CN109047785A - A kind of device and method efficiently preparing low melting point globular metallic powder by drop centrifugal atomization - Google Patents

A kind of device and method efficiently preparing low melting point globular metallic powder by drop centrifugal atomization Download PDF

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Publication number
CN109047785A
CN109047785A CN201811116484.0A CN201811116484A CN109047785A CN 109047785 A CN109047785 A CN 109047785A CN 201811116484 A CN201811116484 A CN 201811116484A CN 109047785 A CN109047785 A CN 109047785A
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CN
China
Prior art keywords
crucible
turntable
drop
shell
powder
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Pending
Application number
CN201811116484.0A
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Chinese (zh)
Inventor
董伟
许富民
孟瑶
朱胜
王晓明
白兆丰
王延洋
韩阳
李国斌
赵阳
石晶
韩国峰
王思捷
常青
任志强
滕涛
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Dalian University of Technology
Academy of Armored Forces of PLA
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Dalian University of Technology
Academy of Armored Forces of PLA
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Application filed by Dalian University of Technology, Academy of Armored Forces of PLA filed Critical Dalian University of Technology
Priority to CN201811116484.0A priority Critical patent/CN109047785A/en
Publication of CN109047785A publication Critical patent/CN109047785A/en
Priority to AU2019351409A priority patent/AU2019351409A1/en
Priority to PCT/CN2019/107697 priority patent/WO2020063620A1/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/10Making 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

Abstract

The present invention provides a kind of device and method that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization.Device includes shell, is set to the intracorporal crucible of shell and powder collecting region, it is characterized by: turntable is embedded structure, the poor material of main body'choice thermal conductivity, it is atomized metal material of the angle of wetting less than 90 ° of plane selection and drop, stability when increasing venthole on turntable axis and improving disk rotational, turntable are externally provided with load coil.Present invention combination 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

A kind of device efficiently preparing low melting point globular metallic powder by drop centrifugal atomization And method
Technical field
The invention belongs to superfine spherical particulate preparation technical fields, specifically, more particularly to a kind of using by drop Centrifugal atomization efficiently prepares the device and method of low melting point globular metallic powder.
Background technique
Globular metallic powder as a kind of important raw material of industry, 3D printing, Electronic Packaging, semiconductor integrated circuit, The fields such as new energy are widely used.With equipment micromation, high-precision development, above-mentioned field to spherical powder and More stringent requirements are proposed for its technology of preparing, especially metal powder rapid shaping field.
At present the whole world to metal material carry out 3D printing demand it is very urgent, as stainless steel, titanium alloy, nickel-base alloy, Silver and gold etc., but these printing techniques also fail to be rapidly developed at present, and wherein metal powder technology of preparing, which becomes, restricts 3D One of the critical issue of printing technique development.3D printing technique requires metal powder that need to meet tiny partial size, narrow particle size distribution, ball The performances such as shape degree is high, easily sprawl, good fluidity and apparent density height.But powder used in the country is largely dependent on import, much It is unable to satisfy the requirement of 3D printing.Therefore, the ultra tiny spherical metal powder that a kind of preparation efficiency is high, powder quality is high is explored Preparation method is significant.
The method of production globular metallic powder mainly has both at home and abroad at present: atomization and pulse micropore emerging in recent years spray Penetrate method.The distribution of powder diameter made from atomization is wide, it is necessary to by repeatedly screening the powder that can be just met the requirements, yield rate It is low;Contain a large amount of satellite droplet in atomized powder, declines its mobility and spreadability;In addition, in conventional centrifugal atomization process In, when melt temperature and excessively high revolving speed, melt easily breaks away, and seriously affects nebulization efficiency.Pulse micropore sprays legal system Although powder sphericity it is high, uniform particle diameter, this method prepare it is inefficient when small particle particle, and application range by To limitation.
Therefore, the powder of both methods production is all unable to satisfy requirements, researches and develops that a kind of preparation efficiency is high, powder quality height Ultra tiny spherical metal powder preparation method it is significant.
Summary of the invention
The poor, yield rate according to the 3D printing set forth above mobility present in metal powder preparation process and spreadability The problems such as low, low efficiency, and provide it is a kind of by drop centrifugal atomization efficiently prepare low melting point globular metallic powder device and Method.The present invention carries out structure mainly in combination with two methods of pulse micropore liquid droplet ejection method and centrifugal atomization, while to turntable Design, and induction heating is carried out to disc surfaces, so that molten metal bath is made to breach the schizotype of conventional melt metal, it is real The fibrous divisional mode being only just able to achieve when atomizing medium is aqueous solution or organic solution is showed, with existing centrifugation mist Change technology compares, and the powder being atomized under this threadiness schizotype can obtain leap progress in terms of micronization, from And can be prepared partial size is very small, particle diameter distribution section is narrow and controllable, sphericity is high, have good fluidity and spreadability, No satellite droplet, nebulization efficiency height, the very high ultra tiny spherical metal powder for meeting 3D printing requirement of fine powder recovery rate.
The technological means that the present invention uses is as follows:
A kind of device efficiently preparing low melting point globular metallic powder by drop centrifugal atomization, including shell, be set to The intracorporal crucible of the shell and powder collecting region, the powder collecting region are placed in the bottom of the shell, and the crucible is placed in institute The top of powder collecting region is stated, the crucible is equipped with the drive rod being connected with the piezoelectric ceramics that the hull outside is arranged in, Against the centre bore of the crucible bottom, the centre bore bottom is equipped with narrow meshed gasket for the lower end of the drive rod;It is described It is equipped with thermocouple inside crucible, is equipped with ring resistance heater outside the crucible;
The shell is equipped with the crucible air inlet pipe that is inserted into the crucible, is additionally provided on the side wall of the shell and institute The mechanical pump and diffusion pump that crucible is connected are stated, is additionally provided with cavity air inlet and cavity exhaust 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 drop 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 metal pow der 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;That is blow vent axial location that turntable is set.
The periphery of the turntable is additionally provided with load coil.
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.
The volume of the shell wants enough drops to fly after centrifugal breaking the range dropped in the catch tray of bottom, energy Enough to guarantee to solidify on the inner wall of the housing, the area of catch tray will guarantee sufficiently large can collect powder.
Further, the center-hole diameter of the crucible bottom is greater than the hole diameter of narrow meshed gasket, the band The pore diameter range of the gasket of aperture is between 0.02mm-2.0mm.
Further, the material of the narrow meshed gasket and the angle of wetting for the melt being placed in the crucible are greater than 90 °.
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 loop type resistance heater, the gasket, the turntable and the load coil are located on same axis.Purpose It is that can preferably be sprawled under the influence of centrifugal force and atomization plane in order to which drop can be dropped in center of turntable position.
Low melting point spherical metal is efficiently prepared by drop centrifugal atomization using above-mentioned device the invention discloses a kind of The method of powder, it is characterised in that include the following steps,
1. charging: after raw material welding wire is cut preset average length, being packed into the crucible of setting in the upper housing, hand In dynamic adjustment short transverse, load coil position to turntable is seal casinghousing after pre-determined distance;
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, makes pressure in shell reach preset value;
3. resistance heating: the heating parameters of ring resistance heater are used according to the setting of the fusing point of raw material to be heated, and By the temperature in crucible described in the thermocouple real-time monitoring that is arranged in the crucible, kept 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;
5. prepared by powder: firstly, manually adjusting the position of drive rod to being default between drive rod and narrow meshed gasket Distance;Secondly, high-purity inertia is protected by the way that the crucible air inlet pipe on the housing and being inserted into the crucible is arranged Gas is passed through, and makes the crucible is inside and outside to form positive pressure difference, melt is promoted to fill up the centre bore of the crucible bottom;Finally, giving Piezoelectric ceramics inputs the pulse signal of certain wave mode, and the piezoelectric ceramics is generated to bottom offset, by being connected with the piezoelectric ceramics Drive rod pass to the melt of centre bore near zone so that melt sprays to be formed from the narrow meshed gasket in center bottom hole portion Symmetrical liquid drop;
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 drive rod being restPosed.
6. particle collection: collecting metal powder with the catch tray for being set to the housing bottom.
Further, the average length of the raw material is 3mm-10mm, and the raw material amount of being put into is the crucible volume 1/4-3/4。
Further, it is 1-2mm higher than turntable to manually adjust load coil position.
Further, the induction heating voltage range of the load coil is 0-50V, and the induction heating time is 5- 15min。
Further, the high-purity inert protective gas is argon gas or helium, which is filled in shell, is made described Pressure after vacuumizing in shell reaches 0.1MPa, and metal material is completely melt that rear soaking time is 15-20 minutes;The crucible It is 0-200kPa with the differential pressure generated in the shell.
Compared with prior art, the invention has the following advantages:
The present invention, which devises a kind of pulse micropore gunite and combines with centrifugal atomization, makes molten drop in threadiness point The device that superfine metal spherical powder is efficiently prepared under mode is split, molten metal material is in differential pressure and pulse-type disturbance in crucible It under effect, is sprayed by the aperture of crucible bottom, forms symmetrical liquid drop, drop drops on high-speed rotating turntable, due to sense The effect that should be heated, also in molten condition when symmetrical liquid drop reaches disk upper surface, due to drop metal and disk upper surface Material has preferable wetability, and drop metal can spread over atomization surface without being ejected, under the influence of centrifugal force, completely Even drop can be sprawled on turntable in threadiness, and more small drop is separated into disk edge, sprawl along threadiness Track flies out, and the microlayer model to fly out, which is freely landed to solidify, forms metal powder.The gold of traditional pulse micropore gunite production It is controllable to belong to particle diameter, but single hole prepares the underproducing to meet increasing demand amount of particle.The present invention is micro- by pulse Hole gunite is combined with centrifugal atomization, while carrying out structure design to rotating circular disk, and it is good with metal material wetability to select Material as atomization plane, and increase induction heating apparatus, molten metal made to realize fibrous divisional mode, this point The mode of splitting efficiently reduces the diameter of atomization gained powder, and greatly improves the productivity of metal powder, therefore, passes through The combination of two methods, obtained metal powder partial size is tiny, particle diameter distribution section is narrow, sphericity is high, particle diameter distribution is controllable, heat Resume are consistent, and fine powder recovery rate is high, meet industrial requirement.
Process controllability of the invention is strong, shows following several points: being accurately controlled by ring resistance heater The heating temperature of crucible can control crucible and the intracorporal pressure difference of shell by being passed through inert gas into crucible and shell;Crucible The size of the aperture of the narrow meshed gasket in bottom can control the size of symmetrical liquid drop;Load coil can control turntable sheet The temperature in face, prevent turntable because caused by high speed rotation surface temperature reduce, solidify molten metal in advance;The revolving speed of turntable Controllably, it can control the fibrous splitting effect of molten metal, so as to further control the particle diameter distribution of metal microparticle; Adjustable and controllable, the globular metallic powder of the available particle size for meeting different requirements and distribution of technological parameter, And high production efficiency.
The present invention can efficiently prepare the metal powder for meeting 3D printing requirement by the threadiness division of molten metal, Size tunable, partial size are tiny, particle diameter distribution section is narrow, and sphericity is high, without satellite droplet, mobility and spreadability is good, hot resume Unanimously, production efficiency is very high, and production cost is low, can be used for industrial 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, drive rod;3, melt;4, crucible;5, ring resistance heater;6, narrow meshed pad Piece;7, cavity;8, turntable;9, motor;10, metal powder;11, catch tray;12, shell;13, load coil;14, liquid Drop;15, cavity air inlet pipe;16, mechanical pump;17, diffusion pump;18, cavity exhaust valve;19, crucible chamber;20, crucible air inlet pipe; 21, carrier;22, support portion;23, it is atomized plane;24, 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.
Low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization as shown in Figure 1, the present invention provides one kind Device, including shell 12, the crucible 4 and powder collecting region that are set in the shell 12, the powder collecting region is placed in institute The bottom of shell 12 is stated, the crucible 4 is placed in the top of the powder collecting region, and the crucible 4 is equipped with and is arranged described The connected drive rod 2 of piezoelectric ceramics 1 outside shell 12, the center of the lower end of the drive rod 2 against 4 bottom of crucible Hole, the centre bore bottom are equipped with narrow meshed gasket 6;It is equipped with thermocouple inside the crucible 4, is equipped with outside the crucible 4 Ring resistance heater 5;The center-hole diameter of 4 bottom of crucible is greater than the hole diameter of narrow meshed gasket 6, the band The pore diameter range of the gasket 6 of aperture is between 0.02mm-2.0mm.It the material of the narrow meshed gasket 6 and is placed in described The angle of wetting of melt 3 in crucible is greater than 90 °.
The shell 12 is equipped with the crucible air inlet pipe 20 being inserted into the crucible 4, goes back on the side wall of the shell 12 Equipped with the mechanical pump 16 and diffusion pump 17 being connected with the crucible 4, cavity air inlet 15 and chamber are additionally provided on the shell 12 Body exhaust valve 18;
The powder collecting region includes that the catch tray 11 of the housing bottom is arranged in and is set on the catch tray 11 The turntable 8 for atomized metal pow der drop 14 of side being connected with motor 9;
As shown in Fig. 2, the turntable 8 includes matrix, described matrix is by the carrier 21 on top and the support portion 22 of lower part The longitudinal section of composition be in class " T-type " main structure, 21 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 23, be disc structure, the disk and the circular groove match and with the circular groove mistake It is full of cooperation, the atomization plane 23 with material of 14 angle of wetting of atomized metal pow der drop less than 90 ° using being made;
Venthole 24, perforation are arranged in the carrier 21 and the support portion 22, the upper surface of the venthole 24 With the lower end face contact of the atomization plane 23, the lower end of the venthole 24 is in communication with the outside;
Preferably, the height of matrix is 10-20mm, and the height of support portion 22 should not be too high, less than the height of carrier 21 It is advisable.The upper surface of the atomization plane 23 protrudes from 21 upper surface of carrier, and protrusion range is 0.1-0.5mm.Protrusion As long as height, which meets, does not contact matrix conducive to discrete molten melt drop 14, directly flies in chamber and fall into catch tray.Institute The diameter range of carrier 21 is stated in 10-100mm, the diameter range of the circular groove is in 5-90mm.
The volume of the shell 12 wants enough molten melt drops 14 to fly after centrifugal breaking and drops to the catch tray 11 of bottom Interior range can guarantee be set on the inner wall of shell 12, and the area of catch tray 11 will guarantee sufficiently large can collect Metal powder 10.
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.It is flat that the upper surface of the venthole 24 is less than or equal to the atomization The lower end surface in face 23, the purpose that venthole 24 is arranged are to take out the gas of 8 internal clearance of turntable more when vacuumizing Completely, safer when 8 high speed rotation of turntable, therefore the contact surface of the upper surface of venthole 24 and the lower end surface of atomization plane 23 The stability of atomization plane 23 is better when product vacuumizes more greatly.
The periphery of the turntable 8 is additionally provided with load coil 13.The revolving speed of the turntable 8 is 10000rpm- 50000rpm.The heating thickness range of the load coil 13 is between 5-20mm, it and setting are outside the shell 12 Frequency converter be connected with regulated power supply, the control reference voltage of the regulated power supply is between 0-50V.
On the top-down direction of described device, the piezoelectric ceramics 1, the drive rod 2, the crucible 4, the ring Form resistance heater 5, the gasket 6, the turntable 8 and the load coil 13 are located on same axis.Purpose It is that can preferably be sprawled under the influence of centrifugal force and atomization plane in order to which drop can be dropped in center of turntable position.
When work, mechanical pump 16 and diffusion pump 17 are for vacuumizing shell 12 and crucible 4;4 bottom of crucible is equipped with small The gasket 6 in hole heats the raw material for needing preparation in crucible 4 using ring resistance heater 5, and passes through crucible air inlet pipe 20 and cavity air inlet pipe 15 be passed through high-purity inert protective gas into crucible 4 and shell 12, such as helium, argon gas, make 4 He of crucible Certain positive pressure difference is kept between shell 12, under the collective effect of piezoelectric ceramics 1 and positive pressure difference, molten melt drop 14 is in band The gasket 6 of aperture nearby generates;The molten melt drop 14 that narrow meshed gasket 6 nearby generates freely drops to high-speed rotating turntable On 8, the load coil 13 of 8 periphery of turntable makes the upper surface temperature of turntable 8 be maintained at the molten of metal material to be prepared Or more, the molten homogeneous drop 14 under molten condition freely drops to the center of turntable 8, since centrifugal force is smaller at this time, liquid Drop 14 will not be gone out by once discrete, but rounded can spread on turntable 8, and when spreading into, a certain range centrifugal force is sufficiently large When, the metal sprawled can be linear discrete to 8 edge of turntable in fiber on turntable 8 under the influence of centrifugal force, finally splits into Small drop flies out, and microlayer model solidifies in dropping process without container, forms metal powder 10, drop on catch tray 11, Drive rod 2 is restPosed simultaneously.
The spherical gold of low melting point is efficiently prepared by drop centrifugal atomization using above-mentioned device the invention also discloses a kind of The method for belonging to powder, includes the following steps,
1. charging: raw material welding wire is cut into the segment of 2-10mm, is packed into and is arranged in the crucible 4 in portion on housing 12, hand In dynamic adjustment short transverse, seal casinghousing 12 after 13 position of load coil is 1-2mm higher than turntable 8;
2. vacuumizing: being vacuumized using mechanical pump 16 and diffusion pump 17 to the crucible 4 and the shell 12, and be filled with height Purity inert protective gas argon gas makes pressure in shell 12 reach 0.1MPa;
3. resistance heating: the heating temperature of setting ring resistance heater 5 is 220-300 DEG C, heating speed 10-30 DEG C/min, and the temperature in crucible 4 described in the thermocouple real-time monitoring by being arranged in the crucible 4, it is complete to metal material 10-20 minutes are kept the temperature after fusing;
4. induction heating: making the turntable 8 high speed rotation under preset rotation speed using motor 9, then use induction heating High-speed rotating 8 surface of turntable is heated to the melting temperature of metal material or more by coil 13, and turntable is edge copper stainless steel disk, Revolving speed is 10000rpm-50000rpm, and induction heating voltage range is 0-50V, and the induction heating time is 5-15min;
5. prepared by powder: manually adjusting the position of drive rod 2, make drive rod 2 and narrow meshed gasket 6 at a distance of 2-5mm, lead to The crucible air inlet pipe 20 for being arranged in and on the shell 12 and being inserted into the crucible is crossed to be passed through high-purity inert protective gas, Make the positive differential pressure for generating 0-200kPa in crucible 4 and the shell 12, melt 3 is promoted to fill up the centre bore of 4 bottom of crucible; The pulse signal that certain wave mode is inputted to piezoelectric ceramics 1 generates piezoelectric ceramics 1 to bottom offset, by with 1 phase of piezoelectric ceramics Drive rod 2 even passes to the melt 3 of centre bore near zone, so that melt 3 is sprayed from the narrow meshed gasket 6 in center bottom hole portion Symmetrical liquid drop 14 is formed out;
Symmetrical liquid drop 14 freely drops on high-speed rotating turntable 8, and the symmetrical liquid drop 14 under molten condition is in centrifugal force Under the action of, it can be sprawled on turntable 8 in threadiness, split into small drop and fly out, microlayer model is in dropping process without appearance Device solidification, forms metal powder 10, drop on catch tray 11.
6. particle collection: collecting metal powder 10 with the catch tray 11 for being set to 12 bottom of shell.
Embodiment 1
Batch prepares the specific embodiment of Sn63Pb37 alloy spherical powder:
Sn63Pb37 welding wire is cut into the segment of 5mm or so, is put into crucible 4 after carrying out ultrasonic vibration cleaning, is selected small Bore dia is that the gasket 6 of 350mm is placed on the bottom of crucible 4, and the amount of being put into of Sn63Pb37 raw material reaches the 3/ of 4 capacity of crucible 4, ring resistance heater 5 is installed on crucible 4, thermocouple is inserted into 4 bottom of crucible;The edge copper stainless steel of choice experiment turns Disk 8 is installed on motor 9, in 8 periphery installation load coil 13 of turntable, so that 13 position of load coil is than turntable 8 The high 1mm of disk, rear seal casinghousing 12;
Shell 12, crucible 4 are extracted into low vacuum 5Pa hereinafter, recycling diffusion pump 17 by shell 12, earthenware using mechanical pump 16 Crucible 4 is extracted into high vacuum 0.001Pa;It is passed through high-purity inert protective gas argon gas using crucible air inlet pipe 20, cavity air inlet pipe 15, Shell 12, the pressure in crucible 4 is set to reach 0.1MPa;
Crucible 4 is heated using ring resistance heater 5, heating temperature be 300 DEG C, heating speed be 15 DEG C/ Min keeps the temperature 10min, the metal material in crucible 4 is made all to be fused into melt 3;
Make the 8 revolving speed 24000r/min of turntable using motor 9, the induction heating of load coil 13 is then set Voltage is 21V, and induction heating current 8A, the induction heating time is 10min, and high-speed rotating 8 surface of turntable is heated to gold Belong to 183 DEG C of melting temperature or more of material;
The position for manually adjusting drive rod 2 makes drive rod 2 and narrow meshed gasket 6 at a distance of 2-5mm, then passes through setting On the shell 12 and high-purity inert protective gas argon gas is passed through by the crucible air inlet pipe 20 that is inserted into the crucible, is made The positive differential pressure that 50kPa is generated in crucible 4 and the shell 12, promotes molten metal 3 to fill up the centre bore of 4 bottom of crucible; The pulse signal of trapezoidal wave is inputted to piezoelectric ceramics 1, and it is 100Hz that frequency, which is arranged, generates piezoelectric ceramics 1 to bottom offset, by The drive rod 2 being connected with the piezoelectric ceramics 1 passes to the molten metal 3 of centre bore near zone, so that molten metal 3 is therefrom The ejection of narrow meshed gasket 6 of heart hole bottom forms symmetrical liquid drop 14;Symmetrical liquid drop 14 freely drops to high-speed rotating turntable 8 On, the symmetrical liquid drop 14 under molten condition under the influence of centrifugal force, can be sprawled in threadiness on turntable 8, be split into small Drop fly out, microlayer model in dropping process without container solidify, formed metal powder 10, drop on catch tray 11;
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 9, so that turntable 8 stops rotating;Ring resistance heater 5 and load coil 13 are closed, is down to room temperature to temperature, Take out the metal powder 10 in catch tray 11;Cavity air inlet pipe 15 and crucible air inlet pipe 20 are finally closed, with mechanical pump 16 by earthenware Crucible 4 and shell 12 are extracted into low vacuum 5Pa hereinafter, to make equipment when deactivated in vacuum 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) is The powder being prepared by means of the present invention, powder diameter have obtained apparent miniaturization, and granule size, which meets use, to be wanted It asks, and sphericity is got higher, powder surface topography also improves, and generates without hemisphere.
As shown in figure 4, the atomizing disk obtained after (b) being atomized for the prior art, due to being atomized the metal of disk material and preparation Dusty material wetability is too small, and too low in atomization process turntable temperature, causes liquid in membranaceous division, and atomization surface meeting There is thicker solidification liquid film, the liquid film surface is very coarse, is unfavorable for the further atomization of subsequent metal drop, can be serious Influence atomizing effect and nebulization efficiency.(a) atomization surface to obtain by the method for the invention, it can be seen that spray patterns transformation For 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.
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 (10)

1. a kind of device for efficiently preparing low melting point globular metallic powder by drop centrifugal atomization, including shell (12), setting In crucible (4) and powder collecting region in the shell (12), the powder collecting region is placed in the bottom of the shell (12), institute The top that crucible (4) is placed in the powder collecting region is stated, the crucible (4) is equipped with setting in the shell (12) outside The connected drive rod (2) of piezoelectric ceramics (1), centre bore of the lower end of the drive rod (2) against the crucible (4) bottom, institute Centre bore bottom is stated equipped with narrow meshed gasket (6);It is equipped with thermocouple inside the crucible (4), is equipped with outside the crucible (4) Ring resistance heater (5);
The shell (12) is equipped with the crucible air inlet pipe (20) being inserted into the crucible (4), the side wall of the shell (12) On be additionally provided with the mechanical pump (16) and diffusion pump (17) being connected with the crucible (4), be additionally provided with cavity on the shell (12) Air inlet (15) and cavity exhaust valve (18);
The powder collecting region includes that the catch tray (11) of the housing bottom is arranged in and is set on the catch tray (11) The turntable (8) for atomized metal pow der drop (14) of side being connected with motor (9);It is characterized by:
The turntable (8) includes matrix, and described matrix is made of vertical the support portion (22) of the carrier (21) on top and lower part Section is in the main structure of class " T-type ", carrier (21) 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 (23), be disc structure, the disk and the circular groove match and with the circular groove interference Cooperation, the atomization plane (23) use and are made with material of atomized metal pow der drop (14) angle of wetting less than 90 °;
Venthole (24), perforation setting in the carrier (21) and the support portion (22), the venthole (24) it is upper The lower end face contact of end face and atomization plane (23), the lower end of the venthole (24) is in communication with the outside;
The periphery of the turntable (8) is additionally provided with load coil (13).
2. the device according to claim 1 that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization, It is characterized in that, the center-hole diameter of crucible (4) bottom is greater than the hole diameter of narrow meshed gasket (6), and the band is small The pore diameter range of the gasket (6) in hole is between 0.02mm-2.0mm.
3. the device according to claim 1 that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization, It is characterized in that, the material of the narrow meshed gasket (6) and the angle of wetting for the melt (3) being placed in the crucible are greater than 90 °.
4. the device according to claim 1 that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization, It is characterized in that, the revolving speed of the turntable (8) is 10000rpm-50000rpm.
5. the device according to claim 1 that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization, It is characterized in that, the heating thickness range of the load coil (13) is between 5-20mm, it and setting are in the shell (12) frequency converter outside is connected with regulated power supply, and the control reference voltage of the regulated power supply is between 0-50V.
6. the device according to claim 1 that low melting point globular metallic powder is efficiently prepared by drop centrifugal atomization, It is characterized in that, on the top-down direction of described device, the piezoelectric ceramics (1), the drive rod (2), the crucible (4), the loop type resistance heater (5), the gasket (6), the turntable (8) and the load coil (13) position In on same axis.
7. a kind of device using as described in claim 1-6 any one claim is efficiently prepared by drop centrifugal atomization The method of low melting point globular metallic powder, it is characterised in that include the following steps,
1. charging: after raw material welding wire is cut preset average length, being packed into setting in the crucible (4) on shell (12) top It is interior, it manually adjusts in short transverse, load coil (13) position to turntable (8) is seal casinghousing (12) after pre-determined distance;
2. vacuumizing: being vacuumized, and filled to the crucible (4) and the shell (12) using mechanical pump (16) and diffusion pump (17) Enter high-purity inert protective gas, shell (12) interior pressure is made to reach preset value;
3. resistance heating: using the heating parameters of ring resistance heater (5) according to the setting of the fusing point of raw material to be heated, and lead to The temperature in crucible described in the thermocouple real-time monitoring being arranged in the crucible (4) is crossed, is kept the temperature after metal material is completely melt;
4. induction heating: making the turntable (8) high speed rotation under preset rotation speed using motor (9), followed by induction heating High-speed rotating turntable (8) upper surface is heated to the melting temperature of metal material or more by coil (13);
5. prepared by powder: firstly, the position for manually adjusting drive rod (2) is between drive rod (2) and narrow meshed gasket (6) Pre-determined distance;Secondly, will by the crucible air inlet pipe (20) for being arranged on the shell (12) and being inserted into the crucible (4) High-purity inert protective gas is passed through, and makes the crucible (4) is inside and outside to form positive pressure difference, melt (3) is promoted to fill up the crucible (4) centre bore of bottom;Finally, inputting the pulse signal of certain wave mode to piezoelectric ceramics (1), the piezoelectric ceramics (1) is generated To bottom offset, the melt (3) of centre bore near zone is passed to by the drive rod (2) being connected with the piezoelectric ceramics (1), so that Melt (3) forms symmetrical liquid drop (14) from the ejection of the narrow meshed gasket (6) in center bottom hole portion;
Symmetrical liquid drop (14) freely drops on high-speed rotating turntable (8), and the symmetrical liquid drop (14) under molten condition first drips At the center of turntable (8), since centrifugal force is smaller at this time, drop (14) will not be gone out by once discrete, but can rounded paving Exhibition on turntable (8), 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 (8) edge in fiber on turntable (8), it finally splits into small drop and flies out, microlayer model was falling It is solidified in journey without container, is formed metal powder (10), drop on catch tray (11), while drive rod (2) are restored into initial shape State.
6. particle collection: collecting metal powder (10) with the catch tray (11) for being set to the shell (12) bottom.
8. the method according to claim 7 for efficiently preparing low melting point globular metallic powder by drop centrifugal atomization, It is characterized in that, it is 1-2mm higher than turntable (8) to manually adjust load coil (13) position.
9. the method according to claim 7 for efficiently preparing low melting point globular metallic powder by drop centrifugal atomization, It is characterized in that, the induction heating voltage range of the load coil (13) is 0-50V, and the induction heating time is 5-15min.
10. the method according to claim 7 for efficiently preparing low melting point globular metallic powder by drop centrifugal atomization, It is characterized in that, the high-purity inert protective gas is argon gas or helium, which is filled in shell (12), the shell is made (12) pressure after vacuumizing in reaches 0.1MPa, and metal material is completely melt that rear soaking time is 15-20 minutes;The crucible It (4) is 0-200kPa with the differential pressure generated in the shell (12).
CN201811116484.0A 2018-09-25 2018-09-25 A kind of device and method efficiently preparing low melting point globular metallic powder by drop centrifugal atomization Pending CN109047785A (en)

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AU2019351409A AU2019351409A1 (en) 2018-09-25 2019-09-25 Droplet-by-droplet centrifugal atomization manner-based device and method for efficiently preparing low-melting-point spherical metal powders
PCT/CN2019/107697 WO2020063620A1 (en) 2018-09-25 2019-09-25 Droplet-by-droplet centrifugal atomization manner-based device and method for efficiently preparing low-melting-point spherical metal powders

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