CN111618294A - Device for preparing spherical rhenium powder and preparation method of spherical rhenium powder - Google Patents
Device for preparing spherical rhenium powder and preparation method of spherical rhenium powder Download PDFInfo
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- CN111618294A CN111618294A CN202010580967.7A CN202010580967A CN111618294A CN 111618294 A CN111618294 A CN 111618294A CN 202010580967 A CN202010580967 A CN 202010580967A CN 111618294 A CN111618294 A CN 111618294A
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- 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
- B22F1/14—Treatment of metallic powder
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- 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
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- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
Abstract
The invention discloses a device and a method for preparing spherical rhenium powder, wherein the device comprises the following steps: the device comprises a feeder, a powder feeding gun, a radio frequency plasma generator, a spheroidizing chamber, a quenching chamber, a first collecting chamber, a solid-gas separator, a second collecting chamber, a vacuum unit and a tail gas discharge mechanism; the discharge hole of the feeder is connected with the powder feeding gun; the powder feeding gun is connected with the radio frequency plasma generator; the radio frequency plasma generator and the quenching chamber are respectively connected with the spheroidizing chamber, and the first collecting chamber is connected with the quenching chamber; the solid-gas separator is connected with the spheroidizing chamber through a pipeline; the second collection chamber is connected with the solid-gas separator; the tail gas discharge mechanism is connected with the solid-gas separator through a pipeline; the vacuum unit is arranged on a pipeline between the solid-gas separator and the tail gas discharge mechanism. The device can prepare the spherical rhenium powder with uniform components, less defects, good fluidity and good sphericity.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a device for preparing spherical rhenium powder and a preparation method of the spherical rhenium powder.
Background
Rhenium (element symbol is Re) is a silver-white heavy metal, the melting point of rhenium is as high as 3180 ℃, the elastic modulus of rhenium is the largest among refractory metals, rhenium does not form carbide even at very high temperature, and rhenium has very high tensile strength at room temperature and high temperature, has excellent plasticity, creep property and low cycle fatigue property, and is widely applied to the fields of national defense, aerospace, nuclear energy, electronic industry and the like.
The rhenium added alloy has obvious effect on improving the performance of the alloy, wherein, the rhenium added into the nickel-based single crystal superalloy can obviously improve the creep resistance, the fatigue resistance and the oxidation resistance.
The molybdenum-rhenium alloy can be used for manufacturing heaters, reflectors, space station components and the like with the temperature of more than 2000 ℃, and can also be used for manufacturing nozzles of rocket engines, radiating fins of converters in international thermonuclear experimental devices, conversion elements in thermonuclear control devices and other defense advanced products in high-tech fields. The molybdenum-rhenium alloy has good conductivity, wear resistance and arc ablation resistance, not only has the characteristics of high thermal stability, thermionic property, high electron escape and high resistance in various gases, but also still keeps good plasticity, higher recrystallization temperature, good thermoelectric property and mechanical impact resistance after heat treatment, thus having very wide application prospect in the field of electronics.
The W-Re alloy is mainly used for electric heating wires and thermometric instruments. The thermocouple made of W-Re alloy wire has wide temperature measuring range (0-2500 deg.c), good linear relation between temperature and thermoelectromotive force, high creep limit and lasting strength and lower cost than that of Pt and Rh thermocouple.
However, rhenium powder or rhenium alloy powder with uniform composition, few defects, good flowability, good sphericity is required in metal injection molding, additive manufacturing (3D printing), hot (cold) isostatic pressing, and plasma spraying processes. At present, the preparation of spherical rhenium powder mainly adopts a rotary electrode method, wherein a consumable electrode is made of metal or alloy, the end face of the consumable electrode is heated by electric arc and melted into liquid, the liquid is thrown out and crushed into fine liquid drops through the centrifugal force of high-speed rotation of the electrode, and then the fine liquid drops are condensed into powder. The rotating electrode method adopts a rhenium rod with the diameter of about 50mm to rotate at 15000-20000r/min, the particle size distribution range of the prepared rhenium powder is wider (50-500 mu m), and less fine spherical rhenium powder is obtained, especially less spherical rhenium powder with-325 meshes.
Another method for preparing spherical rhenium powder is direct current non-arc plasma spraying, which uses a direct current non-arc plasma spraying device consisting of three nozzles at an angle of 20-40 degrees to the vertical. Three nozzles are opposite to the same vertex to form a high-temperature plasma area, and then a rhenium wire with the diameter of 1-3mm is sent to a high-temperature area, the rhenium wire is melted and crushed in the area, and then is cooled and solidified to spherical rhenium powder.
The radio frequency plasma has the characteristics of high temperature, high enthalpy, high activity and large temperature gradient, and has great technical advantages in the aspects of preparation of nano powder materials, spheroidization of micron and submicron powder materials and the like by taking the radio frequency plasma as a heat source. The RF plasma technology and equipment has no impurity, continuous and stable operation, high material treating capacity and moderate cost, and thus has advantages over rotating electrode method and DC non-rotating arc plasma heat source. However, rhenium is easily oxidized into various rhenium oxides, so that the research on how to combine the radio frequency plasma technology with the preparation of high-quality spherical rhenium powder is of great significance.
Disclosure of Invention
The invention provides a device for preparing spherical rhenium powder and a preparation method of the spherical rhenium powder, which solve the problems, and the high-quality spherical rhenium powder can be prepared by adopting the device and the preparation method.
The invention is realized by adopting the following technical scheme:
an apparatus for preparing spherical rhenium powder comprises: the device comprises a feeder, a powder feeding gun, a radio frequency plasma generator, a spheroidizing chamber, a quenching chamber, a first collecting chamber, a solid-gas separator, a second collecting chamber, a vacuum unit and a tail gas discharge mechanism;
the discharge hole of the feeder is connected with the powder feeding gun so as to feed the metal rhenium raw powder carried by inert gas into the powder feeding gun; the powder feeding gun is connected with the radio frequency plasma generator, and metal rhenium raw powder sent out by the powder feeding gun is heated in the radio frequency plasma generator to form metal rhenium liquid drops; the radio frequency plasma generator and the quenching chamber are respectively connected with the spheroidizing chamber, and the metal rhenium liquid drops enter the quenching chamber through the spheroidizing chamber and form spherical rhenium powder; the first collection chamber is connected with the quenching chamber to receive spherical rhenium powder; the solid-gas separator is connected with the spheroidizing treatment chamber through a pipeline to receive part of spherical rhenium powder and separate the spherical rhenium powder; the second collection chamber is connected with the solid-gas separator to receive the spherical rhenium powder separated by the solid-gas separator; the tail gas discharge mechanism is connected with the solid-gas separator through a pipeline to discharge tail gas;
the vacuum unit is arranged on a pipeline between the solid-gas separator and the tail gas discharge mechanism, and is used for firstly pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10-4Pa, filling inert gas into the device for preparing the spherical rhenium powder, vacuumizing the device for preparing the spherical rhenium powder and maintaining the vacuum degree to be (1.0 × 10)4. + -. 200) Pa.
Preferably, the feeder is including sending powder dish and vibration mechanism, vibration mechanism connects send the powder dish in order to drive send the powder dish vibration, send the powder dish to have the cavity that is used for holding the former powder of metal rhenium and be provided with air inlet and discharge gate, be provided with on the inner wall of the cavity of sending powder dish and follow the helix that the internal perisporium spiral of cavity rises, the air inlet of sending powder dish is used for supplying inert gas to get into send in the powder dish, under vibration mechanism's vibration effect, the former powder of metal rhenium is followed send the helix of powder dish from bottom to top to carry the former powder of metal rhenium of carrying the transport from by inert gas the discharge gate of sending powder dish is seen off.
Preferably, the powder feeding gun comprises a gun body and a first cooling loop, wherein the gun body is used for feeding metal rhenium raw powder carried by inert gas into the radio frequency plasma generator, and the first cooling loop is arranged outside the gun body to cool the gun body.
Preferably, one end of the gun mouth of the powder feeding gun is vertically inserted into a high-frequency induction coil of the radio-frequency plasma generator from the top end of the shaft center of the radio-frequency plasma generator, so that the metal rhenium raw powder is sprayed out along the axis of the radio-frequency plasma generator.
Preferably, the distance between the gun mouth of the powder feeding gun and the lower end of the radio frequency plasma formed by the radio frequency plasma generator is 15-45 mm.
Preferably, the lower end nozzle of the radio frequency plasma generator facing the spheroidizing chamber is a divergent nozzle which is flared, and a second cooling loop is arranged on the periphery of the lower end nozzle of the radio frequency plasma generator to cool the lower end nozzle of the radio frequency plasma generator.
Preferably, the glove box is provided with a connecting pipe, the first collecting chamber is accommodated in the glove box, a feed port of the first collecting chamber is detachably connected with a feed port of the connecting pipe, a feed port of the quenching chamber is provided with a first valve, a feed port of the connecting pipe is provided with a second valve, the feed port of the quenching chamber and the feed port of the first collecting chamber are connected through the first valve, the second valve and the connecting pipe, and when the first valve opens the feed port of the quenching chamber, the second valve simultaneously opens the feed port of the connecting pipe to enable the feed port of the quenching chamber to be communicated with the feed port of the first collecting chamber; when the first valve is closed the discharge gate of quench chamber, the second valve is closed simultaneously the feed inlet of connecting pipe is so that the discharge gate of quench chamber with the feed inlet of first collection chamber does not communicate.
Preferably, a jacking mechanism is arranged on the glove box, the jacking mechanism is provided with a lifting jacking surface, and the jacking surface of the jacking mechanism is used for jacking the first collecting chamber so as to enable the discharge hole of the connecting pipe to be tightly jointed with the feed inlet of the first collecting chamber.
Preferably, solid-gas separator includes body, filter core and blowback gas pipe, be provided with on the body and be used for connecting line in order to communicate the mouth of pipe of balling processing chamber, the room is connected is collected to the second the body of solid-gas separator is in order to receive spherical rhenium powder, the filter core sets up adjacently orificial this is internal in order to send into the spherical rhenium powder of body filters, blowback gas pipe is used for blowing down and attaches spherical rhenium powder on the filter core.
Preferably, the mouth of blowing of blowback gas pipe communicates the inner chamber of filter core, be provided with a plurality of intercommunications on the filter core the inside and outside micropore of filter core, blowback gas pipe is used for blowing back gas into the inner chamber of filter core and pass through the micropore of filter core will spherical rhenium powder on the filter core blows off.
A preparation method of spherical rhenium powder comprises the following steps:
step S1, pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10-4Pa, charging inert gas into the device for preparing spherical rhenium powder, vacuumizing the device for preparing spherical rhenium powder and maintaining the vacuum degree at (1.0 × 10)4Within +/-200) Pa;
step S2: starting a radio frequency plasma generator, feeding metal rhenium raw powder into the radio frequency plasma generator through a feeder and a powder feeding gun, heating the metal rhenium raw powder in the radio frequency plasma generator to form metal rhenium liquid drops, and making the metal rhenium liquid drops enter a quenching chamber through a spheroidizing chamber to form spherical rhenium powder;
step S3: spherical rhenium powder that balling process room entering quench room formed is collected to first collection room, and inert gas carries partial spherical rhenium powder and passes through the pipeline and get into solid-gas separator, solid-gas separator separates the spherical rhenium powder in the inert gas and collects by the second collection room, and tail gas passes through tail gas discharge mechanism and outwards discharges.
Preferably, the step S1 includes firstly evacuating the vacuum degree of the apparatus for preparing spherical rhenium powder to less than or equal to 5Pa by using a rotary vane vacuum pump, and then evacuating the vacuum degree of the apparatus for preparing spherical rhenium powder to less than or equal to 5.0 × 10 by using a roots vacuum pump-1Pa, then using an oil diffusion vacuum pumpThe vacuum degree of the device for preparing the spherical rhenium powder is reduced to be less than or equal to 1.0 × 10-4Pa, then, the apparatus for preparing spherical rhenium powder was charged with inert gas, and then, the vacuum degree of the apparatus for preparing spherical rhenium powder was maintained at (1.0 × 10) using a water-ring vacuum pump4. + -. 200) Pa.
Compared with the prior art, the invention has the beneficial effects that at least:
the device for preparing the spherical rhenium powder with the specific structure, the specific process parameters and the high-purity argon are adopted for replacement, the metal rhenium raw powder is processed by the generated radio frequency plasma, the metal rhenium raw powder is ensured to have almost no chemical metallurgical reaction at high temperature, the prepared spherical rhenium powder is ensured to have high chemical purity, and the spherical rhenium powder with uniform components, few defects, good fluidity and good sphericity can be prepared.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for preparing spherical rhenium powder according to an embodiment of the present invention.
Fig. 2 is a scanning electron microscope picture of a rhenium metal raw powder.
Fig. 3 is a scanning electron microscope image of spherical rhenium powder prepared by the apparatus and method for preparing spherical rhenium powder according to the embodiment of the present invention.
FIG. 4 is a schematic view of a feeder according to an embodiment of the present invention.
FIG. 5 is a schematic cross-sectional view of a feeder according to an embodiment of the present invention.
FIG. 6 is a schematic view of a connection structure with a partial cross-section of a powder feeding gun, a radio frequency plasma generator and a spheroidization chamber according to an embodiment of the present invention.
Fig. 7 is a schematic view showing a connection structure of the quenching chamber, the first collecting chamber and the glove box according to the embodiment of the present invention, and a portion S is a partial structure omitted to show an internal structure.
FIG. 8 is a schematic structural diagram with a partial cross section of a solid-gas separator according to an embodiment of the invention.
Fig. 9 is a schematic structural diagram of a vacuum unit according to an embodiment of the present invention.
Fig. 10 is a schematic flow chart of a method for preparing spherical rhenium powder according to an embodiment of the present invention.
In the figure: 10. a feeder; 11. a powder feeding disc; 111. an air inlet; 112. a discharge port; 113. a feed inlet; 114. a barometer; 115. a transparent viewing plate; 116. a helical line; 12. a vibration mechanism; 20. a powder feeding gun; 30. a radio frequency plasma generator; 31. a high-frequency induction coil; 32. a radio frequency argon plasma; 33. a lower end spout; 40. a spheroidizing chamber; 50. a quenching chamber; 61. a first collection chamber; 62. a glove box; 621. a connecting pipe; 622. an interface; 623. an observation window; 624. an operating hand hole; 63. a first valve; 64. a second valve; 65. a jacking mechanism; 70. a solid-gas separator; 71. a body; 72. a filter element; 73. a blowback gas pipe; 74. a pipe orifice; 80. a second collection chamber; 90. a vacuum unit; 91. a rotary vane vacuum pump; 92. a Roots vacuum pump; 93. an oil diffusion vacuum pump; 94. a water-ring vacuum pump; 951. a first air extraction opening; 952. a second air extraction opening; 953. a third air extraction opening; 100. a tail gas discharge mechanism; 110. a pipeline.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The same reference numerals in the drawings denote the same or similar structures, and thus their repetitive description will be omitted.
The words expressing the position and direction described in the present invention are illustrated in the accompanying drawings, but may be changed as required and still be within the scope of the present invention.
Referring to fig. 1 to 9, an embodiment of the present invention provides an apparatus for preparing spherical powder, including: the device comprises a feeder 10, a powder feeding gun 20, a radio frequency plasma generator 30, a spheroidizing chamber 40, a quenching chamber 50, a first collecting chamber 61, a solid-gas separator 70, a second collecting chamber 80, a vacuum unit 90 and a tail gas discharge mechanism 100.
The apparatus for producing spherical powder according to the embodiment of the present invention will be described below by taking the case where the spherical powder is spherical rhenium powder and the metal raw powder is metal rhenium raw powder. The inert gas used in the apparatus for preparing spherical rhenium powder is preferably argon gas, the purity of the argon gas is preferably over 99.995%, and the purchased ordinary argon gas (with the chemical purity of 99.5%) can be subjected to secondary purification treatment by an argon gas purification treatment system to ensure that the chemical purity of the metallic rhenium raw powder is over 99.995% so as to ensure that the metallic rhenium raw powder has almost no chemical metallurgical reaction at high temperature, thereby ensuring that the prepared spherical rhenium powder has high chemical purity.
The feeder 10 is used to feed out metallic rhenium raw powder, which is a raw material for preparing spherical rhenium powder having an irregular shape and each particle having a sharp angle and an extremely rough surface, referring to fig. 2. The discharge port of the feeder 10 is connected with the powder feeding gun 20 to feed the rhenium metal raw powder carried by argon gas into the powder feeding gun 20, and the discharge port of the feeder 10 can be connected with the feed port of the powder feeding gun 20 through a pipeline or a pipeline.
Referring to fig. 4 and 5, in some embodiments of the present invention, feeder 10 includes powder feeding pan 11 and vibrating mechanism 12. The vibration mechanism 12 is connected to the powder feeding plate 11 to drive the powder feeding plate 11 to vibrate, and the vibration mechanism 12 can be a vibration feeding motor. The powder feeding plate 11 has a cavity for accommodating the metallic rhenium raw powder and is provided with an air inlet 111 and an outlet 112, and further provided with an inlet 113, a gas pressure gauge 114 and a transparent observation plate 115. The cavity of the powder feeding plate 11 is, for example, a substantially circular cavity, the inner wall of the cavity of the powder feeding plate 11 is provided with a spiral line 116 which spirally rises along the inner peripheral wall of the cavity, the spiral line 116 is, for example, unfolded in an archimedes involute, and the spiral angle of the spiral line 116 in the powder feeding plate 11 is preferably 8 degrees to 15 degrees, more preferably 10 degrees, so that the metal rhenium raw powder is more uniformly conveyed, and the preparation of the spherical rhenium powder with uniform components, few defects, good fluidity and good sphericity is more facilitated. The inlet 111 of the powder feeding plate 11 is used for introducing inert gas, preferably high purity argon gas having a purity of more than 99.995%, into the powder feeding plate 11 to prevent oxidation of the prepared spherical rhenium powder. The discharge port 112 of the powder feeding disk 11 is used for feeding out the rhenium metal raw powder, and the discharge port 112 is preferably adjacent to the top of the cavity. The feeding hole 113 of the powder feeding disc 11 is used for filling the metal rhenium raw powder, the gas pressure gauge 114 is used for acquiring the gas pressure in the cavity of the powder feeding disc 11, and the transparent observation plate 115 is arranged on the top surface of the powder feeding disc 11 and used for observing the feeding condition in the powder feeding disc 11.
Under the vibration action of the vibration mechanism 12, the rhenium raw metal powder is conveyed upwards along the spiral line 116 of the powder feeding disc 11 from bottom to top and is conveyed out from the discharge hole 112 of the powder feeding disc 11 by carrying argon. By adjusting the amplitude and the vibration frequency of the vibration mechanism 12 and the gas amount of the carrying argon, the rhenium metal raw powder is uniformly and uniformly conveyed upwards from the bottom of the powder feeding disc 11 until the rhenium metal raw powder is sent out from the discharge hole 112 of the powder feeding disc 11 by the carrying argon and then conveyed into the powder feeding gun 20.
Referring to fig. 6, the powder feeding gun 20 is connected to the rf plasma generator 30, and the rhenium metal raw powder fed from the powder feeding gun 20 is heated in the rf plasma generator 30 to form rhenium metal droplets. The working gas of the radio frequency plasma generator 30 is preferably argon gas with purity over 99.995%, the rated power of the radio frequency plasma generator 30 is preferably 100KW, and the oscillation frequency is preferably 3.5 MHz. The radio frequency plasma generator 30 generates high temperature radio frequency argon plasma 32, and by utilizing the high temperature characteristic, the metal rhenium raw powder is sprayed into the high temperature radio frequency argon plasma 32 from the gun mouth of the powder feeding gun 20 under the action of the material carrying argon, under the high temperature action of the radio frequency argon plasma 32, the irregular metal rhenium raw powder absorbs a large amount of heat in a very short time to be heated and melted rapidly, the molten metal rhenium forms droplets with very high sphericity under the action of surface tension, the metal rhenium droplets then leave the high temperature plasma region at a very fast rate, rapidly solidified under extremely high temperature gradient, and after entering the spheroidization chamber 40 and the quenching chamber 50, spherical rhenium powder with good sphericity is formed, since the above-mentioned substances participating in the reaction do not have the problem of contamination by electrode materials, the purity of the spherical rhenium powder prepared by the radio frequency plasma generator 30 is very high in combination with the apparatus for preparing spherical rhenium powder of this embodiment.
In some embodiments of the present invention, the powder feeding gun 20 includes a gun body for feeding the metallic rhenium raw powder carried by the inert gas into the radio frequency plasma generator 30, and a first cooling circuit (not shown) disposed outside the gun body to cool the gun body. The first cooling loop preferably adopts 06Cr19Ni10 alloy cold-drawn seamless tube, the stainless steel material has the advantages of high strength, good corrosion resistance, high heat resistance and the like, and adopts three layers of seamless tubes with different tube diameters to form the first cooling loop, the first cooling loop cools the gun body by injecting cooling liquid, the cooling liquid can be cooling water, the cooling liquid can flow in the three layers of seamless tubes with different tube diameters in sequence, the gun body is cooled by heat exchange, and the rhenium raw metal powder in the powder feeding gun 20 is prevented from being melted by high-temperature radio frequency plasma due to poor local cooling before being sprayed out. In a preferred embodiment, a booster pump (not shown) is used to achieve a cooling water pressure of not less than 0.6MPa into the powder feeding gun 20, and the booster pump is used to circulate the cooling liquid in the first cooling circuit to cool the gun body, forcibly cool the gun body and achieve an optimal cooling effect, thereby preventing any cooling "dead zone" in the powder feeding gun 20.
In some embodiments of the present invention, one end of the muzzle of the powder feeding gun 20 is vertically inserted into the high-frequency induction coil 31 of the rf plasma generator 30 from the top end of the axial center of the rf plasma generator 30, so that the rhenium metal raw powder is sprayed out along the axial line of the rf plasma generator 30, and the sprayed rhenium metal raw powder is heated more uniformly at high temperature.
In some embodiments of the present invention, the distance between the muzzle of the powder feeding gun 20 and the lower end of the rf plasma formed by the rf plasma generator 30 is 15-45mm, which is the installation height of the powder feeding gun 20, which not only ensures that the metallic rhenium raw powder can be rapidly melted into numerous metallic droplets, but also is not affected by the turbulence caused by the spiral airflow of the shielding gas, and the installation height takes into account the melting point height, the particle size and the particle size distribution range of the metallic rhenium raw powder, and the spheroidization effect and the productivity efficiency, so that the spherical rhenium powder with uniform components, fewer defects, good fluidity, and good sphericity can be prepared.
The rf plasma generator 30 and the quenching chamber 50 are connected to the spheroidizing chamber 40, respectively, and the metal rhenium droplets enter the quenching chamber 50 through the spheroidizing chamber 40 and form spherical rhenium powder. In some embodiments of the present invention, the lower nozzle 33 of the rf plasma generator 30 facing the spheroidization chamber 40 is a diverging nozzle that is flared, and the periphery of the lower nozzle 33 of the rf plasma generator 30 is provided with a second cooling circuit (not shown). The lower end nozzle 33 of the radio frequency plasma generator 30 is set to be an outward-expanding divergent nozzle, so that the metal droplets of fine molten rhenium powder can be prevented from being accumulated at the lower end nozzle 33. In the operation process of the device for preparing spherical rhenium powder, the device needs to be pumped to high vacuum, a sealing element (not shown) is usually arranged at the joint of the radio frequency plasma generator 30 and the spheroidization chamber 40, the sealing element is a sealing gasket or a sealing ring and is used for improving the sealing effect, and a second cooling loop is arranged at the periphery of the lower nozzle 33 of the radio frequency plasma generator 30 and cools the lower nozzle 33 of the radio frequency plasma generator 30, so that the sealing element at the joint of the radio frequency plasma generator 30 and the spheroidization chamber 40 can be prevented from deforming, the sealing element is ensured to have a better sealing effect, and metal liquid drops of fine molten rhenium powder can be prevented from being accumulated at the lower nozzle 33.
Referring to fig. 7, a first collecting chamber 61 is connected to the quenching chamber 50 to receive spherical rhenium powder, and the first collecting chamber 61 may be a receiving tank.
In some embodiments of the present invention, the apparatus for preparing spherical rhenium powder further includes a glove box 62, wherein a connection pipe 621 is provided on the glove box 62, and a feed inlet at an upper end and a discharge outlet at a lower end of the connection pipe 621 are respectively located outside the glove box 62 and inside the glove box 62. The glove box 62 is further provided with an interface 622 for vacuum and inflation, a viewing window 623 for observation, and a material receiving operation hand hole 624 for operation.
The first collecting chamber 61 is accommodated in the glove box 62, and the inlet port of the first collecting chamber 61 is detachably connected to the outlet port of the connection pipe 621 and is discharged from the connection pipe 621 when the first collecting chamber 61 collects the spherical rhenium powder. The discharge port of the quenching chamber 50 is provided with a first valve 63, the feed port of the connecting pipe 621 is provided with a second valve 64, the discharge port of the quenching chamber 50 and the feed port of the first collecting chamber 61 are connected through the first valve 63, the second valve 64 and the connecting pipe 621, when the first valve 63 opens the discharge port of the quenching chamber 50, the second valve 64 simultaneously opens the feed port of the connecting pipe 621 to communicate the discharge port of the quenching chamber 50 with the feed port of the first collecting chamber 61, and at this time, the spherical rhenium powder in the quenching chamber 50 is collected into the first collecting chamber 61 through the discharge port of the quenching chamber 50, the connecting pipe 621 and the feed port of the first collecting chamber 61; when the discharge port of the quenching chamber 50 is closed by the first valve 63, the second valve 64 simultaneously closes the feed port of the connecting pipe 621 so that the discharge port of the quenching chamber 50 is not communicated with the feed port of the first collecting chamber 61, at this time, the first collecting chamber 61 for collecting the spherical rhenium powder can be replaced, and meanwhile, due to the effects of the first valve 63 and the second valve 64, the device for preparing the spherical rhenium powder is isolated from the glove box 62, so that the whole device operation system can be kept in a constant vacuum state, the first collecting chamber 61 can be unloaded in the glove box 62, and the transfer operation of the spherical rhenium powder collected in the glove box 62 is completed under the condition that the whole device is not shut down. After the unloading is finished, the glove box 62 is vacuumized through the vacuumized interface 622 to keep the vacuum degree of the first collection chamber 61 consistent with that of the whole equipment, and when the first valve 63 and the second valve 64 are opened again, the vacuum degree of the whole equipment cannot be damaged by the first collection chamber 61, so that the stable and reliable operation of the whole equipment is guaranteed.
In one embodiment, the first valve 63 and the second valve 64 are linkage valves, in other words, the first valve 63 and the second valve 64 are linkage operation, and when the first valve 63 is operated to open the discharge port of the quenching chamber 50, the second valve 64 simultaneously opens the feed port of the connecting pipe 621; when the first valve 63 is operated to close the discharge port of the quenching chamber 50, the second valve 64 simultaneously closes the feed port of the connecting pipe 621, thereby rapidly achieving the opening and closing operation and shortening the material receiving time.
In one embodiment, the glove box 62 is provided with a tightening mechanism 65, the tightening mechanism 65 has a tightening surface capable of being lifted, and the tightening surface of the tightening mechanism 65 is used for tightening the first collecting chamber 61 so as to tightly engage the outlet of the connecting pipe 621 with the inlet of the first collecting chamber 61. The operating handle of the jacking mechanism 65 can be positioned outside the glove box 62, the jacking surface of the jacking mechanism 65 is positioned in the glove box 62, and the ejection port of the connecting pipe 621 is tightly jointed with the feeding port of the first collecting chamber 61 by arranging the jacking mechanism 65, so that the first collecting chamber 61 can be quickly replaced, and the pressure difference between the first collecting chamber 61 and the vacuum glove box 62 is not damaged.
Referring to fig. 8, a solid-gas separator 70 is connected to the spheroidizing chamber 40 through a pipe 110 to receive and separate part of the spherical rhenium powder from the argon gas, and a second collecting chamber 80 is connected to the solid-gas separator 70 to receive the spherical rhenium powder separated by the solid-gas separator 70. In the whole operation process of the equipment, a certain vacuum degree is kept in the device for preparing spherical rhenium powder, one part of the prepared spherical rhenium powder is collected and enters the first collection chamber 61, the other part of the prepared spherical rhenium powder flows to the solid-gas separator 70 through the pipeline 110, the superfine spherical rhenium powder with smaller size flows to the solid-gas separator 70, the average particle size is generally 0.5-5 mu m, the spherical rhenium powder carried by argon is separated by the solid-gas separator 70 and is collected by the second collection chamber 80, the second collection chamber 80 is a material collection tank for example, and the filtered argon is discharged as tail gas.
In some embodiments of the present invention, the solid-gas separator 70 includes a body 71, a filter element 72, and a blowback pipe 73. The body 71 is provided with a pipe orifice 74 for connecting a pipeline 621 to communicate with the spheroidization treatment chamber 40, the pipe orifice 74 can be obliquely arranged on the body 71, the second collection chamber 80 is connected with the body 71 of the solid-gas separator 70 to receive spherical rhenium powder, the second collection chamber 80 can be connected at the lower end of the body 71 of the solid-gas separator 70, the filter element 72 is arranged in the body 71 adjacent to the pipe orifice 74 to filter the spherical rhenium powder sent into the body 71, the filter element 72 is provided with a plurality of micropores capable of adsorbing the spherical rhenium powder, and the blowback pipe 73 is used for blowing the spherical rhenium powder attached to the filter element 72.
In one embodiment, the blowoff port of the blowback pipe 73 is communicated with the inner cavity of the filter element 72, the filter element 72 is provided with a plurality of micropores communicated with the inside and the outside of the filter element 72, the blowback pipe 73 is used for blowing blowback gas into the inner cavity of the filter element 72 and blowing off the spherical rhenium powder on the filter element 72 through the micropores of the filter element 72, the blowback gas is, for example, argon gas with purity exceeding 99.995%, and the blowback pipe 73 is arranged to blow off the spherical rhenium powder adsorbed on the filter element 72 more fully from the inside to the outside. In the embodiment of the invention, when the vacuum degree of the spheroidizing chamber 40 is reduced to 200Pa, the blowback gas pipe 73 is automatically opened, high-pressure blowback argon is blown to the filter element 72 from the blowback gas pipe 73, and the superfine spherical rhenium powder on the outer wall of the filter element 72 is blown off and collected.
At whole equipment preparation spherical rhenium powder in-process, keep certain vacuum in the device of preparation spherical rhenium powder, consequently, vacuum in the solid-gas separator 70 is less than external atmospheric pressure, but along with the going on of preparation spherical rhenium powder, must have some tiny spherical rhenium powder to adsorb on the outer wall of filter core 72, along with the accumulation of time, the micropore of filter core 72 is blockked gradually to interior by these tiny powders from outside, lead to the vacuum decline of balling processing room 40 easily, can cause extinguishing of radio frequency plasma even. The spherical rhenium powder on the filter element 72 is blown off through the blowback pipe 73, so that the vacuum degree of the spheroidizing chamber 40 can be kept constant, and the filter element 72 can keep better filtering performance.
In one embodiment, eight high temperature and corrosion resistant stainless steel filter elements 72 made of 06Cr19Ni10 are arranged in the solid-gas separator 70, and the stainless steel filter elements 72 have the advantages of good corrosion resistance, heat resistance, pressure resistance and wear resistance, good filtering performance, uniform surface filtering performance for powder with the particle size of 0.5-5 μm, repeated washing, long service life and the like.
The tail gas discharge mechanism 100 is connected with the solid-gas separator 70 through a pipeline 110 to discharge tail gas, and the vacuum unit 90 is arranged on the pipeline 110 between the solid-gas separator 70 and the tail gas discharge mechanism 100 to vacuumize the device for preparing spherical rhenium powder.
Referring to FIG. 9, in some embodiments of the present invention, the vacuum assembly 90 includes a rotary vane vacuum pump 91, a Roots vacuum pump 92, an oil diffusion vacuum pump 93, and a water ring vacuum pump 94. Wherein, before the device normal operating of preparation spherical rhenium powder, sliding vane vacuum pump 91 is used for drawing the vacuum degree of the device of preparation spherical rhenium powder to be less than or equal to 5Pa through first extraction opening 951, can dispose the compound vacuum gauge that is used for detecting resistance gauge and ionization gauge of vacuum degree and constitutes in the pipeline 110 of the device of preparation spherical rhenium powder, then, take out the vacuum degree of the device of preparation spherical rhenium powder to be less than or equal to through first extraction opening 951 with roots vacuum pump 925.0×10-1Pa, then pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10 through the second pumping hole 952 by using an oil diffusion vacuum pump 93-4Pa, then, argon gas, for example, argon gas having a purity of more than 99.995% is introduced into the apparatus for preparing spherical rhenium powder, and then, the degree of vacuum of the apparatus for preparing spherical rhenium powder is maintained by a water-ring vacuum pump 94 through a third pumping port 953 (1.0 × 10)4And +/-200) Pa, starting a power supply of the radio frequency plasma system to maintain the normal operation of the radio frequency plasma. By adopting the vacuum unit 90, the specific process parameters of the vacuum unit 90 and the high-purity argon gas for replacement, the metal rhenium raw powder is ensured to have almost no chemical metallurgical reaction at high temperature, so that the prepared spherical rhenium powder has high chemical purity.
Referring to fig. 10, an embodiment of the present invention further provides a method for preparing spherical rhenium powder, where the method preferably uses the apparatus for preparing spherical rhenium powder according to the foregoing embodiment of the present invention, and the method includes the following steps:
step S1, pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10-4Pa, then filling argon into the device for preparing the spherical rhenium powder, and then vacuumizing the device for preparing the spherical rhenium powder and maintaining the vacuum degree to be (1.0 × 10)4. + -. 200) Pa.
Specifically, step S1 includes evacuating the vacuum of the apparatus for preparing spherical rhenium powder to 5Pa or less by using the rotary vane vacuum pump 91, and evacuating the vacuum of the apparatus for preparing spherical rhenium powder to 5.0 × 10 or less by using the roots vacuum pump 92-1Pa, then pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10 by using an oil diffusion vacuum pump 93-4Pa, then, argon gas was introduced into the apparatus for preparing spherical rhenium powder, and then, the degree of vacuum of the apparatus for preparing spherical rhenium powder was maintained by a water ring vacuum pump 94 (1.0 × 10)4. + -. 200) Pa.
Step S2: starting a radio frequency plasma generator 30, feeding metal rhenium raw powder into the radio frequency plasma generator 30 through a feeder 10 and a powder feeding gun 20, heating the metal rhenium raw powder in the radio frequency plasma generator 30 to form metal rhenium liquid drops, and making the metal rhenium liquid drops enter a quenching chamber 50 through a spheroidizing chamber 40 to form spherical rhenium powder;
the ideal technological parameters for preparing spherical rhenium powder with better sphericity comprise 1.0A of anode current of radio frequency argon plasma, 7000V of anode voltage, 0.3MPa of protective gas argon gas pressure and 6.0L/min of flow, 0.3MPa of working gas argon gas pressure and 2.0L/min of flow, 0.05MPa of metal rhenium raw powder carrying gas argon gas pressure and 0.2L/min of flow, 50.0g/min of powder feeding speed of powder feeding gun 20 and 1.0 × 10 of vacuum degree of pipeline4Pa; distance between the muzzle of the powder feeding gun 20 and the lower end of the radio frequency plasma: 15 mm.
Step S3: the first collecting chamber 61 collects the spherical rhenium powder which enters the quenching chamber 50 through the spheroidization chamber 40, the argon-carried partial spherical rhenium powder enters the solid-gas separator 70 through the pipeline 110, the spherical rhenium powder in the argon is separated by the solid-gas separator 70 and collected by the second collecting chamber 80, and the tail gas is discharged outwards through the tail gas discharge mechanism 100.
In step S3, when the vacuum degree of the spheroidizing chamber 40 reaches 200Pa, the blowback pipe 73 is automatically opened, and high-pressure blowback argon is blown from the blowback pipe 73 to the filter element 72 to blow off and collect the ultrafine spherical rhenium powder on the outer wall of the filter element 72.
Referring to fig. 3, each particle of the spherical rhenium powder prepared by the apparatus for preparing spherical rhenium powder according to the embodiment of the present invention is changed into a spherical shape and the surface of each particle is extremely smooth. When measured by ASTMB212-99 standard, the apparent density of the spherical rhenium powder prepared by the spheroidizing treatment of the radio frequency plasma is 3.2g/cm3Increased to 4.3g/cm3. The increase of the apparent density and the change of the particle shape are beneficial to improving the flowability of the spherical rhenium powder, and the spherical rhenium powder with good flowability can ensure that the rhenium or rhenium alloy part has uniform components, less defects and excellent performance in the processes of metal injection molding, additive manufacturing (3D printing), hot (cold) isostatic pressing and plasma spraying.
Although embodiments of the present invention have been shown and described, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that those skilled in the art may make changes, modifications, substitutions and alterations to the above embodiments without departing from the spirit and scope of the present invention, all such changes being within the scope of the appended claims.
Claims (12)
1. The utility model provides a preparation spherical rhenium powder's device which characterized in that includes: the device comprises a feeder, a powder feeding gun, a radio frequency plasma generator, a spheroidizing chamber, a quenching chamber, a first collecting chamber, a solid-gas separator, a second collecting chamber, a vacuum unit and a tail gas discharge mechanism;
the discharge hole of the feeder is connected with the powder feeding gun so as to feed the metal rhenium raw powder carried by inert gas into the powder feeding gun; the powder feeding gun is connected with the radio frequency plasma generator, and metal rhenium raw powder sent out by the powder feeding gun is heated in the radio frequency plasma generator to form metal rhenium liquid drops; the radio frequency plasma generator and the quenching chamber are respectively connected with the spheroidizing chamber, and the metal rhenium liquid drops enter the quenching chamber through the spheroidizing chamber and form spherical rhenium powder; the first collection chamber is connected with the quenching chamber to receive spherical rhenium powder; the solid-gas separator is connected with the spheroidizing treatment chamber through a pipeline to receive part of spherical rhenium powder and separate the spherical rhenium powder; the second collection chamber is connected with the solid-gas separator to receive the spherical rhenium powder separated by the solid-gas separator; the tail gas discharge mechanism is connected with the solid-gas separator through a pipeline to discharge tail gas;
the vacuum unit is arranged on a pipeline between the solid-gas separator and the tail gas discharge mechanism, and is used for firstly pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10-4Pa, filling inert gas into the device for preparing the spherical rhenium powder, vacuumizing the device for preparing the spherical rhenium powder and maintaining the vacuum degree to be (1.0 × 10)4. + -. 200) Pa.
2. The device of spherical rhenium powder of preparation of claim 1, characterized in that, the feeder includes powder feeding dish and vibration mechanism, vibration mechanism connects powder feeding dish is in order to drive the vibration of powder feeding dish, powder feeding dish has the cavity that is used for holding the former powder of metal rhenium and is provided with air inlet and discharge gate, be provided with the edge on the inner wall of the cavity of powder feeding dish the helix of internal perisporium spiral shell screwing in rise of cavity, the air inlet of powder feeding dish is used for supplying inert gas to get into in the powder feeding dish, under vibration mechanism's the vibrating action, the former powder of metal rhenium is followed powder of the helix of powder feeding dish is carried the former powder of metal rhenium of carrying the transport from bottom to top and is followed by inert gas the discharge gate of powder feeding dish is seen.
3. The apparatus for preparing spherical rhenium powder according to claim 1, wherein the powder feeding gun comprises a gun body and a first cooling circuit, the gun body is used for feeding the metallic rhenium raw powder carried by inert gas into the radio frequency plasma generator, and the first cooling circuit is arranged outside the gun body to cool the gun body.
4. The apparatus for preparing spherical rhenium powder according to claim 1, wherein one end of a muzzle of the powder feeding gun is vertically inserted into a high-frequency induction coil of the radio-frequency plasma generator from the top end of the shaft center of the radio-frequency plasma generator, so that the metal rhenium raw powder is sprayed out along the shaft axis of the radio-frequency plasma generator.
5. The apparatus for preparing spherical rhenium powder according to claim 1, wherein the distance between the muzzle of the powder feeding gun and the lower end of the radio frequency plasma formed by the radio frequency plasma generator is 15-45 mm.
6. The apparatus for preparing spherical rhenium powder according to claim 1, wherein the lower end nozzle of the radio frequency plasma generator facing the spheroidization chamber is a divergent nozzle which is externally expanded, and a second cooling loop is arranged on the periphery of the lower end nozzle of the radio frequency plasma generator to cool the lower end nozzle of the radio frequency plasma generator.
7. The apparatus for preparing spherical rhenium powder according to claim 1, further comprising a glove box, wherein a connecting pipe is arranged on the glove box, the first collection chamber is accommodated in the glove box, the feed inlet of the first collection chamber is detachably connected with the feed outlet of the connecting pipe, the feed outlet of the quenching chamber is provided with a first valve, the feed inlet of the connecting pipe is provided with a second valve, the feed outlet of the quenching chamber and the feed inlet of the first collection chamber are connected through the first valve, the second valve and the connecting pipe, and when the feed outlet of the quenching chamber is opened by the first valve, the feed inlet of the connecting pipe is simultaneously opened by the second valve so as to communicate the feed outlet of the quenching chamber with the feed inlet of the first collection chamber; when the first valve is closed the discharge gate of quench chamber, the second valve is closed simultaneously the feed inlet of connecting pipe is so that the discharge gate of quench chamber with the feed inlet of first collection chamber does not communicate.
8. The apparatus for preparing spherical rhenium powder as claimed in claim 7, wherein the glove box is provided with a tightening mechanism, the tightening mechanism is provided with a liftable tightening surface, and the tightening surface of the tightening mechanism is used for tightening the first collection chamber so that the discharge port of the connecting pipe is tightly jointed with the feed port of the first collection chamber.
9. The device of claim 1, characterized in that the solid-gas separator comprises a body, a filter element and a blowback pipe, the body is provided with a pipe orifice for connecting a pipeline to communicate with the spheroidization chamber, the second collection chamber is connected with the body of the solid-gas separator to receive the spherical rhenium powder, the filter element is arranged in the body adjacent to the pipe orifice to filter the spherical rhenium powder fed into the body, and the blowback pipe is used for blowing the spherical rhenium powder attached to the filter element.
10. The device of preparation spherical rhenium powder of claim 9, characterized in that, the mouth of blowing of blowback gas pipe intercommunication the inner chamber of filter core, be provided with a plurality of intercommunications on the filter core the inside and outside micropore of filter core, blowback gas pipe is used for blowing back gas the inner chamber of filter core and pass through the micropore of filter core will spherical rhenium powder on the filter core blows off.
11. The preparation method of the spherical rhenium powder is characterized by comprising the following steps:
step S1, pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10-4Pa, charging inert gas into the device for preparing spherical rhenium powder, vacuumizing the device for preparing spherical rhenium powder and maintaining the vacuum degree at (1.0 × 10)4Within +/-200) Pa;
step S2: starting a radio frequency plasma generator, feeding metal rhenium raw powder into the radio frequency plasma generator through a feeder and a powder feeding gun, heating the metal rhenium raw powder in the radio frequency plasma generator to form metal rhenium liquid drops, and making the metal rhenium liquid drops enter a quenching chamber through a spheroidizing chamber to form spherical rhenium powder;
step S3: spherical rhenium powder that balling process room entering quench room formed is collected to first collection room, and inert gas carries partial spherical rhenium powder and passes through the pipeline and get into solid-gas separator, solid-gas separator separates the spherical rhenium powder in the inert gas and collects by the second collection room, and tail gas passes through tail gas discharge mechanism and outwards discharges.
12. The method for preparing spherical rhenium powder of claim 11, wherein the step S1 includes firstly evacuating the vacuum degree of the device for preparing spherical rhenium powder to be less than or equal to 5Pa by using a rotary vacuum pump, and then evacuating the vacuum degree of the device for preparing spherical rhenium powder to be less than or equal to 5.0 × 10 by using a Roots vacuum pump-1Pa, then pumping the vacuum degree of the device for preparing the spherical rhenium powder to be less than or equal to 1.0 × 10 by using an oil diffusion vacuum pump-4Pa, then, filling the device for preparing the spherical rhenium powderInert gas was introduced, and then, the vacuum degree of the apparatus for preparing spherical rhenium powder was maintained at (1.0 × 10) using a water-ring vacuum pump4. + -. 200) Pa.
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| CN113210820A (en) * | 2021-04-25 | 2021-08-06 | 成都交大焊接科技有限公司 | Flash welding method |
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