根据权利要求1所述的新型球形粉末的制备方法，其特征在于，所述电极连接所述电源的阴极，所述工件连接所述电源的阳极，所述工件设置有中空腔。
  7. 根据权利要求6所述的新型球形粉末的制备方法，其特征在于，所述流体介质从所述工件的中空腔内和/或中空腔外引入。
  8. 根据权利要求1-7任一项所述的新型球形粉末的制备方法，其特征在于，所述流体介质为水基介质和/或惰性气体。
  9. 根据权利要求1-8任一项所述的新型球形粉末的制备方法，其特征在于，通过控制所述运动控制系统、电源参数、转速以及流速，获得不同粒径分布的粉末。
  10. 根据权利要求9所述的新型球形粉末的制备方法，其特征在于，所述电极的转速为3000r/min-60000r/min，或，所述工件的转速为3000r/min-60000r/min。
  11. 根据权利要求9所述的新型球形粉末的制备方法，其特征在于，所述流体介质初始通入时的流速为0.5L/min-500L/min。
  12. 根据权利要求1-11任一项所述的新型球形粉末的制备方法，其特征在于，所述电源为直流脉冲电源、直流恒流电源，交流脉冲电源或交流恒流电源。
  13. 根据权利要求1-11任一项所述的新型球形粉末的制备方法，其特征在于，所述电极和工件均为导体材料或弱导电材料，所述电极和工件的材料相同或不相同。
  14. 根据权利要求1-13任一项所述的新型球形粉末的制备方法，其特征在于，对冷凝后的所述微细球形粉末进行清洗、烘干和筛分，收集粒径在10μm-250μm的球形粉末。
  15. 根据权利要求14所述的新型球形粉末的制备方法，其特征在于，采用多级收粉装置，收集冷凝后的所述微细球形粉末，所述多级收粉装置设置有喇叭状的缓冲部以及与所述喇叭状的缓冲部平滑连接的阶梯状收集平台，每一级 阶梯，均对应为一个收集平台。
  16. 根据权利要求14所述的新型球形粉末的制备方法，其特征在于，对冷凝后的所述微细球形粉末进行清洗时，所采用的清洗剂为醇类清洗剂、醚类清洗剂或碳酸清洗剂。
  17. 一种由权利要求1-16任一项所述的制备方法制得的新型球形粉末。
PCT/CN2019/126466 2019-11-07 2019-12-19 新型球形粉末及其制备方法 WO2021088217A1 (zh)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US17/775,192 US20220395899A1 (en) 2019-11-07 2019-12-19 New spherical powder and preparation method therefor
EP19951796.2A EP4056301A4 (en) 2019-11-07 2019-12-19 NEW SPHERICAL POWDER AND ASSOCIATED PREPARATION METHOD
JP2022526418A JP7407927B2 (ja) 2019-11-07 2019-12-19 新しい球状粉末及びその製造方法
CA3163929A CA3163929C (en) 2019-11-07 2019-12-19 New spherical powder and preparation method therefor

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN201911082177.X 2019-11-07
CN201911082147.9A CN110961644B (zh) 2019-11-07 2019-11-07 球形粉末及其制备方法
CN201911082147.9 2019-11-07
CN201911082177.XA CN110961646B (zh) 2019-11-07 2019-11-07 金属粉末及其制备方法

Publications (1)

Publication Number Publication Date
WO2021088217A1 true WO2021088217A1 (zh) 2021-05-14

Family

ID=75849344

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/126466 WO2021088217A1 (zh) 2019-11-07 2019-12-19 新型球形粉末及其制备方法

Country Status (5)

Country Link
US (1) US20220395899A1 (zh)
EP (1) EP4056301A4 (zh)
JP (1) JP7407927B2 (zh)
CA (1) CA3163929C (zh)
WO (1) WO2021088217A1 (zh)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62227007A (ja) * 1986-03-28 1987-10-06 Daido Steel Co Ltd 粉末の製造方法
WO2000010756A1 (en) * 1998-08-18 2000-03-02 Noranda Inc. Method and transferred arc plasma system for production of fine and ultrafine powders
CN105345019A (zh) * 2015-11-26 2016-02-24 上海交通大学 3d打印用金属粉末高效电弧放电制备装置
CN107994213A (zh) * 2017-11-10 2018-05-04 北京圣比和科技有限公司 双自耗旋转电极电弧等离子体合成硅碳材料的方法及装置
CN109226778A (zh) * 2018-11-15 2019-01-18 深圳创源航天科技有限公司 一种金属粉末颗粒制备装置
CN109332715A (zh) * 2018-12-20 2019-02-15 成都露思特新材料科技有限公司 一种近β型钛合金制粉的方法
CN209139828U (zh) * 2018-11-15 2019-07-23 深圳创源航天科技有限公司 一种金属粉末颗粒制备装置

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS627805A (ja) * 1985-07-04 1987-01-14 Kusano Hiroshi 金属粉末の製造法
JPS6283407A (ja) * 1985-10-07 1987-04-16 Toyo Soda Mfg Co Ltd 微細な金属粉末の製造方法
US20050034668A1 (en) * 2001-03-22 2005-02-17 Garvey James F. Multi-component substances and apparatus for preparation thereof
FR3008014B1 (fr) * 2013-07-04 2023-06-09 Association Pour La Rech Et Le Developpement De Methodes Et Processus Industriels Armines Procede de fabrication additve de pieces par fusion ou frittage de particules de poudre(s) au moyen d un faisceau de haute energie avec des poudres adaptees au couple procede/materiau vise
CN107116219A (zh) * 2017-05-22 2017-09-01 西安欧中材料科技有限公司 一种采用SS‑PREP Ti6Al4V球形粉末的激光铺粉增材制造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62227007A (ja) * 1986-03-28 1987-10-06 Daido Steel Co Ltd 粉末の製造方法
WO2000010756A1 (en) * 1998-08-18 2000-03-02 Noranda Inc. Method and transferred arc plasma system for production of fine and ultrafine powders
CN105345019A (zh) * 2015-11-26 2016-02-24 上海交通大学 3d打印用金属粉末高效电弧放电制备装置
CN107994213A (zh) * 2017-11-10 2018-05-04 北京圣比和科技有限公司 双自耗旋转电极电弧等离子体合成硅碳材料的方法及装置
CN109226778A (zh) * 2018-11-15 2019-01-18 深圳创源航天科技有限公司 一种金属粉末颗粒制备装置
CN209139828U (zh) * 2018-11-15 2019-07-23 深圳创源航天科技有限公司 一种金属粉末颗粒制备装置
CN109332715A (zh) * 2018-12-20 2019-02-15 成都露思特新材料科技有限公司 一种近β型钛合金制粉的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP4056301A4 *

Also Published As

Publication number Publication date
JP2023500373A (ja) 2023-01-05
JP7407927B2 (ja) 2024-01-04
CA3163929A1 (en) 2021-05-14
EP4056301A4 (en) 2023-12-20
CA3163929C (en) 2024-04-09
US20220395899A1 (en) 2022-12-15
EP4056301A1 (en) 2022-09-14

Similar Documents

Publication Publication Date Title
CN110961646B (zh) 金属粉末及其制备方法
CN110961644B (zh) 球形粉末及其制备方法
CN105642879B (zh) 用于激光3d打印的球形tc4钛合金粉末及其制备方法
CN104923797B (zh) 用于激光选区熔化技术的Inconel625镍基合金粉末的制备方法
WO2021179431A1 (zh) 多元合金粉末及其快速制备方法
CN107096925B (zh) 一种新型的等离子体雾化制备球型粉末系统
CN106956008A (zh) 一种3D打印用Hastelloy X合金粉末的制备方法
CN106636748A (zh) 一种用于3d打印技术的tc4钛合金粉末及其制备方法
CN104028770B (zh) 一种医用钴铬钼合金球形颗粒的制备方法
CN101758238A (zh) 采用等离子辅助旋转电极制备钛合金tc4金属小球的方法
CN104148658A (zh) 一种制备增材制造专用Ti6Al4V合金粉末工艺方法
CN104060300B (zh) 钛铝钒合金粉末的制备方法
CN110125425B (zh) 一种电极感应气雾化连续液流制备球形金属粉末的方法
CN108637267A (zh) 一种利用金属丝材制备金属球形粉末的装置及方法
JPWO2003037553A1 (ja) 金属粉末の製造方法及びその装置
CN108526472A (zh) 一种自由电弧制备金属球形粉末的装置和方法
CN101927351A (zh) 采用等离子辅助旋转电极制备高温合金gh4169金属小球的方法
CN101733408A (zh) 采用等离子辅助旋转电极制备钛合金ta15金属小球的方法
CN108421984A (zh) 一种用于增材制造的不锈钢粉末及其制备方法
CN108620597A (zh) 一种高能等离子焰流制备球形粉末的装置和方法
WO2021088217A1 (zh) 新型球形粉末及其制备方法
CN208696304U (zh) 一种低压直流等离子枪制备3d打印用钛粉的装置
CN101767201A (zh) 采用等离子辅助旋转电极制备钛合金Ti60金属小球的方法
CN101767202A (zh) 采用等离子辅助旋转电极制备高温合金gh4648金属小球的方法
WO2021179432A1 (zh) 石墨烯包覆的超细粉体及其制备方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 19951796

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2022526418

Country of ref document: JP

Kind code of ref document: A

ENP Entry into the national phase

Ref document number: 3163929

Country of ref document: CA

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 2019951796

Country of ref document: EP

Effective date: 20220607

ENP Entry into the national phase

Ref document number: 2019951796

Country of ref document: EP

Effective date: 20220607

ENP Entry into the national phase

Ref document number: 2019951796

Country of ref document: EP

Effective date: 20220607