CN109014227A - A kind of device and method preparing superfine spherical metal powder by drop centrifugal atomization - Google Patents

A kind of device and method preparing superfine spherical metal powder by drop centrifugal atomization Download PDF

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Publication number
CN109014227A
CN109014227A CN201811116483.6A CN201811116483A CN109014227A CN 109014227 A CN109014227 A CN 109014227A CN 201811116483 A CN201811116483 A CN 201811116483A CN 109014227 A CN109014227 A CN 109014227A
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China
Prior art keywords
crucible
drop
turntable
shell
metal powder
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CN201811116483.6A
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Chinese (zh)
Inventor
董伟
孟瑶
白兆丰
朱胜
王晓明
赵阳
许富民
王延洋
韩阳
李国斌
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 CN201811116483.6A priority Critical patent/CN109014227A/en
Publication of CN109014227A publication Critical patent/CN109014227A/en
Priority to PCT/CN2019/107703 priority patent/WO2020063625A1/en
Priority to AU2019351410A priority patent/AU2019351410A1/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

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention provides a kind of device and method that superfine spherical metal powder is prepared by drop centrifugal atomization, device includes shell, is set to the intracorporal crucible of shell and powder collecting region, it is characterized by: 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 discloses the methods by preparing superfine spherical metal powder by drop centrifugal atomization, mainly in combination with two methods of uniform droplet spray and centrifugal atomization, breach conventional metals schizotype, molten metal is set to show fibrous division, particle diameter distribution section is narrow, sphericity is high, good fluidity, spreadability are excellent and controllable, the superfine spherical metal powder without satellite droplet of uniform size so as to efficiently preparing, and is suitable for industrialized production.

Description

A kind of device and method preparing superfine spherical metal powder by drop centrifugal atomization
Technical field
The invention belongs to superfine spherical particulate preparation technical fields, specifically, more particularly to a kind of by drop centrifugation Atomization prepares the device and method of superfine spherical metal powder.
Background technique
Metal increases material manufacturing technology can process the part of various complicated shapes, therefore in energy since its molding range is wide The multiple fields such as source, military affairs are all widely applied.And globular metallic powder is as molding raw material, its quality for The quality of finished product has a great impact.Demand of the increases material manufacturing technology to metal powder includes that narrow particle size distribution, oxygen content be low, ball Shape degree height, average grain diameter are less than 50 μm and without performances such as satellite droplets.However the metal powder at present in China market is not of low quality, There is larger gap with foreign technology level, powder in the market is not met by the needs for increasing material technology, this is also seriously limited The development of China's increasing material technology.
The method for preparing globular metallic powder at present mainly has: atomization, including gas atomization, and water atomization is centrifuged mist Change method, rotating electrode atomized method etc..Although atomization milling efficiency is very high, the size distribution of prepared powder is big, It must can just obtain meeting the powder of Particle size requirements by repeatedly sieving, substantially reduce production efficiency, especially when size has sternly When lattice require;Atomization is also easy to produce satellite droplet, makes powder surfaces stick satellite droplet, reduces the mobility and spreadability of powder, and Magazine is easily mixed in production process, is unable to satisfy the requirement of 3D printing powder.
Therefore, how to prepare that particle diameter distribution is narrow and controllable, the high metal powder without satellite droplet of sphericity, which becomes, to be needed to be solved The big problem of one certainly.
Summary of the invention
Poor, spreadability and poor fluidity according to 3D printing set forth above sphericity present in metal powder preparation process Etc. technical problems, and provide a kind of device and method that superfine spherical metal powder is prepared by drop centrifugal atomization.The present invention Structure design is carried out mainly in combination with two methods of uniform droplet spray and centrifugal atomization, while to turntable, and increases induction Heating coil carries out induction heating to disc surfaces, so that molten metal be made to breach the schizotype of conventional melt metal, realizes The fibrous divisional mode being only just able to achieve when atomizing medium is aqueous solution or organic solution, can be with by this mode Realize metal powder micronization and big leap can be obtained in terms of granularity regulation, can be prepared sphericity height, There are good fluidity and spreadability, without satellite droplet, the very high spherical shape met using 3D printing requirement of fine powder recovery rate Metal powder.
The technological means that the present invention uses is as follows:
A kind of device preparing superfine spherical metal powder by drop centrifugal atomization, including shell, it is set to the shell Intracorporal crucible and powder collecting region, wherein the powder collecting region is placed in the bottom of the shell, and the crucible is placed in described The top of powder collecting region;
It is equipped with thermocouple inside the crucible, heating tape is equipped with outside the crucible, the crucible bottom is equipped with band aperture Nozzle, the clapp oscillator being connected with the piezoelectric ceramics that the case top is arranged in is equipped in the crucible;The crucible It is arranged right below electrode plate;
The shell is equipped with the crucible air inlet being inserted into the crucible, is additionally provided with diffusion pump and machine on the shell Tool pumps, and is additionally provided with cavity air inlet and cavity exhaust valve on the shell;
The powder collecting region include the catch tray that the housing bottom is set, be set to above the catch tray with The connected turntable for atomized metal pow der drop of 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 atomization metal 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.
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.
Preferably, the height in substrate support portion should not be too high, and the height less than carrier is advisable.It is described to be atomized the upper of plane End face protrudes from the carrier upper surface, and protrusion range is 0.1-0.5mm.As long as protrusion height, which meets, is conducive to discrete metal Drop does not contact matrix, directly flies in chamber and falls into catch tray.Described matrix uses zirconia ceramic, titanium dioxide Silica glass or stainless steel are made, and are not limited to above-mentioned several materials, 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 lower end surface of the atomization plane, and the purpose of venthole setting is to vacuumize When, can take out the gas of turntable internal clearance cleaner, and when turntable high speed rotation is safer, therefore the upper surface of venthole The stability of atomization plane is better when vacuumizing more greatly with the contact area of the lower end surface of atomization plane.
Further, the material of the crucible and the angle of wetting for the melt being placed in the crucible are greater than 90 °.
Further, the pore diameter range of the aperture of the nozzle is between 0.02mm-2.0mm.
Further, the voltage range of the electrode plate is between 100V-400V;The load coil and setting exist Frequency converter outside the shell is connected with regulated power supply, the heating thickness range of the load coil between 5-20mm, The control reference voltage of the regulated power supply is between 0-50V.
Further, the revolving speed of the turntable is 10000rpm-50000rpm.
Further, the piezoelectric ceramics, the clapp oscillator, described on the top-down direction of described device Crucible, the nozzle, the electrode plate, the turntable and the load coil are located on same axis.
It is used the invention also discloses a kind of above-mentioned device and prepares superfine spherical metal powder by drop centrifugal atomization Method, it is characterised in that include the following steps,
1. charging: raw material loading being arranged in the crucible of shell internal upper part, is manually adjusted in short transverse, induction adds Heat coil position to turntable is pre-determined distance, rear seal casinghousing;
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. heating crucible: using the heating parameters of heating tape according to the setting of the fusing point of raw material to be heated, and by described Temperature in crucible described in the thermocouple real-time monitoring being arranged in 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;
5. prepared by powder: by the way that the crucible air inlet pipe on the housing and being inserted into the crucible is arranged by high-purity Inert protective gas is passed through, and makes the crucible is inside and outside to form positive pressure difference;Then the pulse of certain wave mode is inputted to piezoelectric ceramics Signal, so that clapp oscillator generates the oscillation of certain frequency;Finally, the voltage of setting electrode plate, forms the electricity of preset strength ?;
Since, there are differential pressure, metal can flow out to form cylindrical metal stream from nozzle inside and outside crucible, certain frequency above at this time Under the oscillation of rate, cylindrical metal stream will be broken into a series of small molten drops, make during molten drop decline in electric field It, can be due to the skin effect of charge, so that mutually exclusive between each molten drop avoid polymerizeing again for molten drop under;
Molten drop freely drops on high-speed rotating turntable, is first dropped in the center of turntable, due to centrifugal force at this time Smaller, drop will not be gone out by once discrete, but rounded can spread on turntable, sufficient when spreading into a certain range centrifugal force When enough big, the metal sprawled can be linear discrete to disk edge in fiber on turntable under the influence of centrifugal force, finally divides It flies out at small drop, microlayer model solidifies in dropping process without container, forms metal powder, drop on catch tray;
6. particle collection: collecting metal powder with the catch tray for being set to the housing bottom.
Further, the raw material metal amount of being put into is the 1/4-3/4 of the crucible volume.
Further, it is 1-2mm higher than rotating circular disk to manually adjust induction coil position.
Further, the high-purity inert protective gas is argon gas or helium, which is filled in shell, shell is made Interior pressure reaches 0.1MPa, and metal material is completely melt that rear soaking time is 15-20 minutes.
Further, the induction heating voltage range of the load coil is 0-50V, and the induction heating time is 5- 15min。
Further, the crucible and the interior differential pressure generated of the shell are 0-200kPa.
Compared with the prior art, the invention has the following advantages that
The present invention devises one kind mainly in combination with two methods of uniform droplet spray and centrifugal atomization, makes molten drop The device of superfine metal spherical powder is prepared under fibrous schizotype, molten metal material is in differential pressure and oscillation in crucible It under the action of generator, is sprayed by the nozzle of crucible bottom, formation droplet, in droplet dropping process, in the work of electric field It will not polymerize under, drop drops on high-speed rotating turntable, and due to the effect of induction heating, symmetrical liquid drop is reached on turntable Also in molten condition when surface, since drop metal and disk upper surface material have preferable wetability, in the work of centrifugal force Under, symmetrical liquid drop can be sprawled on turntable in threadiness, and be separated into more small drop in disk edge and flown out, freely Landing solidification forms metal powder.The metallic size tunable of pulse micropore gunite production, but single hole prepares the production of particle Amount is insufficient for increasing demand amount.By innovation, pulse micropore gunite is combined with centrifugal atomization, simultaneously Structure design is carried out to turntable, is selected with the good material of metal material wetability as atomization surface, and increase induction heating Device, makes molten metal realize fibrous divisional mode, and this divisional mode efficiently reduces the straight of atomization gained powder Diameter, and greatly improve the productivity of metal powder, therefore, by the combination of two methods, obtained metal powder partial size It is tiny, particle diameter distribution section is narrow, sphericity is high, particle diameter distribution is controllable, hot resume are consistent, fine powder recovery rate is high, and it is raw to meet industry The requirement of production.
Process controllability of the invention is strong, shows following several points: accurately controlling adding for crucible by heating tape Hot temperature can control crucible and the intracorporal pressure difference of shell by being passed through inert gas into crucible and shell;Crucible bottom band is small The size of the nozzle in hole can control the size of symmetrical liquid drop;Electrode plate can control the size of electric field;Load coil can To control the temperature of disc surfaces, the revolving speed of rotating circular disk is controllable, can control the fibrous splitting effect of molten metal, thus The particle diameter distribution of metal microparticle can further be controlled;Adjustable and controllable, the available satisfaction difference of technological parameter It is required that particle size and distribution globular metallic powder, and high production efficiency.
To sum up, the present invention can efficiently prepare the metal for meeting 3D printing requirement by the threadiness division of molten metal Powder, size tunable, partial size are tiny, particle diameter distribution section is narrow, and sphericity is high, good without satellite droplet, mobility and spreadability, hot Resume are consistent, and 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 invention.
Fig. 3 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.
In figure: 1, piezoelectric ceramics;2, crucible;3, clapp oscillator;4, crucible air inlet pipe;5, melt;6, heating tape;7, electric Pole plate;8, turntable;9, metal powder;10, catch tray;11, motor;12, load coil;13, molten drop;14, nozzle; 15, cavity air inlet pipe;16, mechanical pump;17, diffusion pump;18, cavity exhaust valve;19, thermocouple;20, shell;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.
As shown in Figure 1, the present invention provides a kind of device for preparing superfine spherical metal powder by drop centrifugal atomization, Including shell 20, the crucible 2 and powder collecting region that are set in the shell 20, wherein the powder collecting region is placed in described The bottom of shell 20, the crucible 2 are placed in the top of the powder collecting region;
It is equipped with thermocouple 19 inside the crucible 2, is equipped with heating tape 6 outside the crucible 2,2 bottom of crucible is equipped with Narrow meshed nozzle 14, the material of the crucible 2 and the angle of wetting for the melt 5 being placed in the crucible are greater than 90 °.The nozzle The pore diameter range of 14 aperture is between 0.02mm-2.0mm.The pressure for being equipped in the crucible 2 and the case top being set The connected clapp oscillator 3 of electroceramics 1;The crucible is arranged right below electrode plate 7;The voltage range of the electrode plate 7 exists Between 100V-400V;
The shell 20 is equipped with the crucible air inlet 4 being inserted into the crucible 2, is additionally provided with diffusion on the shell 20 17 and mechanical pump 16 are pumped, is additionally provided with cavity air inlet 15 and cavity exhaust valve 18 on the shell 20;
The powder collecting region includes the catch tray 10 that 20 bottom of shell is arranged in, is set on the catch tray 10 The turntable 8 for atomized metal pow der drop of side being connected with motor 11;
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 13 angle of wetting of atomization metal 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;
The periphery of the turntable 8 is additionally provided with load coil 12.The revolving speed of the turntable 8 is 10000rpm- 50000rpm.The load coil 12 is connected with the frequency converter and regulated power supply being arranged in outside the shell 20, the sense Answer the heating thickness range of heating coil 12 between 5-20mm, 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 clapp oscillator 3, the crucible 2, institute Nozzle 14, the electrode plate 7, the turntable 8 and the load coil 12 is stated to be located on same axis.Purpose be in order to Drop can uniformly be dropped in center of turntable, conducive to sprawling.
The volume of the shell 20 wants enough drops to fly after centrifugal breaking the range dropped in the catch tray of bottom, It can guarantee be set on the inner wall of shell 20, the area of catch tray 10 will guarantee sufficiently large can collect powder.
When work, mechanical pump 16 and diffusion pump 17 are for vacuumizing shell 20 and crucible 2;2 bottom of crucible is equipped with small The nozzle 14 in hole heats the raw material for needing preparation in crucible 2 using heating tape 6, and passes through crucible air inlet pipe 4 and cavity Air inlet pipe 15 is passed through high-purity inert protective gas into crucible 2 and shell 20, such as helium, argon gas, make crucible 2 and shell 20 it Between keep certain positive pressure difference, the pulse signal of certain wave mode is then inputted to piezoelectric ceramics 1 so that clapp oscillator 3 produce The oscillation of raw certain frequency, finally, the voltage of setting electrode plate 7, forms a sizeable electric field.Inside and outside crucible 2 There are differential pressure, metal can be flowed out from nozzle 14 forms cylindrical metal stream, at this time above under the oscillation of certain frequency, cylindrical metal Stream will be broken into a series of small molten drops 13 can be due to charge during the decline of molten drop 13 under electric field action Skin effect so that mutually exclusive between each molten drop 13 avoid polymerizeing again for molten drop 13.Molten drop 13 It freely drops on high-speed rotating turntable 8, the molten drop 13 under molten condition is first dropped in the center of turntable 8, due to this When centrifugal force it is smaller, molten drop 13 will not be gone out by once discrete, but rounded can spread on turntable 8, when spreading into When a certain range centrifugal force is sufficiently large, the metal sprawled can be discrete extremely in fiber threadiness on turntable 8 under the influence of centrifugal force 8 edge of turntable finally splits into small drop and flies out, and microlayer model solidifies in dropping process without container, forms metal powder 9, it drop on catch tray 10.
It is used the invention also discloses a kind of above-mentioned device and prepares superfine spherical metal powder by drop centrifugal atomization Method, include the following steps,
1. charging: raw material loading being arranged in the crucible 2 of 20 internal upper part of shell, is manually adjusted in short transverse, is felt Answering 12 position of heating coil to turntable 8 is pre-determined distance, rear seal casinghousing 20;The raw material metal amount of being put into is the crucible The 1/4-3/4 of 2 volumes.
2. vacuumizing: being vacuumized using mechanical pump 16 and diffusion pump 17 to the crucible 2 and the shell 20, and be filled with height Purity inert protective gas makes pressure in shell 20 reach preset value;
3. heating crucible: using the heating parameters of heating tape 6 according to the setting of the fusing point of raw material to be heated, and by described Temperature in crucible 2 described in 19 real-time monitoring of thermocouple being arranged in crucible 2, keeps the temperature after metal material is completely melt;
4. induction heating: making the turntable 8 high speed rotation under preset rotation speed using motor 11, followed by induction heating High-speed rotating 8 upper surface of turntable is heated to the melting temperature of metal material or more by coil 12;The load coil 12 Induction heating voltage range be 0-50V, the induction heating time be 5-15min.
5. prepared by powder: by being arranged on the shell 20 and the crucible air inlet pipe 4 being inserted into the crucible 2 will be high Purity inert protective gas is passed through, and makes the crucible 2 is inside and outside to form positive pressure difference;The high-purity inert protective gas is argon gas Or helium, which is filled in shell 20, so that pressure in shell is reached 0.1MPa, metal material is completely melt rear soaking time It is 15-20 minutes.Then the pulse signal of certain wave mode is inputted to piezoelectric ceramics 1, so that clapp oscillator 3 generates certain frequency Oscillation;Finally, the voltage of setting electrode plate 7, forms the electric field of preset strength;
Cylindrical metal stream is formed since, there are differential pressure, metal can be flowed out from nozzle 14 inside and outside crucible 2, it is certain above at this time Under the oscillation of frequency, cylindrical metal stream will be broken into a series of small molten drops 13, molten drop 13 decline during It, can be due to the skin effect of charge, so that mutually exclusive between each molten drop 13 avoid molten drop under electric field action 13 again polymerize;
Molten drop 13 freely drops on high-speed rotating turntable 8, is first dropped in the center of turntable 8, due at this time from Mental and physical efforts are smaller, drop will not by once it is discrete go out, but can it is rounded spread on turntable 8, when spread into a certain range from When mental and physical efforts are sufficiently large, the metal sprawled can be linear discrete to 8 edge of turntable in fiber on turntable 8 under the influence of centrifugal force, It finally splits into small drop to fly out, microlayer model solidifies in dropping process without container, forms metal powder 9, drop to receipts On catch basin 10;
6. particle collection: collecting metal powder 9 with the catch tray 10 for being set to the housing bottom.
Embodiment 1
Batch prepares the specific embodiment of Sn63Pb37 alloy spherical powder:
It is put into crucible 2 after Sn63Pb37 raw material are carried out ultrasonic vibration cleaning, the amount of being put into of Sn63Pb37 raw material Reach the 3/4 of 2 capacity of crucible, heating tape 6 is installed on crucible 2, is inserted into thermocouple inside crucible 2;Choice experiment turns Disk 8 is installed on motor 11, in 8 periphery installation load coil 12 of turntable, so that 12 position of load coil is than turntable 8 The high 1mm of disk, rear seal casinghousing 20;
Shell 20, crucible 2 are extracted into low vacuum 5Pa hereinafter, recycling diffusion pump 17 by shell 20, earthenware using mechanical pump 16 Crucible 2 is extracted into high vacuum 0.001Pa;It is passed through high-purity inert protective gas argon gas using crucible air inlet pipe 4, cavity air inlet pipe 15, Shell 20, the pressure in crucible 2 is set to reach 0.1MPa;
Crucible 2 is heated using heating tape 6, heating temperature is 300 DEG C, and heating speed is 15 DEG C/min, heat preservation 10min makes the metal material in crucible 2 all be fused into melt 5;
Make the 8 revolving speed 24000r/min of turntable using motor 11, the induction that load coil 12 is then arranged adds Thermal 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 183 DEG C of melting temperature or more of metal material;
The voltage that electrode plate is arranged is 300V, then by the crucible air inlet pipe 4 that is arranged in the crucible 2 by high-purity Inert protective gas argon gas is passed through, and makes the positive differential pressure that 50kPa is generated in crucible 2 and the shell 20;Ladder is inputted to piezoelectric ceramics 1 The pulse signal of shape wave, and it is 1MHZ that frequency, which is arranged, so that piezoelectric ceramics 1 is generated concussion up and down, by being connected with the piezoelectric ceramics 1 Clapp oscillator 3 pass to the melt 5 of 14 near zone of nozzle so that melt 5 sprayed from narrow meshed nozzle 14 formed it is equal Even molten drop 13;Homogeneous metal drop 13 freely drops on high-speed rotating turntable 8, the homogeneous metal liquid under molten condition Drop 13 under the influence of centrifugal force, can be sprawled in threadiness on turntable 8, split into small drop and fly out, microlayer model be under It is solidified during falling without container, forms metal powder 9, drop on catch tray 10;
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 11, so that turntable 8 stops rotating;Heating tape 6 and load coil 12 are closed, room temperature is down to temperature, takes out and receive Metal powder 9 in catch basin 10;Cavity air inlet pipe 15 and crucible air inlet pipe 4 are finally closed, with mechanical pump 16 by crucible 2 and shell 20 are extracted into low vacuum 5Pa hereinafter, to make equipment when deactivated in vacuum state.
As shown in figure 3, 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.
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 preparing superfine spherical metal powder by drop centrifugal atomization, including shell (20), be set to it is described Crucible (2) and powder collecting region in shell (20), wherein the powder collecting region is placed in the bottom of the shell (20), institute State the top that crucible (2) is placed in the powder collecting region;
Thermocouple (19) are equipped with inside the crucible (2), are equipped with heating tape (6) outside the crucible (2), crucible (2) bottom Portion is equipped with narrow meshed nozzle (14), is equipped in the crucible (2) and is connected with the piezoelectric ceramics (1) that the case top is arranged in Clapp oscillator (3);The crucible is arranged right below electrode plate (7);
The shell (20) is equipped with the crucible air inlet (4) being inserted into the crucible (2), is additionally provided on the shell (20) Diffusion pump (17) and mechanical pump (16) are additionally provided with cavity air inlet (15) and cavity exhaust valve (18) on the shell (20);
The powder collecting region include setting the shell (20) bottom catch tray (10), be set to the catch tray (10) The turntable (8) for atomized metal pow der drop of top being connected with motor (11);
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 atomization metal drop (13) 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 (12).
2. the device according to claim 1 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the material of the crucible (2) and the angle of wetting for the melt (5) being placed in the crucible are greater than 90 °.
3. the device according to claim 1 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the pore diameter range of the aperture of the nozzle (14) is between 0.02mm-2.0mm.
4. the device according to claim 1 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the voltage range of the electrode plate (7) is between 100V-400V;The load coil (12) and setting are in the shell The frequency converter of body (20) outside is connected with regulated power supply, the heating thickness range of the load coil (12) 5-20mm it Between, the control reference voltage of the regulated power supply is between 0-50V.
5. the device according to claim 1 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the revolving speed of the turntable (8) is 10000rpm-50000rpm.
6. the device according to claim 1 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In, on the top-down direction of described device, the piezoelectric ceramics (1), the clapp oscillator (3), the crucible (2), The nozzle (14), the electrode plate (7), the turntable (8) and the load coil (12) are located on same axis.
7. device described in a kind of claim 1-6 any one claim, which is used, prepares ultra-fine ball by drop centrifugal atomization The method of shape metal powder, it is characterised in that include the following steps,
1. charging: raw material being packed into setting in the crucible (2) of shell (20) internal upper part, manually adjusts in short transverse, feels Answering heating coil (12) position to turntable (8) is pre-determined distance, rear seal casinghousing (20);
2. vacuumizing: being vacuumized, and filled to the crucible (2) and the shell (20) using mechanical pump (16) and diffusion pump (17) Enter high-purity inert protective gas, shell (20) interior pressure is made to reach preset value;
3. heating crucible: using the heating parameters of heating tape (6) according to the setting of the fusing point of raw material to be heated, and pass through the earthenware Temperature in crucible (2) described in thermocouple (19) real-time monitoring being arranged in crucible (2), keeps the temperature after metal material is completely melt;
4. induction heating: making the turntable (8) high speed rotation under preset rotation speed using motor (11), followed by induction heating High-speed rotating turntable (8) upper surface is heated to the melting temperature of metal material or more by coil (12);
5. prepared by powder: will by the crucible air inlet pipe (4) for being arranged on the shell (20) and being inserted into the crucible (2) High-purity inert protective gas is passed through, and makes the crucible (2) is inside and outside to form positive pressure difference;Then to piezoelectric ceramics (1) input one The pulse signal of standing wave type, so that clapp oscillator (3) generates the oscillation of certain frequency;Finally, the electricity of setting electrode plate (7) Pressure, forms the electric field of preset strength;
Since crucible (2) is inside and outside there are differential pressure, metal can be flowed out from nozzle (14) forms cylindrical metal stream, certain above at this time Under the oscillation of frequency, cylindrical metal stream will be broken into a series of small molten drops (13), and molten drop (13) declines process In under electric field action, can due to charge skin effect so that mutually exclusive between each molten drop (13) avoid gold Belong to polymerizeing again for drop (13);
Molten drop (13) freely drops on high-speed rotating turntable (8), the center of turntable (8) is first dropped in, due at this time Centrifugal force is smaller, and drop will not be gone out by once discrete, but rounded can spread on turntable (8), when spreading into certain model Enclose centrifugal force it is sufficiently large when, the metal sprawled can be linear discrete to turntable in fiber on turntable (8) under the influence of centrifugal force (8) edge finally splits into small drop and flies out, and microlayer model solidifies in dropping process without container, forms metal powder (9), it drop on catch tray (10);
6. particle collection: collecting metal powder (9) with the catch tray (10) for being set to the housing bottom.
8. the method according to claim 7 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the raw material metal amount of being put into is the 1/4-3/4 of the crucible (2) volume.
9. the method according to claim 7 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the high-purity inert protective gas is argon gas or helium, which is filled in shell (20), pressure in shell is reached 0.1MPa, metal material are completely melt that rear soaking time is 15-20 minutes.
10. the method according to claim 7 for preparing superfine spherical metal powder by drop centrifugal atomization, feature exist In the induction heating voltage range of the load coil (12) is 0-50V, and the induction heating time is 5-15min.
CN201811116483.6A 2018-09-25 2018-09-25 A kind of device and method preparing superfine spherical metal powder by drop centrifugal atomization Pending CN109014227A (en)

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PCT/CN2019/107703 WO2020063625A1 (en) 2018-09-25 2019-09-25 Device and method for preparing ultrafine spherical metal powder using drop-by-drop centrifugal atomization method
AU2019351410A AU2019351410A1 (en) 2018-09-25 2019-09-25 Device and method for preparing ultrafine spherical metal powder using drop-by-drop centrifugal atomization method

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Application publication date: 20181218