CN111331145A - Device and method for preparing metal powder by ultrasonic - Google Patents
Device and method for preparing metal powder by ultrasonic Download PDFInfo
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- CN111331145A CN111331145A CN202010347548.9A CN202010347548A CN111331145A CN 111331145 A CN111331145 A CN 111331145A CN 202010347548 A CN202010347548 A CN 202010347548A CN 111331145 A CN111331145 A CN 111331145A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
-
- 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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
- B22F2009/0808—Mechanical dispersion of melt, e.g. by sieves
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a device and a method for preparing metal powder by ultrasound, wherein the device comprises: the device comprises a blanking device, an ultrasonic atomization device and a powder collection device which are sequentially arranged from top to bottom, wherein the blanking device drops molten metal on an atomization vibrator of the ultrasonic atomization device; the ultrasonic atomizing apparatus includes: the energy converter drives the atomization vibrator to vibrate; the powder collecting device is used for collecting particles formed by scattering metal drops by the atomizing vibrators, and the particles are cooled into solid in the powder collecting device. By applying the embodiment of the invention, the lower atomization efficiency is higher.
Description
Technical Field
The invention relates to the technical field of metal material preparation, in particular to a device and a method for preparing metal powder by ultrasonic.
Background
Metal powder here means spherical metal particles. The metal powder has wide application in the fields of powder metallurgy, 3D printing, spraying, corrosion prevention and the like.
At present, the invention patent with application number 201611068664.7 in the prior art discloses an ultrasonic tin powder atomizing device, which comprises a tool head, wherein an amplitude transformer is arranged on one side of the tool head, a cooling device is arranged on one side of the amplitude transformer, a transducer front cover is arranged at one end of the amplitude transformer in the cooling device, a transducer rear cover is arranged on one side of the transducer front cover, a piezoelectric ceramic stack is arranged between the transducer front cover and the transducer rear cover, an electrode lead electrically connected to the piezoelectric ceramic stack is arranged on one side of the cooling device, and a signal generator is arranged at one end of the electrode lead. The ultrasonic atomized tin powder developed by the invention can fundamentally solve the defects, the ultrasonic waves are atomized according to the liquid surface tension wave forming, namely, liquid films are formed on the surfaces of the atomizing heads of the liquid metal under the vibration of the ultrasonic waves, the liquid films are broken by the vibration action and are separated from the liquid films to form uniform spheres, and the sphericity of the generated powder is higher.
However, as can be seen from paragraph 24 of the specification of "an ultrasonic tin powder atomizing device" and its specification fig. 2, the inventor found that the ultrasonic atomization method uses two oppositely disposed tool heads to emit ultrasonic waves relatively and atomizes the passing tin liquid, and this method uses ultrasonic waves to act on the liquid tin, and the tool heads do not contact with the liquid tin, so the driving effect of the ultrasonic waves is not good, and the production efficiency of the prior art is low.
Disclosure of Invention
The technical problem to be solved by the invention is how to improve the production efficiency of the atomization process.
The invention solves the technical problems through the following technical means:
the embodiment of the invention provides a device for preparing metal powder by ultrasonic, which comprises: a blanking device, an ultrasonic atomization device and a powder collection device which are arranged from top to bottom in sequence, wherein,
the blanking equipment drops the molten metal on an atomization vibrator of the ultrasonic atomization equipment;
the ultrasonic atomizing apparatus includes: the energy converter drives the atomization vibrator to vibrate;
the powder collecting device is used for collecting particles formed by scattering metal drops by the atomizing vibrators, and the particles are cooled into solid in the powder collecting device.
By applying the embodiment of the invention, the blanking device drops the molten metal liquid on the atomizing vibrator of the ultrasonic atomizing device, the atomizing vibrator directly vibrates the metal liquid to atomize the metal liquid, and compared with the prior art in which ultrasonic waves are used for acting on the metal liquid, the embodiment of the invention belongs to contact type atomization, and has stronger driving force, so that the atomization efficiency is higher.
Optionally, the unloading equipment includes: a metal bar clamping device and a metal bar melting device which are arranged from top to bottom in sequence, wherein,
the metal rod clamping device clamps the top end of the metal rod, and the bottom end of the metal rod is inserted into the metal rod melting device.
Optionally, the metal rod melting apparatus includes: one or a combination of an electromagnetic induction heating device and a resistance heating device.
Optionally, the metal bar clamping device is fixed on the lifting device, and the lifting device bears the metal bar clamping device to move up and down.
Optionally, the central line of the metal rod coincides with the central line of the metal rod melting device.
Optionally, the powder collecting device is a cavity structure, and a cooling liquid is contained in the cavity structure, wherein the cooling liquid includes; water;
the ultrasonic atomization equipment is positioned in the cavity inside the powder collection equipment and is positioned above the liquid level of the cooling liquid.
Optionally, the nebulizer comprises:
one or a combination of disk-shaped atomizing vibrators and spherical atomizing vibrators.
The embodiment of the invention provides a method for preparing metal powder by ultrasonic, which comprises the following steps:
clamping one end of a metal rod with the diameter of 1-150mm and the purity of more than 99% on blanking equipment;
controlling blanking equipment to drop metal liquid formed after the metal rod is melted onto ultrasonic atomization equipment;
an energy converter in the ultrasonic atomization equipment drives an atomization vibrator, and the atomization vibrator breaks up metal drops into particles;
the particles fall under gravity into a powder collection device.
Optionally, the control unloading equipment falls the metal liquid drop that forms after the metal rod melts on ultrasonic atomization equipment, includes:
controlling the metal bar clamping equipment to insert one end of the metal bar into the metal bar melting equipment at a rotating speed of 10-60rpm and a descending speed of 10-150 mm/min;
the metal rod melting equipment melts the metal rod into liquid to form metal drops, the metal drops drop on the atomization vibrator, and the ultrasonic power used by the atomization vibrator is 50-8000W; the ultrasonic frequency is 10kHz-150 kHz; the amplitude of the ultrasonic vibrator is 5-100 microns.
Optionally, the metal rod melting device is an induction heating device, wherein,
the electromagnetic coil of the induction heating equipment is a D-shaped copper coil, the outer diameter of the coil is 120-150mm, the height of the coil is 50-60mm, and the distance from the bottom of the coil to the top of the ultrasonic atomization vibrator is 25-50 mm; the number of turns is 5-8 turns; the working frequency of the electromagnetic coil is 10 kHz-100 kHz;
the copper coil is of a hollow structure, and circulating cooling water is contained in the copper coil; the water temperature is 3-20 ℃.
The invention has the advantages that:
by applying the embodiment of the invention, the blanking device drops the molten metal liquid on the atomizing vibrator of the ultrasonic atomizing device, the atomizing vibrator directly vibrates the metal liquid to atomize the metal liquid, and compared with the prior art in which ultrasonic waves are used for acting on the metal liquid, the embodiment of the invention belongs to contact type atomization, and has stronger driving force, so that the atomization efficiency is higher.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a metal rod clamping device in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
FIG. 3 is a schematic view of a first structure of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a second structure of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of a third structure of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
FIG. 6 is a schematic structural diagram of an intermediate frequency coil in the metal rod melting apparatus according to the embodiment of the present invention;
FIG. 7 is a schematic structural diagram of a cooling apparatus in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention;
FIG. 8 is a scanning electron micrograph of zinc powder prepared by a prior art method.
FIG. 9 is a first scanning electron micrograph of a zinc powder prepared in example 2 of the present invention;
FIG. 10 is a second SEM image of a zinc powder prepared in example 2 of the present invention;
FIG. 11 is a third SEM image of a zinc powder prepared in example 2 of the present invention;
FIG. 12 is a fourth SEM image of a zinc powder prepared in example 2 of the present invention;
FIG. 13 is a fifth scanning electron micrograph of a zinc powder prepared according to example 2 of the present invention;
FIG. 14 is a particle size distribution diagram of a zinc powder prepared in example 2 of the invention;
FIG. 15 is a first scanning electron micrograph of a zinc powder prepared in example 3 of the present invention;
FIG. 16 is a second SEM image of a zinc powder prepared in example 3 of the present invention;
FIG. 17 is a third scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention;
FIG. 18 is a fourth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention;
FIG. 19 is a fifth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention;
FIG. 20 is a sixth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention;
FIG. 21 is a seventh scanning electron micrograph of a zinc powder prepared in example 3 of the present invention;
FIG. 22 is an eighth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention;
FIG. 23 is a particle size distribution diagram of a zinc powder prepared in example 3 of the invention.
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 with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In order to solve the problems of the prior art, the embodiment of the invention provides a device for preparing metal powder by ultrasonic.
The embodiment of the invention is suitable for preparing metal powder of tin alloy, indium, aluminum alloy, iron-based alloy, nickel-based alloy, cobalt-based alloy, titanium alloy, shape memory alloy and metal-based composite material.
Fig. 1 is a schematic structural diagram of an apparatus for ultrasonically preparing zinc powder according to an embodiment of the present invention, as shown in fig. 1, the apparatus includes: the blanking device 100, the ultrasonic atomization device 200 and the powder collection device 300 are arranged in sequence from top to bottom, wherein,
1. unloading equipment 100 includes: a zinc rod clamping device 101 and a zinc rod melting device 103 which are arranged from top to bottom in sequence. Fig. 2 is a schematic structural diagram of a zinc rod clamping device 101 in an apparatus for ultrasonically preparing zinc powder according to an embodiment of the present invention, and as shown in fig. 2, the zinc rod clamping device 101 clamps a top end of a zinc rod 102, the zinc rod clamping device 101 is fixed on a lifting device, and the lifting device bears the zinc rod clamping device 101 to move up and down. The zinc bar holding apparatus 101 includes: a rotating device 105 located at the upper part, a lifting rod 106 located at the middle part, and a material fixing device 107; the rotating device can be an existing mechanical structure fixed on the lifting equipment and is driven by electricity. The lifting equipment drives the rotating device to move up and down, the rotating device can drive the lifting rod to rotate, the movement of the lifting rod is a composite movement formed by the up-and-down movement and the rotating movement, and then the zinc rod can be rotated to ascend or descend.
The zinc rod melting device 103 can be one of an electromagnetic induction heating device or a resistance heating device. When the electromagnetic induction heating apparatus is used, the zinc rod is moved downward by the zinc rod holding apparatus 101, and the lower end is inserted into the electromagnetic induction coil. The electromagnetic induction heating equipment rectifies the three-phase power frequency alternating current to form direct current, then converts the direct current into adjustable current, supplies alternating current flowing through a capacitor and an induction coil, generates high-density magnetic lines in the induction coil, cuts metal materials contained in the induction coil, generates large eddy current in the metal materials, and can generate heat on the surface of the zinc rod due to the resistance in the zinc rod, so that the zinc rod is melted; the zinc bar melting equipment 103 melts the zinc bar into liquid to form zinc drops, and the zinc drops fall on the atomization vibrator 203; the bar can be heated to red and melted only by adjusting the frequency and the current intensity, so that the bar is convenient to adjust and is beneficial to operation. The center line of the zinc rod is superposed with the center line of the coil, so that the surface temperature of the zinc rod is the same, and the control of the production process is facilitated; in addition, the zinc bar does not generate harmful gas, strong light pollution and the like in the heating and melting process.
Further, in order to form metal droplets better, fig. 6 is a schematic structural diagram of an intermediate frequency coil in the metal rod melting apparatus according to the embodiment of the present invention, as shown in fig. 6, a zinc rod may be heated by using an intermediate frequency coil having an overall shape of an inverted cone structure, a copper pipe 401 is wound into a spiral intermediate frequency coil, and diameters of three layers of coils uniformly distributed from top to bottom are sequentially reduced, the copper pipe 401 is a copper pipe having an outer diameter of 15mm and an inner diameter of 13mm, an outer diameter of a top coil of the intermediate frequency coil is 120mm, an outer diameter of a bottom coil of the intermediate frequency coil is 60mm, and a height of the intermediate frequency coil is 50 mm.
In practical application, an intermediate frequency coil wound into four layers of coils can be used, the diameters of the four layers of coils which are uniformly distributed from top to bottom are sequentially reduced, the copper pipe 401 is a copper pipe with the outer diameter of 15mm and the inner diameter of 13mm, the outer diameter of the top coil of the intermediate frequency coil is 150mm, the outer diameter of the bottom coil of the intermediate frequency coil is 80mm, and the height of the intermediate frequency coil is 60 mm.
In practical application, a larger electromagnetic induction coil can be used, and the power of the electromagnetic induction coil can be 10-500W to adapt to a larger diameter zinc rod.
When the zinc rod falls, the zinc rod is inserted into the intermediate frequency coil from top to bottom, the coil at the top is far away from the zinc rod, and the generated induced current is small, so that the zinc rod can be heated at a low temperature, the position heated by the coil at the top enters the heating range of the coil at the middle layer along with the falling of the zinc rod, the heating at a higher temperature is realized, and then the zinc rod is heated and melted by the coil at the bottom to form zinc drops.
In the embodiment of the invention, the lifting device is used for centering the zinc rod and the intermediate frequency coil.
2. As shown in fig. 1, the ultrasonic atomizing apparatus 200 includes: the device comprises a transducer 201 and an atomization vibrator 203, wherein the transducer 201 drives the atomization vibrator 203 to vibrate; the atomization vibrator 203 can be a disk-shaped atomization vibrator 203, the disk-shaped atomization vibrator 203 is horizontally arranged and is positioned at the uppermost part of the ultrasonic atomization device 200, and the disk-shaped atomization vibrator 203 is connected with the transducer 201 through an amplitude transformer 202 which is connected in series up and down; transducer 201 is located below horn 202; the transducer 201 drives the amplitude transformer 202, and the amplitude transformer 202 drives the disc-shaped atomization vibrator 203 to vibrate at high frequency, so that zinc drops dropping on the top surface of the disc-shaped vibrator are atomized into small particles.
The ultrasonic atomization device 200 has the advantages of high power, stable performance, high reliability and simple installation; the core of the ultrasonic atomizing apparatus 200 is an ultrasonic vibration unit and a mating ultrasonic vibration source. The ultrasonic vibration component mainly comprises a high-power ultrasonic transducer, a variable amplitude rod 202 and an atomization vibrator 203, wherein,
the transducer is used to generate ultrasonic vibrations. The vibration energy is transmitted into the metal melt, the transducer converts the input electric energy into mechanical energy, namely ultrasonic wave, the expression form of the ultrasonic wave is that the transducer makes back and forth telescopic motion in the longitudinal direction, the amplitude is generally a few micrometers, the amplitude power density is not enough, and the ultrasonic wave cannot be directly used, so the vibration energy is transmitted into the metal melt through the series amplitude rods in the embodiment of the invention. It is emphasized that the series connection described in the embodiments of the present invention may use an existing series connection method.
Thus, the horn 202 serves to amplify the amplitude of the vibration, isolate the metal melt and thermal energy transfer, and also serves to anchor the entire ultrasonic vibration system. One end of the atomization vibrator 203 is connected with the amplitude transformer 202, the amplitude transformer 202 transmits ultrasonic energy to the atomization vibrator 203, the metal solution flows on a set area of the atomization vibrator 203, the metal liquid is broken up under the excitation of the ultrasonic vibration, then splashed out, and is collected after cooling and precipitation, so that the purpose of metal powder preparation is achieved.
Table 1 is a structural schematic diagram of an ultrasonic atomizing apparatus corresponding to a disk-shaped atomizing vibrator, and as shown in table 1, the distribution sequence of each component from top to bottom when the apparatus is operated from left to right corresponds to:
TABLE 1
Table 2 is a structural schematic table of the ultrasonic atomizing apparatus corresponding to the spherical atomizing vibrator, and as shown in table 2, the distribution sequence of the components from top to bottom when the apparatus operates from left to right:
TABLE 2
Table 3 shows specifications of the ultrasonic atomizing apparatus 200, as shown in table 3,
TABLE 3
Model number | SHAPEMEMORY001 |
Frequency of operation | 10kHz-150KHz |
Maximum power | 50W-8000W |
Maximum throughput kg/h | ≥10 |
Structural form | Longitudinal conical/longitudinal oblique wedge type/rotary disc transverse vibration type |
Form of atomizing vibrator | Conical rod/oblique rod/disc type for wedge |
Average particle diameter | 15-100μm |
Corresponding to table 3, fig. 3 is a first structural schematic diagram of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention; FIG. 4 is a schematic diagram of a second structure of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention; FIG. 5 is a schematic diagram of a third structure of an ultrasonic nebulizer in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention; as shown in fig. 3, fig. 3 shows a horizontally arranged disk-shaped vibrator, and an arrow indicates a dropping direction of zinc drops; as shown in fig. 4, a conical vibrator is shown in fig. 4, and an arrow indicates a dropping direction of zinc drops; as shown in fig. 5, the wedge type vibrator shown in fig. 5 has a zinc droplet dropping direction perpendicular to the central axis of the horn 202 so that the zinc droplet drops on the inclined surface.
In practical applications, the spherical atomizer 203 can also be used as the atomizer 203. The spherical atomizer 203 is arranged on top of an amplitude transformer 202 and operates on the same principle as the disc-shaped atomizer 203.
3. The zinc droplets of small particles are dispersed in the cabin body, and are cooled to fall to form zinc powder, and the zinc powder falls behind in the cooling liquid contained in the powder collecting device 300 and is then cooled to be solid and deposited to form a zinc powder deposition layer.
Further, the center line of the zinc rod is inserted into the center position of the zinc rod melting device 103.
Further, the powder collecting device 300 is a cavity structure, and contains a cooling liquid therein, wherein the cooling liquid includes; water; the lower end of the atomizer oscillator 203 extends into the powder collection device 300 and is located above the liquid level of the coolant.
Furthermore, the device is also provided with an LCD display screen and a key control button.
It is emphasized that, in order to avoid the oxidation of the material, the blanking device 100, the ultrasonic atomization device 200 and the powder collection device 300 which are arranged in sequence from top to bottom are all arranged in a sealed cabin body, for example, the blanking device is positioned in an upper cabin body, and the bottom of the upper cabin body is opened for zinc droplets to pass through; the housing of the powder collection apparatus 300 forms a lower chamber that is open at the top and is welded and sealed to the bottom opening of the upper chamber. The ultrasonic atomization device 200 is held within a cavity inside the powder collection device 300 by a holder. The zinc droplets pass through the opening at the bottom of the upper cabin body and pass through the opening at the top of the powder collecting device 300, and then fall onto the atomizing vibrator in the ultrasonic atomizing device 200, so that atomization is realized. During production, the chamber is evacuated and then filled with an inert gas, such as nitrogen.
In a specific implementation of an embodiment of the invention, the device is further provided with a water cooling device:
the circulating water cooling device part supplies power to a compressor, a fan, a water pump and the like through a contactor. The automatic control part comprises a temperature controller, a pressure protector, a device, a relay, an overload protector and the like which are mutually combined to achieve the purpose of automatically starting and stopping according to the water temperature, a circulating water cooling device (inner ribbing of an outer fin) is protected to be expanded and connected on the tube plate, and a safety valve is arranged to ensure the safety of the equipment.
The refrigerating capacity is based on the temperature condition
The return water temperature of the chilled water is 12 ℃; the water outlet temperature of the chilled water is 7 ℃; the condensation temperature is 35 DEG C
Selecting a power supply: 380V 50HZ/415V 60HZ 3-phase main power supply (three-phase)
The working range is as follows: the ambient temperature is 35 ℃ to 45 ℃; the outlet temperature of the chilled water is 3-20 ℃; the temperature difference of the outlet of the chilled water is 2.5-7 ℃.
Fig. 7 is a schematic structural diagram of a cooling device in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention, and as shown in fig. 7, in the closed liquid circulation apparatus according to an embodiment of the present invention, power is generated by a water pump 601, water is pumped out from a lower water tank 602, and then the water is conveyed to a flow transmitter 603 through a pipeline, and then cooling water enters the apparatus through a first manual valve 605 after being regulated by a solenoid valve 604, and then circularly absorbs heat from the apparatus and then flows into an upper water tank 607 through a second manual valve 606; the upper water tank 607 is located above the lower water tank 602, the two water tanks are communicated through at least one communication pipeline 608, hot water flowing out of the equipment flows into the communication pipeline 608 from the upper water tank 607 to dissipate heat, so that cooling is realized, then the hot water flows into the lower water tank 602, is further cooled in the lower water tank, and the circulation is carried out. The heat conductivity of the existing water cooling device is 20 times of that of the traditional air cooling mode, and the water cooling device used in the embodiment of the invention can enable the cooling effect to reach 25-35 times of that of the traditional air cooling mode by matching two water tanks. The heat dissipation problem of equipment can be solved better.
In addition, the pipeline is also provided with a pressure gauge 610, a branch electromagnetic valve 611, an electric control valve 612 and a liquid level transmitter 613.
The embodiment of the invention has the advantages of simple structure, easy assembly, economy and applicability.
Example 2
The embodiment of the invention also provides a method for preparing zinc powder by ultrasonic waves, which comprises the following steps:
s101: the lifting device is controlled to ascend, and the top end of the zinc bar with the diameter of 20mm and the purity of more than 99 percent is clamped on the material fixing device in the zinc bar clamping device 101. And then the lifting equipment is controlled to descend to drive the rotating device to descend, and the rotating device is controlled to rotate, so that the zinc bar is rotated and descended. The zinc rod holding apparatus 101 was controlled to insert one end of the zinc rod into the zinc rod melting apparatus 103 at a rotation speed of 10rpm, a lowering speed of 15 mm/min.
S102: firstly, the transducer 201 is started, the transducer 201 drives the amplitude transformer 202 to drive the atomization vibrator 203 to vibrate, the temperature of the atomization vibrator 203 rises under the action of the transducer 201, and the temperature of the atomization vibrator 203 rises above the melting point of zinc. Controlling a zinc bar melting device 103 to melt the zinc bar, wherein an induction heating device is used in the step; the coil is two-layer, outer three circles, 2 circles in the inlayer, and the total number of turns is 5 circles, and copper pipe 401 is external diameter 15mm, and internal diameter 13 mm's copper tubing, and intermediate frequency coil's top coil external diameter is 120mm, and bottom coil external diameter is 60mm, and the intermediate frequency coil height is 50 mm. The power of the intermediate frequency coil is 45W, the frequency is 25kHz, and the distance from the bottom of the intermediate frequency coil to the top of the ultrasonic vibrator is 25 mm. The ultrasonic transmitting power is 150W, and the ultrasonic frequency is 35 kHz; amplitude of 40 microns; the distance from the bottom of the intermediate frequency coil to the top of the ultrasonic atomization vibrator is 25 mm; the copper coil is internally provided with circulating cooling water; the water temperature is 18 degrees. The molten zinc formed by melting the zinc rod is dropped on the disk-shaped atomization vibrator 203.
S103: the transducer 201 in the ultrasonic atomization device 200 drives the atomization vibrator 203, and the atomization vibrator 203 breaks up zinc drops into particles; the particles fall under gravity into the powder collection apparatus 300.
The disc-shaped atomization vibrator 203 is horizontally arranged and is positioned at the uppermost part of the ultrasonic atomization device 200, and the disc-shaped atomization vibrator 203 is connected with the transducer 201 through an amplitude transformer 202 which is connected in series up and down; transducer 201 is located below horn 202; the transducer 201 drives the amplitude transformer 202, and the amplitude transformer 202 drives the disc-shaped atomization vibrator 203 to vibrate at high frequency, so that zinc drops dropping on the top surface of the disc-shaped vibrator are atomized into small particles.
Fig. 8 is a schematic structural diagram of a cooling device in an apparatus for ultrasonically preparing metal powder according to an embodiment of the present invention, and as shown in fig. 8, the zinc powder prepared in the prior art has adhesion and nodules, which indicates that the quality of the zinc powder prepared in the prior art is not good.
FIG. 9 is a first scanning electron micrograph of a zinc powder prepared in example 2 of the present invention; FIG. 10 is a second SEM image of a zinc powder prepared in example 2 of the present invention; FIG. 11 is a third SEM image of a zinc powder prepared in example 2 of the present invention; FIG. 12 is a fourth SEM image of a zinc powder prepared in example 2 of the present invention; FIG. 13 is a fifth scanning electron micrograph of a zinc powder prepared according to example 2 of the present invention, and as shown in FIGS. 9 to 13, the zinc powder prepared according to example 2 of the present invention has a good sphericity and a uniform particle size distribution.
The national center for analysis and test of nonferrous metals and electronic materials tests the powder prepared in example 2 according to the GB/T19077-2016 standard, FIG. 14 is a distribution graph of the particle size of the zinc powder prepared in example 2 of the invention, and as shown in FIG. 4, the D (10) value of the zinc powder prepared in example 2 of the invention is 31.708 microns; a D (50) value of 43.584 microns; the D (100) value was 59.547 μm.
The zinc powders prepared in example 2 of the invention were tested according to the monitoring requirements specified in GB/T6890-2000, table 4 is a table of the test results of the zinc powders prepared in example 2 of the invention, as shown in table 4,
TABLE 4
Example 3
The embodiment of the invention also provides a method for preparing zinc powder by ultrasonic waves, which comprises the following steps:
s101: the lifting device is controlled to ascend, and the top end of the zinc bar with the diameter of 60mm and the purity of more than 99 percent is clamped on the material fixing device in the zinc bar clamping device 101. And then the lifting equipment is controlled to descend to drive the rotating device to descend, and the rotating device is controlled to rotate, so that the zinc bar is rotated and descended. The zinc rod holding apparatus 101 was controlled to insert one end of the zinc rod into the zinc rod melting apparatus 103 at a rotation speed of 60rpm, a lowering speed of 120 mm/min.
S102: firstly, the transducer 201 is started, the transducer 201 drives the amplitude transformer 202 to drive the atomization vibrator 203 to vibrate, the temperature of the atomization vibrator 203 rises under the action of the transducer 201, and the temperature of the atomization vibrator 203 rises above the melting point of zinc. Controlling a zinc bar melting device 103 to melt the zinc bar, wherein an induction heating device is used in the step, coils are divided into two layers, each layer has 4 turns, the total number of turns is 8, a copper pipe 401 is a red copper pipe with the outer diameter of 10mm and the inner diameter of 8mm, the outer diameter of a top coil of a medium-frequency coil is 150mm, the outer diameter of a bottom coil of the medium-frequency coil is 100mm, and the height of the medium-frequency coil is 60 mm; the power of the intermediate frequency coil is 85W, the frequency is 80kHz, and the distance from the bottom of the intermediate frequency coil to the top of the ultrasonic vibrator is 45 mm. The ultrasonic wave transmitting power is 600W, the ultrasonic wave frequency is 45kHz, and the amplitude is 100 micrometers; the distance from the bottom of the intermediate frequency coil to the top of the ultrasonic atomization vibrator is 50 mm; the copper coil is of a hollow structure, and circulating cooling water is contained in the copper coil; the water temperature is 5 ℃. The working frequency of the electromagnetic coil is 100 kHz; the molten zinc formed by melting the zinc rod is dropped on the disk-shaped atomization vibrator 203.
S103: the transducer 201 in the ultrasonic atomization device 200 drives the atomization vibrator 203, and the atomization vibrator 203 breaks up zinc drops into particles; the particles fall under gravity into the powder collection apparatus 300.
The disc-shaped atomization vibrator 203 is horizontally arranged and is positioned at the uppermost part of the ultrasonic atomization device 200, and the disc-shaped atomization vibrator 203 is connected with the transducer 201 through an amplitude transformer 202 which is connected in series up and down; transducer 201 is located below horn 202; the transducer 201 drives the amplitude transformer 202, and the amplitude transformer 202 drives the disc-shaped atomization vibrator 203 to vibrate at high frequency, so that zinc drops dropping on the top surface of the disc-shaped vibrator are atomized into small particles.
In the process of preparing the zinc powder, the lifting device moves downwards, and the zinc rod is continuously inserted into the zinc rod melting device 103; and when the zinc bar is consumed, controlling the lifting device to move upwards, and then replacing the zinc bar.
The quality of the powder is affected by a plurality of factors such as temperature, pressure and the like, so that the process flow for improving the performance of the powder product can obtain the current and frequency data matched with various materials after a large number of repeated tests, for example, the frequency changes along with the current, and the diameter/inner diameter and height of the coil need to be adjusted according to the size of the processed raw material and the ultrasonic atomization device. The matched data can ensure that the effect of the melted bar is matched with the atomizing device to achieve the best state of powder making.
In addition, the production process of zinc powder in the prior art has three types: distillation, meltblowing, and electrolysis. However, the three production processes have the defects of large investment, large pollution, high energy consumption, large loss and small yield; in addition, the prior art also has the problems that the zinc powder production is easy to explode, oversize products of large particles generated by screening need to be reprocessed, the effective zinc powder of the zinc powder is low, the particle size of the zinc powder is concentrated in a range of 60 meshes to 100 meshes, and the service life of a high-pressure nozzle is short.
FIG. 15 is a first scanning electron micrograph of a zinc powder prepared in example 3 of the present invention; FIG. 16 is a second SEM image of a zinc powder prepared in example 3 of the present invention; FIG. 17 is a third scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention; FIG. 18 is a fourth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention; FIG. 19 is a fifth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention; FIG. 20 is a sixth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention; FIG. 21 is a seventh scanning electron micrograph of a zinc powder prepared in example 3 of the present invention; FIG. 22 is an eighth scanning electron micrograph of a zinc powder prepared according to example 3 of the present invention, and as shown in FIGS. 15 to 22, the zinc powder prepared according to example of the present invention has a good sphericity and a uniform particle size distribution.
The national center for analysis and test of nonferrous metals and electronic materials tests the powder prepared in example 3 according to the GB/T19077-2016 standard, FIG. 23 is a distribution graph of the particle size of the zinc powder prepared in example 3 of the invention, and as shown in FIG. 23, the D (10) value of the zinc powder prepared in example 3 of the invention is 54.666 microns; a D (50) value of 80.199 microns; the D (100) value was 119.255 μm.
Compared with the prior art, the embodiment of the invention has high yield; compared with gas atomization, the ultrasonic atomization does not need gas as atomization power, so that the consumption of inert gas is greatly reduced, the cost is reduced, and the ultrasonic atomization device is environment-friendly and free of dust emission. Fig. 6 is a scanning electron microscope image of zinc powder prepared by the method for ultrasonically preparing zinc powder provided in the embodiment of the invention, as shown in fig. 6, the particle size range of the prepared zinc powder is within 20-500 meshes, and the range is larger; high purity, extremely low harmful impurities, high activity and good corrosion resistance, and solves the defect that the zinc powder prepared by a distillation method and an atomization method cannot overcome. . The coating can be widely applied to high-strength anti-corrosion coating materials, is suitable for being exposed in high-corrosion environments of C5-I or C5-M (ISO 12944-2), and is used as long-acting protective spraying in the fields of petrochemical storage tanks and equipment, power stations, bridges, marine facilities, steel structures, harbor machinery, outdoor equipment and the like, matched with other coatings, and has durable corrosion resistance.
In addition, in the embodiment of the present invention, the droplets of the metallic zinc may be changed to be continuous for continuous production; the equipment structure of the embodiment of the invention is simpler, and the equipment investment is reduced; high automation degree, safety, high efficiency and accuracy.
Further, the heating mode of the zinc rod melting device 103 includes, but is not limited to, the following:
the zinc bar with the center positioned at the center can be directly heated by an electromagnetic induction coil;
or after the electromagnetic induction coil heats the annular heating body, the annular heating body heats the zinc rod positioned in the center;
the resistance type heating body can also heat the zinc rod positioned in the center;
the zinc rod or the zinc block can be arranged in a crucible made of graphite, magnesium oxide, aluminum oxide and the like, the crucible is positioned in an alternating electromagnetic field, the alternating electromagnetic field generates eddy current on the surface of the zinc rod or the zinc block in the crucible so as to realize heating, and heated liquid can drip from a small hole at the bottom of the crucible or flow out from a flow channel at the edge of the crucible so as to realize dripping on the ultrasonic vibrator.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. An apparatus for ultrasonically producing a metal powder, the apparatus comprising: a blanking device, an ultrasonic atomization device and a powder collection device which are arranged from top to bottom in sequence, wherein,
the blanking equipment drops the molten metal on an atomization vibrator of the ultrasonic atomization equipment;
the ultrasonic atomizing apparatus includes: the energy converter drives the atomization vibrator to vibrate;
the powder collecting device is used for collecting particles formed by scattering metal drops by the atomizing vibrators, and the particles are cooled into solid in the powder collecting device.
2. The apparatus of claim 1, wherein the blanking device comprises: a metal bar clamping device and a metal bar melting device which are arranged from top to bottom in sequence, wherein,
the metal rod clamping device clamps the top end of the metal rod, and the bottom end of the metal rod is inserted into the metal rod melting device.
3. The apparatus for ultrasonically producing a metal powder as claimed in claim 2, wherein the metal rod melting device comprises: one or a combination of an electromagnetic induction heating device and a resistance heating device.
4. An apparatus for ultrasonic production of metal powder according to claim 3, wherein the metal rod holding means is fixed to a lifting means which carries the metal rod holding means in up and down movement.
5. An apparatus for ultrasonically producing a metallic powder according to claim 4 wherein the centre line of the metal rod is coincident with the centre line of the metal rod melting device.
6. The apparatus of claim 1, wherein the powder collecting device is a chamber structure containing a cooling fluid therein, wherein the cooling fluid comprises; water;
the ultrasonic atomization equipment is positioned in the cavity inside the powder collection equipment and is positioned above the liquid level of the cooling liquid.
7. The apparatus of claim 1, wherein the nebulizer comprises:
one or a combination of disk-shaped atomizing vibrators and spherical atomizing vibrators.
8. Method for the ultrasonic production of metal powders based on the device according to any one of claims 1 to 7, characterized in that it comprises:
clamping one end of a metal rod with the diameter of 1-150mm and the purity of more than 99% on blanking equipment;
controlling blanking equipment to drop metal liquid formed after the metal rod is melted onto ultrasonic atomization equipment;
an energy converter in the ultrasonic atomization equipment drives an atomization vibrator, and the atomization vibrator breaks up metal drops into particles;
the particles fall under gravity into a powder collection device.
9. The method for preparing metal powder by ultrasonic waves according to claim 8, wherein the controlling of the blanking device to drop the metal droplets formed after the metal rod is melted onto the ultrasonic atomization device comprises:
controlling the metal bar clamping equipment to insert one end of the metal bar into the metal bar melting equipment at a rotating speed of 10-60rpm and a descending speed of 10-150 mm/min;
the metal rod melting equipment melts the metal rod into liquid to form metal drops, the metal drops drop on the atomization vibrator, and the ultrasonic power used by the atomization vibrator is 50-8000W; the ultrasonic frequency is 10kHz-150 kHz; the amplitude of the ultrasonic vibrator is 5-100 microns.
10. The method of claim 8, wherein the metal rod melting apparatus is an induction heating apparatus, wherein,
the electromagnetic coil of the induction heating equipment is a D-shaped copper coil, the outer diameter of the coil is 120-150mm, the height of the coil is 50-60mm, and the distance from the bottom of the coil to the top of the ultrasonic atomization vibrator is 25-50 mm; the number of turns is 5-8 turns; the working frequency of the electromagnetic coil is 10 kHz-100 kHz;
the copper coil is of a hollow structure, and circulating cooling water is contained in the copper coil; the water temperature is 3-20 ℃.
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