CN109093128A - A kind of device and method preparing superfine low melting point globular metallic powder by drop atomization - Google Patents
A kind of device and method preparing superfine low melting point globular metallic powder by drop atomization Download PDFInfo
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- CN109093128A CN109093128A CN201811119596.1A CN201811119596A CN109093128A CN 109093128 A CN109093128 A CN 109093128A CN 201811119596 A CN201811119596 A CN 201811119596A CN 109093128 A CN109093128 A CN 109093128A
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- crucible
- turntable
- drop
- shell
- atomization
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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
- 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
- B22F9/10—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 using centrifugal force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
Abstract
The present invention provides a kind of device and method that superfine low melting point globular metallic powder is prepared by drop atomization.Device includes shell, is set to the intracorporal crucible of shell and powder collecting region, it is characterized in that, the turntable that powder collecting region is arranged in is embedded structure, the body portion for the material turntable for selecting thermal conductivity poor, metal material of the angle of wetting less than 90 ° of selection and drop, the atomization plane into main part as turntable is inlayed, is equipped with venthole in turntable.The invention also discloses preparation methods, in conjunction with pulse micropore gunite and centrifugal atomization, cooperate turntable structure and to disc surfaces induction heating, to make molten metal breach the schizotype of conventional melt metal, realize the fibrous divisional mode being only just able to achieve when atomizing medium is aqueous solution or organic solution, leap progress is obtained in terms of micronization, and sphericity height is made, has good fluidity and spreadability, the ultra tiny spherical metal powder of low melting point for meeting requirement without satellite droplet.
Description
Technical field
The invention belongs to superfine spherical particulate preparation technical fields, specifically, more particularly to a kind of using by drop
Atomization prepares the device and method of superfine low melting point globular metallic powder.
Background technique
With the change of technology, globular metallic powder 3D printing rapid shaping, in terms of have
Very big demand, and quality requirement is also being continuously improved.3D printing metal powder requires sphericity high, uniform particle diameter,
Without satellite droplet, there is good spreadability and uniform mobility.
Currently, the method for production spherical metal powder has atomization, including gas atomization, water atomization, centrifugation both at home and abroad
Atomization etc..But the dispersion degree that above-mentioned atomization prepares powder is wider, it is necessary to be used by repeatedly sieving just obtain meeting
It is required that the particle of partial size, and sphericity is poor, there are a large amount of satellite droplet on powder, is unable to satisfy requirement, and produce
Low efficiency.
Powder used in the country is largely dependent on import, is much unable to satisfy the requirement used.Therefore, a kind of prepare is explored
The preparation facilities and method of ultra tiny globular metallic powder high-efficient, powder quality is high are significant.
Summary of the invention
Mobility and spreadability are poor, yield rate is low according to present in existing metal powder preparation process set forth above, effect
The low technical problem of rate, and a kind of device and method that superfine low melting point globular metallic powder is prepared by drop atomization is provided.
The present invention carries out structure design mainly in combination with two methods of pulse micropore gunite and centrifugal atomization, while to turntable, and right
Disc surfaces, which carry out induction heating, to be realized so that molten metal be made to breach the schizotype of conventional melt metal and only works as mist
Change the fibrous divisional mode being just able to achieve when medium is aqueous solution or organic solution, compared with existing centrifugal atomizing technology
Compared with the powder being atomized under this threadiness schizotype can obtain leap progress in terms of micronization, while by this
Mode can be prepared sphericity height, have good fluidity and spreadability, the low melting point for meeting requirement without satellite droplet
Ultra tiny spherical metal powder.
The technological means that the present invention uses is as follows:
A kind of device preparing superfine low melting point globular metallic powder by drop atomization characterized by comprising shell
Body is set to the intracorporal crucible of the shell and powder collecting region, wherein the powder collecting region is placed in the intracorporal bottom of the shell
Portion, the crucible are placed in powder collecting region top；
The crucible is using center line as axis, inside and outside nested circle ring, the bottom of the interior accommodating chamber of the crucible
The centre bore to connect, the bottom of the interior accommodating chamber and the outer accommodating chamber are equipped with the bottom of the outer accommodating chamber of the crucible
Bottom between be equipped with for molten metal circulation space；The interior accommodating chamber of the crucible is equipped with and is arranged outside the shell
The connected drive rod of the piezoelectric ceramics in portion, the drive rod lower end are equipped with tabletting, in interior accommodating chamber described in the tabletting face
Above heart hole；
The shell is equipped with the crucible air inlet pipe being inserted into the crucible, is additionally provided with and the crucible on the shell
Mechanical pump, the diffusion pump being connected are additionally provided with cavity air inlet pipe and cavity vent valve on the shell；
The powder collecting region includes that the catch tray of the housing bottom is arranged in and is set to above the catch tray
The turntable for atomized metal pow der particle being connected to the motor；
It is characterized by:
The turntable includes matrix, and the longitudinal section that described matrix is made of the support portion of the carrier on top and lower part is in class
The main structure of " T-type ", the carrier upper surface are equipped with the circular groove with certain radius coaxial with its center of circle；Its
In, material of the described matrix using thermal conductivity less than 20W/m/k is made；
Be atomized plane, be disc structure, the disk and the circular groove match and with the circular groove interference
Cooperation, the atomization plane are made of the material with atomized drop angle of wetting less than 90 °；
Venthole, perforation are arranged in the carrier and the support portion, the upper surface of the venthole and the mist
Change the lower end face contact of plane, the lower end of the venthole is in communication with the outside；
The periphery of the turntable is additionally provided with load coil.
Above-mentioned crucible form is that metal material is put into outer layer chamber there are the two chambers of inside and outside nesting, molten
It is flowed during melting by liquid, converges to the region of crucible centre bore, by the tabletting and tabletting that are covered on centre bore
The drive rod of side moves down, and sprays drop from the centre bore of crucible bottom.Certainly, crucible form is also not limited to described above
Situation can generate back pressure after being filled with protective gas, liquid is promoted to flow to center as long as there are closed chambers in crucible
The structure type of hole near zone.The volume of the shell wants enough drops to fly after centrifugal breaking and drops to bottom
Range in catch tray can guarantee solidify on the inner wall of the housing, and the area of catch tray will guarantee sufficiently large can receive
Collect powder.
Preferably, the height of matrix is 10-20mm, and the height of support portion should not be too high, and the height less than carrier is advisable.
The upper surface of the atomization plane protrudes from the carrier upper surface, and protrusion range is 0.1-0.5mm.As long as protrusion height is full
Foot is conducive to discrete molten drop and does not contact matrix, directly flies in chamber and falls into catch tray.The carrier it is straight
Diameter range is in 10-100mm, and the diameter range of the circular groove is in 5-90mm.
Described matrix is made of zirconia ceramic, silica glass or stainless steel, is not limited to above-mentioned several materials
Matter, as long as meeting the material that thermal conductivity is less than 20W/m/k.The upper surface of the venthole is less than or equal to the atomization plane
Lower end surface, the purpose of venthole setting be it is cleaner in order to be taken out the gas of turntable internal clearance when vacuumizing, turn
It is safer when disk high speed rotation, therefore the upper surface of venthole and the contact area of the lower end surface of atomization plane vacuumize more greatly
When atomization plane stability it is better.
Further, it is equipped with thermocouple in the crucible, is additionally provided with resistance heater on the outside of the crucible.Preferably, earthenware
The angle of wetting of the material of crucible and molten metal disposed within is greater than 90 °.
Further, the center-hole diameter range of the crucible is between 0.02mm-2.0mm.
Further, the revolving speed of the turntable is 10000rpm-50000rpm.
Further, the heating thickness range of the load coil is between 5-20mm, it and setting are in the shell
External frequency converter is connected with regulated power supply, and the control reference voltage of the regulated power supply is between 0-50V.
Further, on the top-down direction of described device, the piezoelectric ceramics, the drive rod, the crucible,
The resistance heater, the tabletting, the turntable and the load coil are located on same axis.
Superfine low melting point spherical metal powder is prepared by drop atomization using above-mentioned device the invention also discloses a kind of
The method at end, it is characterised in that include the following steps,
1. charging: being sealed after the metal material wait melt is put into the crucible that shell internal upper part is arranged in；
2. vacuumizing: being vacuumized using mechanical pump and diffusion pump to the crucible and the shell, and it is lazy to be filled with high-purity
Property protective gas (usually select helium or argon gas), so that pressure in shell is reached preset value；
3. resistance heating: using the heating parameters of resistance heater according to the setting of the fusing point of raw material to be heated, and pass through
Temperature in crucible described in the thermocouple real-time monitoring being arranged in the crucible, keeps the temperature after metal material is completely melt；
4. induction heating: making turntable high speed rotation under preset rotation speed using motor, followed by induction heating line
High-speed rotating disk upper surface is heated to the melting temperature of metal material or more by circle；
4. prepared by particle: by the way that the first air inlet pipe of crucible on the housing and being inserted into the crucible, earthenware is arranged
High-purity inert protective gas is passed through by the second air inlet pipe of crucible, and back pressure is generated in the crucible, promotes molten metal to fill up described
The centre bore of crucible bottom；Inputting the pulse signal of certain wave mode to piezoelectric ceramics, the piezoelectric ceramics is generated to bottom offset, by
The drive rod being connected with the piezoelectric ceramics and the tabletting being arranged in below the drive rod pass to centre bore near zone
Molten metal, so that molten metal sprays to form symmetrical liquid drop from center bottom hole portion；
Symmetrical liquid drop freely drops on high-speed rotating turntable, and the symmetrical liquid drop under molten condition is first dropped in turntable
Center, since centrifugal force is smaller at this time, drop will not by once it is discrete go out, but can it is rounded spread on turntable, when
Spread into a certain range centrifugal force it is sufficiently large when, the metal sprawled can be linear in fiber on turntable under the influence of centrifugal force
Discrete finally to split into small drop and fly out to disk edge, microlayer model solidifies in dropping process without container, forms metal
Powder is drop on catch tray, while tabletting and drive rod being restPosed, and the molten bath in the crucible is to central hole
Supplement molten metal liquid；
5. particle collection: collecting uniform-spherical metal powder with the catch tray for being set to the housing bottom.
Further, it is the outer accommodating chamber volume that the metal material, which is encased in the charge weight in the outer accommodating chamber,
50%-70%.
Further, the pressure after vacuumizing in the shell reaches 0.1MPa, when metal material is kept the temperature after being completely melt
Between be 15-20 minutes.
Further, the induction heating voltage range of the load coil is 0-50V, and the induction heating time is 5-
15min。
Compared with the prior art, the invention has the following advantages that
The invention discloses a kind of prepared in conjunction with centrifugal atomization by drop atomization using pulse micropore gunite to surpass
The device and method of thin low melting point globular metallic powder, effect of the molten metal material in pressure and pulse-type disturbance in crucible
Under, it is sprayed by crucible bottom centre bore, forms symmetrical liquid drop, symmetrical liquid drop drops on high-speed rotating turntable, and in circle
It is sprawled on disk, the metal sprawled can be linear discrete to disk edge in fiber on turntable under the influence of centrifugal force, finally divides
It is cleaved into small drop to fly out, microlayer model solidifies in dropping process without container.The gold of traditional pulse micropore gunite production
It is consistent to belong to particle sphericity height, hot resume, but the powder produced also fails to reach micronization, in conjunction with centrifugal atomization
Afterwards, the fiber threadiness division for realizing molten metal, which greatly improves the miniaturization of metal powder (partial size is less than 50 μm),
And size tunable may be implemented, meet the needs of forming technique.
Further more, turntable disclosed by the invention is embedded structure, using the poor i.e. thermal conductivity of thermal conductivity less than 20W/m/k's
Material can effectively reduce the heat being transmitted on high-speed motor by turntable as matrix, prevent it from influencing the normal work of high-speed motor
Make；Have material of the good wettability, that is, angle of wetting less than 90 ° as atomization plane using with atomization melt material, is conducive to liquid
Sprawling in atomization plane is dripped, so as to so that molten metal atomization is abundant；Plane and matrix inner wall are atomized using interference fit
Mode is fixed, and guarantees that turntable is atomized plane when rotating at high speed and will not fly out, it is ensured that its safety；Atomization plane be installed to turn
When on disk, stomata can be had by being atomized between plane and matrix, when to cavity pumping high vacuum, will make to be atomized the generation of plane both ends
Great pressure difference influences the stability for being atomized plane, therefore setting one is logical between the carrier and support portion of turntable matrix
Stomata is in communication with the outside plane lower end surface is atomized, and is consistent atomization plane pressure at two ends, is further ensured that high speed centrifugation
The stability and safety of turntable when atomization.
Process controllability of the invention is strong, shows following several points: accurately controlling crucible by resistance heater
Temperature；By being passed through inert gas into crucible and shell, the pressure difference of crucible and shell can control, while making in crucible chamber
Molten metal constantly supplemented into crucible centre bore；The size of crucible bottom centre bore can control the size of drop；Induction
Heating coil can control the temperature of disc surfaces, and the revolving speed of turntable is controllable, can control the threadiness division effect of molten metal
Fruit, so as to further control the particle diameter distribution of metal microparticle；Technological parameter it is adjustable with it is controllable, it is available to surpass
Fine globular metallic powder.
The present invention can efficiently prepare the ultra micro fine metal powder for meeting requirement, and size tunable, distributed area are narrow,
Sphericity is high, hot resume are consistent, structure is simple, at low cost, yield is high, is suitable for industrialized production.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the structural diagram of the present invention.
Fig. 2 is the structural schematic diagram of turntable of the present invention.
Fig. 3 is the comparison diagram of the powder and powder made from unmodified device that are prepared using apparatus of the present invention and method,
Wherein, (a) is powder prepared by the present invention, (b) is the powder of prior art preparation.
Fig. 4 is turntable of the invention its surface and the surface comparison diagram after former rotating dishpan experiment after the test, wherein (a) is
It is (b) disc surfaces in the prior art in the disc surfaces of threadiness division.
Fig. 5 is disc surfaces liquid stream line chart of the invention, wherein (a) is position liquid fluid line among turntable, (b) is turntable
Edge liquid fluid line.
In figure: 1, piezoelectric ceramics；2, the first air inlet pipe of crucible；3, drive rod；4, resistance heater 5, tabletting；6, right part is molten
Pond；7, crucible；8, cavity；9, turntable；10, motor；11, metal powder；12, catch tray；13, shell；14, induction heating line
Circle；15, drop；16, cavity air inlet pipe；17, mechanical pump；18, diffusion pump；19, cavity vent valve；20, left part molten bath；21, earthenware
The second air inlet pipe of crucible；22, carrier；23, support portion；24, it is atomized plane；25, venthole.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.It is real to the description of at least one exemplary embodiment below
It is merely illustrative on border, never as to the present invention and its application or any restrictions used.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Unless specifically stated otherwise, positioned opposite, the digital table of the component and step that otherwise illustrate in these embodiments
It is not limited the scope of the invention up to formula and numerical value.Simultaneously, it should be clear that for ease of description, each portion shown in attached drawing
The size divided not is to draw according to actual proportionate relationship.Technology known for person of ordinary skill in the relevant, side
Method and equipment may be not discussed in detail, but in the appropriate case, and the technology, method and apparatus should be considered as authorizing explanation
A part of book.In shown here and discussion all examples, appointing should be construed as merely illustratively to occurrence, and
Not by way of limitation.Therefore, the other examples of exemplary embodiment can have different values.It should also be noted that similar label
Similar terms are indicated in following attached drawing with letter, therefore, once it is defined in a certain Xiang Yi attached drawing, then subsequent attached
It does not need that it is further discussed in figure.
In the description of the present invention, it is to be understood that, the noun of locality such as " front, rear, top, and bottom, left and right ", " it is laterally, vertical,
Vertically, orientation or positional relationship indicated by level " and " top, bottom " etc. is normally based on orientation or position shown in the drawings and closes
System, is merely for convenience of description of the present invention and simplification of the description, in the absence of explanation to the contrary, these nouns of locality do not indicate that
It must have a particular orientation or be constructed and operated in a specific orientation with the device or element for implying signified, therefore cannot manage
Solution is limiting the scope of the invention: the noun of locality " inside and outside " refers to inside and outside the profile relative to each component itself.
For ease of description, spatially relative term can be used herein, as " ... on ", " ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be understood that spatially relative term is intended to comprising the orientation in addition to device described in figure
Except different direction in use or operation.For example, being described as if the device in attached drawing is squeezed " in other devices
It will be positioned as " under other devices or construction after part or construction top " or the device of " on other devices or construction "
Side " or " under its device or construction ".Thus, exemplary term " ... top " may include " ... top " and
" in ... lower section " two kinds of orientation.The device can also be positioned with other different modes and (is rotated by 90 ° or in other orientation), and
And respective explanations are made to the opposite description in space used herein above.
In addition, it should be noted that, limiting components using the words such as " first ", " second ", it is only for be convenient for
Corresponding components are distinguished, do not have Stated otherwise such as, there is no particular meanings for above-mentioned word, therefore should not be understood as to this
The limitation of invention protection scope.
As shown in Figure 1, the present invention provides a kind of dresses for preparing superfine low melting point globular metallic powder by drop atomization
It sets, comprising: shell 13, the crucible 7 and powder collecting region being set in the shell 13, wherein the powder collecting region is placed in
Bottom in the shell 13, the crucible 7 are placed in powder collecting region top；
The crucible 7 is seen to divide crucible 7 from figure and is using center line as axis, inside and outside nested circle ring
The two chambers of left and right, i.e. left part molten bath 20 and right part molten bath 6, substantial two molten baths are (outer in the same annular compartment
In accommodating chamber), in actual use can according to prepare powder number come to the molten bath of side inject metal material, can portion
Divide or all pours into；The bottom of the outer accommodating chamber of the bottom of the interior accommodating chamber of the crucible 7 and the crucible 7, which is equipped with, to connect
Centre bore is equipped with the space for molten metal circulation between the bottom of the interior accommodating chamber and the bottom of the outer accommodating chamber；
The interior accommodating chamber of the crucible 7 is equipped with the drive rod 3 being connected with the piezoelectric ceramics 1 being arranged in outside the shell 13, the biography
3 lower end of lever is equipped with tabletting 5, the centre bore top of interior accommodating chamber described in 5 face of tabletting；
The position in left part molten bath 20 and right part molten bath 6 on the shell 13 also in corresponding diagram is equipped with and is inserted into the earthenware
Crucible air inlet pipe in crucible 7 respectively corresponds to second air inlet pipe of crucible 21 in left part molten bath 20 and the crucible in corresponding right part molten bath 6
First air inlet pipe 2 is additionally provided with the mechanical pump 17 being connected with the crucible 7, diffusion pump 18, the shell 13 on the shell 13
On be additionally provided with cavity air inlet pipe 16 and cavity vent valve 19；
The powder collecting region includes that the catch tray 12 of the housing bottom is arranged in and is set on the catch tray 12
The turntable 9 for atomized metal pow der particle of side being connected with motor 10；
As shown in Fig. 2, the turntable 9 includes matrix, described matrix is by the carrier 22 on top and the support portion 23 of lower part
The longitudinal section of composition be in class " T-type " main structure, 22 upper surface of carrier be equipped with its center of circle it is coaxial have centainly
The circular groove of radius；Wherein, material of the described matrix using thermal conductivity less than 20W/m/k is made；
Be atomized plane 24, be disc structure, the disk and the circular groove match and with the circular groove mistake
It is full of cooperation, the atomization plane 24 with material of 15 angle of wetting of atomized drop less than 90 ° using being made；
Venthole 25, perforation are arranged in the carrier 22 and the support portion 23, the upper surface of the venthole 25
With the lower end face contact of the atomization plane 24, the lower end of the venthole 25 is in communication with the outside；
The periphery of the turntable 9 is additionally provided with load coil 14.The heating thickness range of the load coil 14
Between 5-20mm, it is connected with the frequency converter and regulated power supply being arranged in outside the shell 13, the voltage of the regulated power supply
Control range is between 0-50V.Make turntable high speed rotation under preset rotation speed using motor, followed by induction heating line
High-speed rotating 9 upper surface of turntable is heated to the melting temperature of metal material or more by circle 14；
The center-hole diameter range of the crucible 7 is between 0.02mm-2.0mm.
The revolving speed of the turntable is 10000rpm-50000rpm.
On the top-down direction of described device, the piezoelectric ceramics 1, the drive rod 3, the crucible 7, the electricity
Resistance heater 4, the tabletting 5, the turntable 9 and the load coil 14 are located on same axis.
When work, the crucible 7 and the shell 13 are vacuumized using mechanical pump 17 and diffusion pump 18, are being passed through inertia
Under conditions of gas generates back pressure, the material for needing preparation in crucible 7 is heated using resistance heater 4, gives piezoelectric ceramics 1
The pulse signal of certain wave mode is inputted, piezoelectric ceramics 1 is generated to bottom offset, passes to 7 center of crucible by drive rod 3 and tabletting 5
The molten metal of hole near zone, so that molten metal sprays to form symmetrical liquid drop 15, uniform liquid from the centre bore of crucible bottom
Drop 15 freely drops on high-speed rotating rotating circular disk 9, and the symmetrical liquid drop 15 under molten condition is first dropped in rotating circular disk 9
Center, since centrifugal force is smaller at this time, drop 15 will not be gone out by once discrete, but rounded can spread over rotating circular disk 9
On, when spread into a certain range centrifugal force it is sufficiently large when, the metal sprawled can under the influence of centrifugal force, on rotating circular disk 9
It is linear discrete to 9 edge of rotating circular disk in fiber, it finally splits into small drop and flies out, microlayer model is in dropping process without appearance
Device solidification, forms metal powder 11, drop on catch tray 12.
Superfine low melting point spherical metal powder is prepared by drop atomization using above-mentioned device the invention also discloses a kind of
The method at end, includes the following steps,
1. charging: being sealed after the metal material wait melt being put into the crucible 7 that 13 internal upper part of shell is arranged in；The gold
Belong to material and is encased in the 50%-70% that the charge weight in the outer accommodating chamber is the outer accommodating chamber volume.
2. vacuumizing: being vacuumized using mechanical pump 17 and diffusion pump 18 to the crucible 7 and the shell 13, and be filled with height
Purity inert protective gas makes pressure in shell 13 reach preset value；Pressure after vacuumizing in the shell 13 reaches
0.1MPa, metal material are completely melt that rear soaking time is 15-20 minutes.
3. resistance heating: using the heating parameters of resistance heater 4 according to the setting of the fusing point of raw material to be heated, and pass through
Temperature in crucible 7 described in the thermocouple real-time monitoring being arranged in the crucible 7, keeps the temperature after metal material is completely melt；
4. induction heating: making the turntable 9 high speed rotation under preset rotation speed using motor 10, followed by induction heating
High-speed rotating 9 upper surface of turntable is heated to the melting temperature of metal material or more by coil 14；The load coil 14
Induction heating voltage range be 0-50V, the induction heating time be 5-15min.
4. prepared by particle: passing through the first air inlet pipe of crucible being arranged on the shell 13 and be inserted into the crucible 7
2, high-purity inert protective gas is passed through by the second air inlet pipe of crucible 21, generates back pressure in the crucible 7, molten metal is promoted to fill out
The centre bore of full 7 bottom of crucible；Input the pulse signal of certain wave mode to piezoelectric ceramics 1, the piezoelectric ceramics 1 generate to
Bottom offset passes to center by the drive rod 3 being connected with the piezoelectric ceramics 1 and the tabletting 5 being arranged in below the drive rod 3
The molten metal of hole near zone, so that molten metal sprays to form symmetrical liquid drop 15 from center bottom hole portion；
Symmetrical liquid drop 15 freely drops on high-speed rotating turntable 9, and the symmetrical liquid drop 15 under molten condition is first dropped in
The center of turntable 9, since centrifugal force is smaller at this time, drop 15 will not be gone out by once discrete, but rounded can spread over and turn
On disk 9, when spread into a certain range centrifugal force it is sufficiently large when, the metal sprawled can be on turntable 9 under the influence of centrifugal force
Fiber is linear discrete to 9 edge of turntable, finally splits into small drop and flies out, microlayer model is solidifying without container in dropping process
Gu forming metal powder 11, it drop on catch tray 12, while tabletting 5 and drive rod 3 being restPosed, the crucible 7
Interior molten bath supplements molten metal liquid to central hole；
5. particle collection: collecting uniform-spherical metal powder with the catch tray 12 for being set to the housing bottom.
Embodiment 1
The specific embodiment of Sn63Pb37 alloy spherical powder is prepared using device batch as shown in Figure 1:
Sn63Pb37 welding wire is cut into the segment of 5mm or so, is put into the molten bath of crucible 7 after carrying out ultrasonic vibration cleaning,
The center bore size of crucible is selected according to demand, and center-hole diameter range is between 0.02mm-2.0mm, such as 25 μm -50 of preparation
μm particle, selects the centre bore of 0.02mm-1.0mm, such as prepares 50 μm of -100 μm of particles, selects the centre bore of 1.0mm-2.0mm；
The amount of being put into of Sn63Pb37 raw material reaches the 50%-70% of molten bath volume；
The crucible 7 and the shell 13 are vacuumized using mechanical pump 17 and diffusion pump 18, are extracted into 0.001pa；It utilizes
The first air inlet pipe of crucible 2 and the second air inlet pipe of crucible 20, cavity air inlet pipe 16 is passed through inert gas argon gas, makes shell 13, crucible 7
Interior pressure reaches 0.1MPa；
Resistance heater 4 is installed on crucible 7, thermocouple is inserted into 7 bottom of crucible；The edge copper stainless steel of choice experiment
Turntable 9 is installed on motor 10, in 9 periphery installation load coil 14 of turntable, rear seal casinghousing 13；
Crucible 7 is heated using resistance heater 4, heating temperature is 260 DEG C, and heating speed is 15 DEG C/min, is protected
Warm 10min melts the metal material in crucible 7 all；
Make the 9 revolving speed 24000r/min of turntable using motor 10, the induction that load coil 14 is then arranged adds
Thermal voltage is 21V, and induction heating current 8A, the induction heating time is 10min, and high-speed rotating 9 surface of turntable is heated to
183 DEG C of melting temperature or more of metal material；
The pulse signal of trapezoidal wave is inputted to piezoelectric ceramics 1, and it is 100Hz that frequency, which is arranged, piezoelectric ceramics 1 is generated to bottom
It moves, the molten metal of 7 centre bore near zone of crucible is passed to by drive rod 3 and tabletting 5, so that molten metal is from crucible bottom
Centre bore spray to form symmetrical liquid drop 15, symmetrical liquid drop 15 freely drops on high-speed rotating turntable 9, under molten condition
Symmetrical liquid drop 15 is first dropped in the center of turntable 9, and since centrifugal force is smaller at this time, drop 15 will not be gone out by once discrete, and
Be can it is rounded spread on turntable 9, when spread into a certain range centrifugal force it is sufficiently large when, the metal sprawled can be in centrifugal force
It is linear discrete to 9 edge of turntable in fiber on turntable 9 under effect, it finally splits into small drop and flies out, microlayer model is under
It is solidified during falling without container, forms metal powder 11, drop on catch tray 12.
After to be prepared, stop applying trapezoidal wave pulse signal to piezoelectric ceramics 1, i.e. the injection of stopping drop；Stop high
Speed motor 10, so that turntable 9 stops rotating；Resistance heater 4 and load coil 14 are closed, room temperature is down to temperature, takes
Metal powder 11 in catch tray 12 out；Cavity air inlet pipe 16 and crucible are finally closed into the second air inlet of the first tracheae 2 and crucible
Crucible 7 and shell 13 are extracted into low vacuum 5Pa hereinafter, to make equipment when deactivated in vacuum shape with mechanical pump 10 by pipe 20
State.
As shown in figure 3, can be seen that powder diameter made from the prior art is thicker from (b), and there is hemisphere generation, and (a)
In for the powder that is prepared by means of the present invention, powder diameter has obtained apparent miniaturization, and granule size satisfaction makes
With requiring, and sphericity is got higher, and powder surface topography also improves, and is generated without hemisphere.
As shown in figure 4, being the atomizing disk obtained after prior art atomization in (b), due to being atomized the gold of disk material and preparation
It is too small and too low in atomization process turntable temperature to belong to dusty material wetability, causes liquid in membranaceous division, and atomization surface
It will appear thicker solidification liquid film, the liquid film surface is very coarse, is unfavorable for the further atomization of subsequent metal drop, can be tight
Ghost image rings atomizing effect and nebulization efficiency.(a) atomization surface to obtain by the method for the invention, it can be seen that spray patterns turn
Become apparent fibrous schizotype, linear schizotype substantially increases the miniaturization and production efficiency of metal powder.
As shown in figure 5, (a) is the liquid fluid line at position among turntable, 50 μm can be both less than with the width of liquid fluid line from figure,
The reason of so as to illustrate the miniaturization of the powder as made from this method, is precisely due to fine fibrous liquid stream is atomized and to be formed
's.It (b) is the liquid fluid line of disk edge, it can be seen that have the trace left after droplet outflow, so as to illustrate molten metal
It is all to go out by complete centrifugal atomizing edge is discrete.
To sum up, the present invention makes molten metal breach the schizotype of conventional melt metal, realizes and only works as atomizing medium
It is this compared with existing centrifugal atomizing technology for the fibrous divisional mode being just able to achieve when aqueous solution or organic solution
The powder being atomized under linear schizotype can obtain leap progress in terms of micronization, while can be with by this mode
Sphericity height is prepared, has good fluidity and spreadability, the ultra tiny gold of low melting point for meeting requirement without satellite droplet
Belong to spherical powder.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (9)
1. a kind of device for preparing superfine low melting point globular metallic powder by drop atomization characterized by comprising shell
(13), crucible (7) and the powder collecting region being set in the shell (13), wherein the powder collecting region is placed in the shell
Bottom in body (13), the crucible (7) are placed in powder collecting region top；
The crucible (7) is using center line as axis, inside and outside nested circle ring, the bottom of the interior accommodating chamber of the crucible (7)
The bottom of the outer accommodating chamber of portion and the crucible (7) is equipped with the centre bore to connect, the bottom of the interior accommodating chamber and described outer
The space for molten metal circulation is equipped between the bottom of accommodating chamber；The interior accommodating chamber of the crucible (7) is equipped with to exist with setting
The connected drive rod (3) of the external piezoelectric ceramics (1) of the shell (13), drive rod (3) lower end are equipped with tabletting (5), institute
Above the centre bore for stating interior accommodating chamber described in tabletting (5) face；
The shell (13) is equipped with the crucible air inlet pipe that is inserted into the crucible (7), be additionally provided on the shell (13) with
Mechanical pump (17) that the crucible (7) is connected, diffusion pump (18), be additionally provided on the shell (13) cavity air inlet pipe (16) and
Cavity vent valve (19)；
The powder collecting region includes that the catch tray (12) of the housing bottom is arranged in and is set on the catch tray (12)
The turntable (9) for atomized metal pow der particle of side being connected with motor (10)；
It is characterized by:
The turntable (9) includes matrix, and described matrix is made of vertical the support portion (23) of the carrier (22) on top and lower part
Section is in the main structure of class " T-type ", carrier (22) upper surface be equipped with its center of circle it is coaxial there is certain radius
Circular groove；Wherein, material of the described matrix using thermal conductivity less than 20W/m/k is made；
Be atomized plane (24), be disc structure, the disk and the circular groove match and with the circular groove interference
Cooperation, the atomization plane (24) use and are made with material of atomized drop (15) angle of wetting less than 90 °；
Venthole (25), perforation setting in the carrier (22) and the support portion (23), the venthole (25) it is upper
The lower end face contact of end face and atomization plane (24), the lower end of the venthole (25) is in communication with the outside；
The periphery of the turntable (9) is additionally provided with load coil (14).
2. the device according to claim 1 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, the center-hole diameter range of the crucible (7) is between 0.02mm-2.0mm.
3. the device according to claim 1 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, the revolving speed of the turntable (9) is 10000rpm-50000rpm.
4. the device according to claim 1 for preparing superfine low melting point globular metallic powder by drop atomization, feature
Be, the heating thickness range of the load coil (14) between 5-20mm, it and setting the shell (13) outside
Frequency converter be connected with regulated power supply, the control reference voltage of the regulated power supply is between 0-50V.
5. the device according to claim 1 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, on the top-down direction of described device, the piezoelectric ceramics (1), the drive rod (3), the crucible (7), institute
It states resistance heater (4), the tabletting (5), the turntable (9) and the load coil (14) and is located at same axis
On.
6. a kind of device using as described in claim 1-5 any one claim prepares ultra-fine eutectic by drop atomization
The method of point globular metallic powder, it is characterised in that include the following steps,
1. charging: the metal material wait melt is put into sealing after being arranged in the crucible (7) of shell (13) internal upper part；
2. vacuumizing: being vacuumized, and filled to the crucible (7) and the shell (13) using mechanical pump (17) and diffusion pump (18)
Enter high-purity inert protective gas, shell (13) interior pressure is made to reach preset value；
3. resistance heating: using the heating parameters of resistance heater (4) according to the setting of the fusing point of raw material to be heated, and pass through institute
The temperature in crucible (7) described in the thermocouple real-time monitoring being arranged in crucible (7) is stated, is kept the temperature after metal material is completely melt；
4. induction heating: making the turntable (9) high speed rotation under preset rotation speed using motor (10), followed by induction heating
High-speed rotating turntable (9) upper surface is heated to the melting temperature of metal material or more by coil (14)；
4. prepared by particle: passing through the first air inlet pipe of crucible for being arranged on the shell (13) and being inserted into the crucible (7)
(2), high-purity inert protective gas is passed through by the second air inlet pipe of crucible (21), and back pressure is generated in the crucible (7), promotes to melt
Metal fills up the centre bore of the crucible (7) bottom；The pulse signal of certain wave mode, the piezoelectricity are inputted to piezoelectric ceramics (1)
Ceramic (1) is generated to bottom offset, by the drive rod (3) being connected with the piezoelectric ceramics (1) and is arranged under the drive rod (3)
The tabletting (5) of side passes to the molten metal of centre bore near zone, so that molten metal sprays to be formed from center bottom hole portion
Even drop (15)；
Symmetrical liquid drop (15) freely drops on high-speed rotating turntable (9), and the symmetrical liquid drop (15) under molten condition first drips
At the center of turntable (9), since centrifugal force is smaller at this time, drop (15) will not be gone out by once discrete, but can rounded paving
Exhibition on turntable (9), when spread into a certain range centrifugal force it is sufficiently large when, the metal sprawled can under the influence of centrifugal force,
It is linear discrete to turntable (9) edge in fiber on turntable (9), it finally splits into small drop and flies out, microlayer model was falling
It is solidified in journey without container, is formed metal powder (11), drop on catch tray (12), while tabletting (5) and drive rod (3) is extensive
Original state is answered, the molten bath in the crucible (7) supplements molten metal liquid to central hole；
5. particle collection: collecting uniform-spherical metal powder with the catch tray (12) for being set to the housing bottom.
7. the method according to claim 6 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, the metal material is encased in the 50%-70% that the charge weight in the outer accommodating chamber is the outer accommodating chamber volume.
8. the method according to claim 6 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, the pressure after vacuumizing in the shell (13) reaches 0.1MPa, and metal material is completely melt that rear soaking time is 15-20
Minute.
9. the method according to claim 6 for preparing superfine low melting point globular metallic powder by drop atomization, feature
It is, the induction heating voltage range of the load coil (14) is 0-50V, and the induction heating time is 5-15min.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811119596.1A CN109093128A (en) | 2018-09-25 | 2018-09-25 | A kind of device and method preparing superfine low melting point globular metallic powder by drop atomization |
| PCT/CN2019/107696 WO2020063619A1 (en) | 2018-09-25 | 2019-09-25 | Device and method for preparing superfine low-melting-point spherical metal powder using one-by-one droplet atomization method |
| RU2021103035A RU2765190C1 (en) | 2018-09-25 | 2019-09-25 | Device and method for producing superfine low-melting spherical metal powder using drop spraying |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811119596.1A CN109093128A (en) | 2018-09-25 | 2018-09-25 | A kind of device and method preparing superfine low melting point globular metallic powder by drop atomization |
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|---|---|
| CN109093128A true CN109093128A (en) | 2018-12-28 |
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| CN201811119596.1A Pending CN109093128A (en) | 2018-09-25 | 2018-09-25 | A kind of device and method preparing superfine low melting point globular metallic powder by drop atomization |
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| Country | Link |
|---|---|
| CN (1) | CN109093128A (en) |
| RU (1) | RU2765190C1 (en) |
| WO (1) | WO2020063619A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020063627A1 (en) * | 2018-09-25 | 2020-04-02 | 大连理工大学 | Rotary disc structure special for drop-by-drop centrifugal atomization method |
| WO2020063619A1 (en) * | 2018-09-25 | 2020-04-02 | 大连理工大学 | Device and method for preparing superfine low-melting-point spherical metal powder using one-by-one droplet atomization method |
| CN113724992A (en) * | 2021-08-26 | 2021-11-30 | 中国科学院江西稀土研究院 | Neodymium iron boron rare earth permanent magnet waste regenerated magnet and preparation method thereof |
| JP2022548571A (en) * | 2019-09-18 | 2022-11-21 | 河南科技大学 | 3D printing apparatus and method by centrifugal atomization |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115430947B (en) * | 2022-09-29 | 2024-01-30 | 郑州机械研究所有限公司 | Preparation method of granular coating brazing filler metal |
| CN117548679B (en) * | 2024-01-09 | 2024-03-22 | 湖南艾缇欧新材料有限公司 | Tin powder preparation equipment and operation method |
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Also Published As
| Publication number | Publication date |
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| RU2765190C1 (en) | 2022-01-26 |
| WO2020063619A1 (en) | 2020-04-02 |
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Application publication date: 20181228 |