CN114472910A - Method for preparing superfine titanium powder by magnetized plasma rotary electrode method - Google Patents
Method for preparing superfine titanium powder by magnetized plasma rotary electrode method Download PDFInfo
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- CN114472910A CN114472910A CN202210197714.0A CN202210197714A CN114472910A CN 114472910 A CN114472910 A CN 114472910A CN 202210197714 A CN202210197714 A CN 202210197714A CN 114472910 A CN114472910 A CN 114472910A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000006698 induction Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 50
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 52
- 229910052719 titanium Inorganic materials 0.000 description 51
- 239000002184 metal Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- -1 argon ions Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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
- 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
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to the technical field of metal materials, and provides a method for preparing ultrafine titanium powder by a magnetized plasma rotating electrode method. The method prepares the superfine titanium powder by utilizing electrostatic coulomb repulsion force, not only avoids the technical difficulty of high-speed rotation when the PREP separates the titanium powder by centrifugal force, but also can meet the application occasions with stricter requirement on the titanium powder particle size because the prepared titanium powder has good spherical appearance and the average particle size is less than 10 mu m.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a method for preparing ultrafine titanium powder by a magnetized plasma rotating electrode method.
Background
The plasma rotating electrode method (PREP) is to make a consumable electrode from a high-purity titanium rod, heat and melt the end face of the consumable electrode by rare gas (argon) plasma to form a metal liquid film, and finally atomize and prepare titanium powder by the centrifugal force of electrode rotation.
At present, the plasma rotating electrode method has gradually replaced the rotating electrode method (REP) and the electron beam rotating disc method (EBRD) for preparing the fine spherical titanium powder. The main advantages of PREP compared to REP and EBRD are high sphericity of the prepared powder, good surface morphology, low impurity content, and the powder particle size distribution can be adjusted by the rotation speed and electrode diameter. However, since the electrode rotation speed is limited by the problem of dynamic sealing, the average particle size of the powder prepared by the plasma rotating electrode method is large. The particle size of the powder is generally distributed in the range of 50-300 μm, and the powder below 100 μm accounts for about 20%, and the average particle size of the powder is large, so that the application range is limited.
For example, 3D printing requires pure titanium powder that is ultra-fine (particle size less than 5 μm), high purity (oxygen content < 0.1%), spherical (sphericity better than 98%), which cannot be prepared using PREP.
Therefore, how to overcome the technical difficulty of high-speed rotation in the PREP, and to prepare and obtain the ultrafine titanium powder with good morphology becomes a problem to be solved at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing superfine titanium powder by a magnetized plasma rotating electrode method, which prepares the superfine titanium powder by utilizing electrostatic coulomb repulsion force, not only avoids the technical difficulty of high-speed rotation when the titanium powder is separated by a centrifugal force in PREP, but also ensures that the prepared titanium powder has good spherical shape and average particle size less than 10 mu m and can meet the application occasions with stricter requirements on the particle size of the titanium powder.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
the invention provides a method for preparing superfine titanium powder by a magnetized plasma rotating electrode method, which comprises the following steps: a magnetic field is increased between an arc and a rotating electrode in a plasma rotating electrode method.
Further, in a preferred embodiment of the present invention, the magnetic field is a magnetic mirror field.
Further, in the preferred embodiment of the present invention, the magnetic induction of the magnetic field is 300-500 Gs.
Further, in the preferred embodiment of the present invention, the electron density of the magnetically confined plasma is 1018m-3。
Further, in the preferred embodiment of the present invention, the electron temperature of the magnetically confined plasma is about 10 eV.
The method for preparing the superfine titanium powder by the magnetized plasma rotating electrode method has the beneficial effects that:
the magnetized plasma rotating electrode method provided by the invention utilizes electrostatic coulomb repulsion force to separate titanium particles so as to prepare ultrafine titanium powder, and the PREP is titanium powder with larger particle size obtained by separating titanium powder by centrifugal force.
Specifically, the method comprises the following steps: (1) according to the invention, on the basis of PREP, a magnetic field with the magnetic induction intensity of 300-500Gs is added in a transfer arc section (between an arc and a rotating electrode), so that most electrons of arc plasma are restrained from radially escaping and longitudinally escaping, and the density and the temperature of plasma electrons are improved. And further, in the high electron density plasma, the electron charge density on the surface of the large-diameter titanium particles thrown out by the rotating electrode due to the rotating centrifugal force is increased, and high electrostatic charge is formed, so that a strong electrostatic coulomb repulsive force is formed, and when the electrostatic coulomb repulsive force is larger than the viscous attractive force of a molten titanium metal interface, the titanium particles are driven to be separated to form titanium particles with smaller diameters. The satellite type titanium particles are separated under the action of electrostatic coulomb repulsive force, and then the satellite type particles are difficult to form. Thereby obtaining the ultrafine titanium powder (the grain diameter is less than 10 mu m).
(2) The plasma spheroidizing treatment is to heat and melt the powder fed into a high-temperature plasma torch, and then the molten liquid drops are re-solidified under the action of surface tension to form spherical powder. The plasma spheroidizing treatment can improve the surface appearance of the powder and also can reduce the pores and cracks of the original powder particles to a certain extent. In this embodiment, since the titanium particles are charged, the satellite-type titanium particles are separated into a plurality of separated powders by electrostatic coulomb repulsion, the separated powders are further heated by electrons in the plasma, and the surface tension of the titanium particles drives the separated powders to form a more standard spherical shape.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for preparing ultrafine titanium powder by a magnetized plasma rotating electrode method, which comprises the following steps: a magnetic mirror magnetic field with the magnetic induction intensity of 300-500Gs is added between an electric arc and a rotating electrode in the plasma rotating electrode method, and the electron temperature is about 10 eV.
Since the electron temperature of the plasma is about 10eV, the potential of the surface of the titanium particle is about-10V, and further accumulation of plasma electrons on the surface of the titanium particle is prevented. The debye length of the plasma is λ _ D, so the potential distribution of the charged titanium particles in the plasma is:
wherein r is more than or equal to Ro, r is the distance from a space point to the spherical center of the titanium particles, Ro is the radius of the titanium particles,
is the Debye shielding coulomb potential, lambda, of charged titanium particles in a plasmaDIs the debye radius of the plasma,
εo＝8.85×10-12(F/m) is the vacuum dielectric constant, QoIs the total charge carried by the titanium particles, k is the boltzmann constant,te is the temperature of the electrons, e is the charge of the electrons, neIs the electron density of the magnetized plasma. The temperature of electrons in the magnetized plasma is about 10eV, and the thermal velocity of electrons is:
the electron's cyclotron radius in a 300Gs magnetic field is approximately:
the magnetic moment of an electron when the electron moves along the direction of the magnetic field in the magnetic mirror magnetic field is a gradual invariant, namely, the magnetic moment of the electron:
the electrons do not only circle around magnetic lines in the magnetic field of the magnetic mirror, but also do reciprocating motion between the end points of the magnetic mirror, if the velocity distribution of the electrons is in the capture area of the magnetic mirror, the magnetic field of the magnetic mirror type restrains the longitudinal and radial escape of plasma electrons, so that the electrons generated by the transferred arc are restrained in the magnetic mirror. The magnetic field of 300Gs restrains the radial escape of electrons and also plays a role in improving the electron density of the plasma. The primary arc nozzle is at zero potential, the cathode of the arc is at negative potential, and the consumable rotating electrode is at positive potential, forming a transferred arc between the primary arc and the rotating electrode. Assuming that the distance between the primary arc nozzle and the rotating electrode is L, the applied voltage is V, and the electron density of the transferred arc plasma is about 1019m-3Electron temperature of about 10eV, and density of neutral gas of about 10eV24m-3The temperature of the neutral gas is about 3000K. The elastic collision cross-sectional area of argon atoms is about 2 x 10-19m2Mean free path of electron collision with argon atom:
the collision frequency of electrons with neutral gas atoms is about:
electrons in the magnetic mirror type cause partial radial escape due to collisions and longitudinal escape from the loss cone of the magnetic mirror. The heat flux density delivered by the transferred arc electrons to the consumable anode is about:
Γeth＝0.5nevethkTe＝0.5×1018×2.1×106×16×10-19
＝1.68(MWm-2)
and the heat flux density delivered by the neutral atoms of the transferred arc to the consumable anode is about:
the transferred arc electron and neutral directed flow gas provide about 3.3MWm for the rotating electrode-2The diameter of the end face of the consumable electrode is about 0.1m, and the cross-sectional area is about 7.85 x 10-3m2The net power of the transferred arc is about 26 kW. Because the heat conductivity of the titanium metal is about 20W/m × K, the heat flux density transmitted along the titanium rod is less than that transmitted by the transfer arc, the end surface of the titanium rod is heated and melted, the centrifugal force is larger than the viscous attraction of the interface of the titanium metal molten drops under the action of the rotary centrifugal force, and the produced titanium molten drops are thrown out.
In the PREP method, if the diameter of the titanium rod is about 100mm and the rotation speed is about 8000rpm, molten titanium particles having a diameter of 200um can be generated due to the rotational centrifugal force.
A titanium particle 200um in diameter having a mass of about:
the centrifugal force of the titanium particles at the edge of the rotating electrode is about:
the liquid titanium metal at the edge of the rotating electrode is subjected to a centrifugal force FrSurface tension F of molten titanium metalγAnd interfacial viscous attraction F with molten titaniumη. When the sum of the centrifugal force and the surface tension at the edge of the rotating electrode is greater than the viscous attraction of the molten titanium metal, the molten titanium metal is caused to separate from the edge of the rotating electrode, forming titanium particles.
Fr+Fγ＝Fη
The centrifugal force of the titanium particles is about 6.7X 10 if the surface tension of the molten titanium metal is neglected-4(N) equal to the viscous attraction F of the molten titanium metalηThe titanium particles are Direct Droplet Formed (DDF). The surface area of the interface viscous attraction of the titanium liquid drop is about Sσ＝πRo 2＝3.14×10-8(m2) The coefficient of viscous attraction of the titanium metal liquid is as follows:
electrons are constrained by the magnetic field of the magnetic mirror in the magnetized plasma, so that the electron density is increased to 1018m-3The temperature of the electrons is increased to 10eV under the acceleration of the transferred arc electric field, and the current density of the electrons injected into the titanium particles by the plasma electrons is as follows:
Je＝-0.5eneveth＝-0.8×10-19×1018×2.1×106＝170(kAm-2)
the thermal rate of the argon ions is:
the ion current density of the argon ion implantation is:
Ji＝0.5enivArth＝0.8×10-19×1018×1300＝104(Am-2)＜＜Je
assuming that the secondary electron emission current density of titanium particles in plasma is about 10Am-2＜＜JeThus, in a magnetized plasma, the titanium particles are charged primarily by the plasma electron current, while the ion current and the secondary electron current are negligible. When the charge potential of the titanium particles is about-10V relative to the zero potential of the plasma, the negative potential of the titanium particles prevents plasma thermal electrons of 10eV from continuing to charge the titanium particles, and the negative potential of the titanium particles cannot continue to rise, so that the titanium particles are maintained at a negative potential of-10V. A metallic titanium particle having a diameter of about 200 μm, the surface of which is charged to-10V and which has a total charge of about QoThe potential of the spherical surface of the conductor can be simplified into a spherical center QoTotal charge at radius RoCoulomb potential at the sphere:
total charge of metallic titanium particles:
Qo＝-40πεoRo＝-40×3.14×8.85×10-12×10-4＝-1.1×10-13(C)
the titanium metal ball with the diameter of 200 mu m is charged in magnetized plasma and has the surface charge density of
If a small hemisphere with a diameter of 10 μm protrudes above a spherical titanium particle with a diameter of 200 μm, the potential at the surface of the small hemisphere remains-10V (the conductivity of titanium metal is about 2.6 x 10)6S/m), the titanium particles are equi-potential bodies. But the charge density of the small hemisphere surface is largeAt the charge density of the large sphere, because the conductor tip is charged. The charge density of the small hemisphere is:
wherein R isoIs the radius of the large sphere, RsIs the radius of the pellet. The surface area of the small convex hemisphere is about
The charge carried is about:
Qs＝σqsAs＝2πRsRoσqo＜＜Qo
assuming that the surface area of the small hemispheres of the protrusions is much smaller than the surface area (R) of the large diameter titanium dropletss＜＜Ro) The total charge on the surface of the sphere becomes (Q)o-Qs) The distance between the big ball and the small convex hemisphere is about RoThe electrostatic coulomb repulsion between two charged spheres is about:
the viscous attraction between the small hemisphere and the large sphere interface is about:
if the viscous attraction is less than the electrostatic coulomb repulsion force experienced by the small hemisphere, the small hemisphere separates from the large sphere to form small titanium particles:
the small radius protrusions on the surface of the large titanium particles, which are caused by the accidental fluctuation, are broken into smaller particles by overcoming the viscous attraction of the interface between the molten titanium metals under the electrostatic coulomb repulsion.
In conclusion, the method for preparing the superfine titanium powder by adopting the magnetized plasma rotating electrode method provided by the invention prepares the superfine titanium powder by utilizing the electrostatic coulomb repulsion force, not only avoids the technical difficulty of high-speed rotation when the PREP separates the titanium powder by adopting a centrifugal force, but also can meet the application occasion with stricter requirement on the titanium powder particle size because the average particle size of the prepared titanium powder is less than 10 mu m.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for preparing superfine titanium powder by a magnetized plasma rotating electrode method is characterized by comprising the following steps: the method comprises the following steps: a magnetic field is increased between an arc and a rotating electrode in a plasma rotating electrode method.
2. The method for preparing the ultrafine titanium powder by the magnetized plasma rotating electrode method according to claim 1, which is characterized in that: the magnetic field is a magnetic mirror magnetic field.
3. The method for preparing the ultrafine titanium powder by the magnetized plasma rotating electrode method according to claim 2, wherein the method comprises the following steps: the magnetic induction intensity of the magnetic field is 300-500 Gs.
4. The method for preparing the ultrafine titanium powder by the magnetized plasma rotating electrode method according to claim 1, which is characterized in that: the electron density of the magnetically confined plasma was 1018m-3。
5. The method for preparing the ultrafine titanium powder by the magnetized plasma rotating electrode method according to claim 1, which is characterized in that: the electron temperature of the magnetically confined plasma was about 10 eV.
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