CN116408208A - Centrifugal liquid phase forming device and method for preparing ultra-micro tin-base alloy welding powder - Google Patents
Centrifugal liquid phase forming device and method for preparing ultra-micro tin-base alloy welding powder Download PDFInfo
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- CN116408208A CN116408208A CN202210789219.9A CN202210789219A CN116408208A CN 116408208 A CN116408208 A CN 116408208A CN 202210789219 A CN202210789219 A CN 202210789219A CN 116408208 A CN116408208 A CN 116408208A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B1/00—Centrifuges with rotary bowls provided with solid jackets for separating predominantly liquid mixtures with or without solid particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B13/00—Control arrangements specially designed for centrifuges; Programme control of centrifuges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
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- B04B15/06—Other accessories for centrifuges for cleaning bowls, filters, sieves, inserts, or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B7/00—Elements of centrifuges
- B04B7/02—Casings; Lids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The centrifugal liquid phase forming device and method for preparing the ultra-micro tin-base alloy welding powder comprises a primary centrifugal device, a condensing device and a secondary centrifugal device; the primary centrifugal device comprises a centrifugal cup and an outer cup; the centrifugal cup rotates, and the outer cup is fixed; the wall of the centrifugal cup is provided with a centrifugal cup through hole for flowing out the mixed solution; the cup wall of the outer cup is provided with an outer cup rectangular hole; the rectangular hole of the outer cup is communicated with the condensing device; the condensing device is communicated with the secondary centrifugal device. Injecting the mixed solution of the molten liquid alloy and the medium oil into a centrifugal cup for centrifugal mixing; the mixed solution tiny liquid drops centrifuged out from the rectangular holes of the outer circular cup enter a condensing device for cooling; and (3) feeding the cooled mixed solution of the alloy powder and the medium oil into a secondary centrifugal device, and performing centrifugal separation on the alloy powder and the medium oil. The whole process is in medium oil, and is simple, convenient and efficient; and avoid the collision of alloy particles in the forming process, and well maintain the shape and the size of the alloy particles.
Description
Technical Field
The application relates to the technical field of electronic element welding material preparation methods and devices, in particular to preparation of metal powder, and especially relates to a centrifugal liquid phase forming device and method for manufacturing ultra-micro tin-base alloy welding powder.
Background
Along with the development of technology, the 5G communication artificial intelligence era comes, and microelectronic and semiconductor packaging technologies are widely applied in the fields of photoelectric display, intelligent wearable equipment and Internet of things equipment. Electronic components are moving toward miniaturization, the size of the chip is greatly reduced, but the requirements on the power, the power consumption and the reliability of the device are higher and higher, so that the requirements on the performance of packaging welding materials, such as smaller spacing, lower void ratio of welding spots, higher electrical reliability around the welding spots, short welding time, lower welding temperature and the like, are also more and more severe. Accordingly, the size of the package solder, which is one of the package materials for electronic connection, is becoming smaller and smaller, and the solder size is being developed from conventional T3, T4, T5 to finer solders, such as T6, T7, T8, and even later ultra-fine solders, such as T9, T10. Ultra-fine solders are typically applied in the form of solder paste, or anisotropic conductive paste in the solder material.
In the prior art, the main production methods of the low-melting-point alloy with the liquid phase temperature below 300 ℃ comprise an air atomization method, a centrifugal atomization method, an ultrasonic atomization method and an ultra-micro liquid phase forming process. The air atomization method and the centrifugal atomization method have the defects that the ultra-fine powder with finer grain diameter has low yield and cannot realize the accurate separation of the powder with the grain diameter of less than 15 mu m due to the limitation of the rotating speed of a motor, and the defects of poor sphericity, wide grain size distribution, small content of the particles with the grain diameter of less than 10 mu m, high oxygen content and the like are generated, so that the application performance of the ultra-fine welding powder is seriously influenced.
The patent publication No. CN102974834A, CN104439259A discloses a centrifugal preparation method of superfine spherical alloy welding powder, which comprises the steps of conveying molten alloy melt into an atomizer in an atomization bin by a liquid conveying pipe, atomizing the alloy melt into tiny liquid drops in an atomization chamber filled with inert gas, spheroidizing and cooling the liquid drops in the atomization chamber, and then carrying out a grading screening and packaging process. Although the patent can prepare T6-T8 ultrafine welding powder, the yield is low, the sphericity of tin powder is poor, tiny liquid drops thrown out by a centrifugal disc collide with each other in an atomization chamber, sticky belts and special-shaped particle powder can appear, and the surface damage of the tin powder is obvious in the screening process. The quality of tin powder seriously affects the application performance of the solder paste.
In the patent application with the publication number of CN113210620A, a preparation method and equipment of superfine low-oxygen tin powder are disclosed, a molten tin ingot is atomized in an air atomizing mode, and then the molten tin ingot is separated by an air flow machine to obtain superfine tin powder. The tin powder prepared by the method has poor sphericity and obvious sticky tape, and the tin powder collides and rubs in the sorting process, so that the tin powder is damaged, and the quality of the tin powder is affected.
The patent application with the publication number of CN101985177A discloses a liquid phase forming process, namely a production method of spherical low-melting metal powder, which comprises the steps of melting low-melting metal or alloy and mixing with hot oil, and the steps of preliminary dispersion by inert gas, high-power ultrasonic dispersion and emulsification, filtration and separation and the like, so that the defects are overcome, and the process is an advanced powder process with higher production efficiency, narrow product granularity distribution, low oxygen content and no sieving process, but with the expansion of the market scale of ultra-micro welding powder, a large amount of heat is generated in operation by a high-power ultrasonic device in the powder process, and high-efficiency continuous production cannot be realized in a high-temperature environment due to long-time load. The scheme can not meet the market demand, continuous production operation can not be realized, and the medium used in the production process can not be recycled, so that the waste of materials and the increase of loss are caused.
In the present specification, the specification of the particle size in the tin alloy powder or IPC J to STD to 005A to 2012 for soldering electronic products is adopted by the electronic industry standard SJ/T11391 to 2019; symbols T3 to T10 represent particle diameter range signals; the units are micrometers, i.e. μm;
the T3 type powder represents a range of particle diameters therein: 25-45 μm;
the T4 type powder represents a range of particle diameters therein: 20-38 mu m;
the T5 type powder represents a range of particle diameters therein: 15-25 μm;
the T6 type powder represents a range of particle diameters therein: 5-15 μm;
the T7 type powder represents a range of particle diameters therein: 2-11 mu m;
the T8 type powder represents a range of particle diameters therein: 2-8 μm;
the T9 type powder represents a range of particle diameters therein: 1-5 mu m;
the T10 type powder represents a range of particle diameters therein: 1 μm to 3 μm.
Disclosure of Invention
The technical scheme of the application overcomes the defects of low production efficiency, poor sphericity of products, uneven surface quality and incapability of continuous production of the ultra-micro tin-base alloy welding powder in the prior art, and provides a centrifugal liquid phase forming device method for preparing the ultra-micro tin-base alloy welding powder; can be continuously produced, and the excircle cup is skillfully arranged.
The technical scheme for solving the technical problems is that the centrifugal liquid phase forming device for preparing the ultra-micro tin-base alloy welding powder comprises a primary centrifugal device, a condensing device and a secondary centrifugal device; the primary centrifugal device comprises a centrifugal cup and an outer cup; both the centrifugal cup and the outer cup are hollow; the centrifugal cup is connected with the centrifugal motor M1 for centrifugal rotation, and the outer cup is fixed; the wall of the centrifugal cup is provided with a centrifugal cup through hole for centrifuging the mixed solution; the diameter of the outer cup is larger than that of the centrifugal cup, and the outer cup is sleeved on the periphery of the centrifugal cup; the cup wall of the outer cup is provided with an outer cup rectangular hole; the rectangular hole of the outer cup is communicated with the condensing device; the condensing device is communicated with the secondary centrifugal device.
The primary centrifugal device comprises a centrifugal cup and an outer circular cup which are coaxially arranged; the cross sections of the outer circular cup and the centrifugal cup have the same center; the diameter of the centrifugal cup ranges from 50 mm to 300 mm; the wall thickness of the centrifugal cup ranges from 1 mm to 5 mm; the diameter of the through hole of the centrifugal cup ranges from 0.02 mm to 0.5 mm.
The width of the rectangular hole of the outer circular cup ranges from 2 mm to 5 mm; the length of the rectangular hole of the outer cup ranges from 10 mm to 50 mm.
The outer cup rectangular hole formed in the cup wall of the outer cup comprises an outer cup rectangular hole A and an outer cup rectangular hole B; the center-to-center distance between the rectangular hole A of the outer cup and the rectangular hole B of the outer cup is 5 mm to 10 mm; the outer cup is provided with a heat preservation device which is used for keeping the temperature balance of the centrifugal cup and the outer cup.
The centrifugal motor M1 is a high-speed motor, and the motor rotation speed ranges from 1000rpm to 10000rpm.
The condensing device comprises a rectangular circular receiving pipe and a condensing pipe; the condensing pipe is used for cooling the alloy liquid drops in the mixed liquid into alloy powder; a pipe sleeve is arranged outside the condensing pipe, and cooling oil is arranged between the pipe sleeve and the outer wall of the condensing pipe; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid flowing out of the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is communicated with one end of the condensing pipe; the other end of the condensing tube is communicated with the secondary centrifugal device; or the condensing device comprises a rectangular circular receiving pipe, a valve, a condensing pipe A and a condensing pipe B; the condensing pipe A and the condensing pipe B are used for cooling alloy liquid in the mixed liquid into alloy powder; the outside of the condensing pipe A and the condensing pipe B are respectively provided with a pipe sleeve, and cooling oil is arranged between the pipe sleeves and the outer wall of the condensing pipe A; cooling oil is arranged between the pipe sleeve and the condensing pipe B; the secondary centrifugal device comprises a secondary centrifugal device A and a secondary centrifugal device B; the condensing pipe A is communicated with the secondary centrifugal device A; the condensing pipe B is communicated with the secondary centrifugal device B; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid centrifuged out from the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is connected with a valve, and the valve controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe A or controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe B; the centrifugal liquid phase forming device for preparing the ultra-micro tin-base alloy welding powder also comprises a melting furnace and a return pipe; the outside or bottom of the melting furnace is provided with a heating and heat-preserving device which can be used for melting solid alloy into liquid alloy; one end of the melting furnace is communicated with the hollow centrifugal cup and is used for feeding the mixed solution of the high-temperature medium oil and the alloy liquid into the centrifugal cup; one end of the return pipe is communicated with a medium oil outlet of the secondary centrifugal device, and the other end of the return pipe is communicated with the smelting furnace; the return pipe is used for returning the medium oil flowing out of the secondary centrifugal device to the smelting furnace; a flow regulating device is also arranged between the melting furnace and the centrifugal cup; the flow regulating device comprises a flow meter A and a flow regulating valve A; a reflux flow regulating device is also arranged between the reflux pipe and the melting furnace; the reflux flow regulating device comprises a reflux flow meter B and a reflux flow regulating valve B; the secondary centrifugal device comprises a hollow secondary centrifugal device main body; the secondary centrifugal device main body is used for receiving the medium oil and alloy powder mixed solution output from the condensing device; the medium oil outlet of the secondary centrifugal device is arranged at the upper part of one side of the main body of the secondary centrifugal device; the secondary centrifugal device main body is internally provided with a liquid separation basket for bearing alloy welding powder; the powder-liquid separation basket comprises a filter paper or a non-woven cloth hanging basket; the powder-liquid separation basket is driven by a motor M2 to rotate at a high speed, a filtering small hole is drilled on the outer circle of the powder-liquid separation basket, the aperture of the filtering small hole is 3-5 mm, the rotation speed of the motor M2 is 600-1000 rpm, a concentric barrel, namely a secondary centrifugal device main body, is sleeved outside the powder-liquid separation basket, oil suspension in the powder-liquid separation basket overflows from the outer circular hole of the powder-liquid separation basket under the action of centrifugal force, and powder of alloy welding powder is left in a filter paper or non-woven cloth hanging basket; the centrifugal cup and the outer cup are made of any one or more materials of zirconia, alumina and titanium alloy.
The technical scheme for solving the technical problems is that the centrifugal liquid phase forming method for preparing the ultra-micro tin-base alloy welding powder is based on the centrifugal liquid phase forming device for preparing the ultra-micro tin-base alloy welding powder; the method comprises the following steps of: continuously injecting the mixed solution of the molten liquid alloy and the medium oil into a centrifugal cup of a primary centrifugal device; centrifugal mixing is carried out in a centrifugal cup; the rotational linear velocity of the centrifugal cup is 5 m/s to 50 m/s; or the rotational speed of the centrifugal cup is in the range of 1000rpm to 10000rpm; step C: the mixed solution of the liquid alloy and the medium oil which are centrifuged out from the rectangular hole of the outer circular cup enters a condensing device for cooling; the cooling temperature ranges from (T-20) DEG C to (T-50) DEG C, wherein T is the alloy liquid phase temperature; step D: and C, cooling the mixed solution of the alloy powder and the medium oil in the step, and feeding the mixed solution into a secondary centrifugal device for centrifugal separation of the alloy powder and the medium oil.
The centrifugal liquid phase forming method for preparing the ultra-micro tin-base alloy welding powder further comprises the step E: collecting the alloy powder obtained in the step D, cleaning the collected alloy powder, and drying in a nitrogen protection atmosphere; in the step E, the cleaning agent used for cleaning is a degreasing solvent, and comprises any one or more of acetone ethanol, isopropanol, dichloromethane and trichloroethylene.
The mixed solution of the molten liquid alloy and the medium oil comprises a dispersing agent; the dispersant comprises any one or more of paraffin wax, polyamide wax, hydrogenated castor oil and petroleum sulfonate.
Step B is preceded by step A: melting the solid alloy into liquid alloy, and placing the liquid alloy solution into medium oil with the temperature higher than the melting point of the alloy; the medium oil is vegetable oil, including any one of olive oil, peanut oil, soybean oil, castor oil and rapeseed oil; further comprising step F: collecting the medium oil obtained in the step D, and returning the medium oil to the step A.
The saidLiquid alloyIs a tin-based alloy, and contains any one or more elements of Sb, bi, cu, ag, ni, co, in, ge, au; or saidLiquid alloyIs a tin-based alloy; the tin-based alloy includes any one of SnAgCu, snAg, snCu, snSb, snBi, snBiAg, snBiCu, snAu, snIn.
Compared with the prior art, one of the beneficial effects of this application is: the arrangement of the outer cup and the rectangular hole of the outer cup on the outer cup greatly reduces the possibility of collision among alloy particles to be formed in one-time centrifugation process. When the alloy particles to be formed are in a liquid state, the alloy particles are not solidified into a liquid state, and the appearance is very easy to be influenced by external forces such as collision. Collisions are unavoidable during the atomization centrifugation or other centrifugation; according to the technical scheme, the alloy after primary centrifugation enters the outer circular cup together with the medium oil in a liquid state, and flows into the condensing device through the rectangular hole of the outer circular cup, and the whole process is positioned in the medium oil, so that the shape and the size of alloy particles are well maintained under the surface tension of the liquid alloy; the size of the alloy liquid drops obtained by atomization after one-time centrifugation determines the size of alloy particles in the cooling process; the size of the finally prepared alloy particles can be controlled by controlling the size of the alloy liquid drops, so that the method is very simple, convenient and efficient; and avoid the collision of alloy particles in the forming process, and further maintain the shape integrity and the size consistency of the alloy particles.
Compared with the prior art, the second beneficial effect of this application is: the centrifugal cup and the outer cup are coaxially arranged, so that the coordination between the centrifugal cup and the outer cup is ensured, and the mixed solution of the medium oil and the alloy liquid is uniformly distributed between the outer cup and the outer cup, so that the mixed solution can be output from the rectangular hole of the outer cup at a stable flow rate; meanwhile, through holes of the centrifugal cup centrifugally atomize metal alloy melt liquid drops with equal diameters, and the liquid metal flow is cut into ultra-micro liquid drops with equal diameters and equal dimensions by rectangular holes of the outer circular cup, so that consistency and stability of particles generated in the process are ensured.
Compared with the prior art, the beneficial effect of this application is three: the plurality of rectangular holes of the outer circular cup are arranged at intervals, so that the flow is increased, and the consistency and stability of the flow are ensured.
Compared with the prior art, the beneficial effects of the application are as follows: the high-speed motor ensures that the liquid alloy and the medium oil can be fully mixed at the speed of one-time centrifugation, so that the alloy dispersion degree and the mixing uniformity are ensured; the liquid alloy can be dispersed to the degree of ultrafine particles, is very suitable for the preparation of ultrafine particles, and the output ultrafine particles are more concentrated in distribution.
Compared with the prior art, the beneficial effects of the application are as follows: the rectangular round receiving pipe and the condensing pipe are arranged, so that the solidification process of the liquid alloy becomes more controllable.
Compared with the prior art, the beneficial effects of the application are as follows: the condensing pipe A is communicated with the secondary centrifugal device A, and the condensing pipe B is communicated with the secondary centrifugal device B; the two sets of cooling and secondary centrifugal devices are arranged, so that the preparation can be continuously carried out, the two sets of cooling and secondary centrifugal devices can be switched, and the centrifugal liquid phase forming device for preparing the ultra-micro tin-base alloy welding powder can be ensured to continuously operate.
Compared with the prior art, the seventh beneficial effect of this application is: the arrangement of the return pipe enables the medium oil in the return pipe to be recycled in the device, so that the loss of the medium oil in the process is avoided, the medium oil in the return pipe also has partial energy, the energy loss of heating from room temperature is avoided, and the device is more energy-saving and environment-friendly.
Compared with the prior art, the eighth beneficial effect of this application is: the flow regulating device and the reflux flow regulating device enable the flow in the process to be conveniently managed and controlled in real time.
Compared with the prior art, the nine beneficial effects of this application are: the medium oil outlet in the secondary centrifugal device is arranged at the upper part of one side of the main body of the secondary centrifugal device, so that the medium oil can flow back conveniently; the system efficiency is improved; the centrifugal paper or the centrifugal non-woven cloth hanging basket for bearing the alloy powder also facilitates the taking out of the superfine alloy powder.
Compared with the prior art, ten beneficial effects of this application are: the centrifugal cup and the outer cup made of zirconia, alumina and titanium alloy are very suitable for high-temperature application scenes such as alloy melting.
Compared with the prior art, the eleven beneficial effects of this application are: the alloy powder enters a condensing device for cooling through the centrifugal outlet of the rectangular hole of the outer cup between the two centrifugal processes, so that the liquid alloy can be fully dispersed to prepare the alloy powder of ultrafine particles during one-time centrifugation; can be separated from medium oil during secondary centrifugation, and is a very efficient production method.
Compared with the prior art, twelve beneficial effects of the application are as follows: the cleaning enables the carbon compound grease adhered to the surface of the ultrafine powder to be removed, reduces the oxygen content of the ultrafine powder, increases the fluidity of the ultrafine powder, forms a compact oxide film, and increases the chemical matching stability of the ultrafine powder and the soldering paste.
Compared with the prior art, the thirteen beneficial effects of this application are: the dispersing agent can effectively reduce the surface tension of liquid metal, so that the liquid metal is suspended in medium oil with large density difference, and the centrifugated ultrafine liquid drop particles do not shrink or polymerize.
Compared with the prior art, fourteen of the beneficial effects of this application are: the medium oil can be recycled, so that the loss is reduced, the energy consumption is reduced, and the comprehensive efficiency of the process is improved.
Drawings
FIG. 1 is a schematic view of a first embodiment of a centrifugal liquid phase forming apparatus;
FIG. 2 is a schematic front view of a centrifuge cup in a primary centrifuge;
FIG. 3 is a schematic front view of an outer cup in a primary centrifuge;
FIG. 4 is a schematic front view showing the combination of the outer cup and the centrifugal cup in the primary centrifugal device;
FIG. 5 is a schematic illustration of the connection of an outer cup and a rectangular rounded receiving tube in a primary centrifuge;
FIG. 6 is a schematic view of a second embodiment of a centrifugal liquid phase forming apparatus;
in fig. 1 to 6, reference numeral 10 denotes a melting furnace, reference numeral 12 denotes medium oil, reference numeral 11 denotes a metal alloy, reference numeral 15 denotes a flow rate adjusting device, and reference numeral 16 denotes a powder-liquid separated superalloy welding powder; reference numeral 21 is a centrifugal cup, and reference numeral 215 is a centrifugal cup through hole; reference numeral 22 is an outer cup, reference numeral 225 is a rectangular hole of the outer cup; reference numeral 23 is a centrifugal motor M1; reference numeral 31 is a rectangular-to-circular receiving pipe, and reference numeral 315 is an ultra-micro droplet after centrifugation; reference numeral 32 denotes a condenser tube, 321 denotes a condenser tube a, and 322 denotes a condenser tube B; reference numeral 70 denotes a secondary centrifugal device B, and reference numeral 50 denotes a secondary centrifugal device a; reference numeral 52 denotes a secondary centrifuge main body, reference numeral 55 denotes a medium oil outlet, reference numeral 53 denotes a drive motor M2 of the secondary centrifuge, and reference numeral 54 denotes a powder-liquid separation basket; reference numeral 62 denotes a return pipe, and reference numeral 63 denotes a return flow rate adjustment device;
FIG. 7 is an SEM image of example 1 of the production of an ultra-fine solder powder at 1000 magnification;
FIG. 8 is an SEM image of example 2 of the production of an ultra-fine solder powder at 5000 magnification;
FIG. 9 is an SEM image of example 3 of the production of an ultra-fine solder powder at 5000 magnification;
FIG. 10 is an SEM image of example 4 of the production of an ultra-fine solder powder at 8000 Xmagnification;
FIG. 11 is an SEM image of example 5 of the production of an ultra-fine solder powder at 3300;
FIG. 12 is an SEM image of comparative example 1, which shows a magnification of 1000;
FIG. 13 is an SEM image of comparative example 2, the magnification of the image being 2000;
FIG. 14 is an SEM image of comparative example 3, the magnification of the image being 3000;
FIG. 15 is an SEM image of comparative example 4, the magnification of the image being 2000;
SEM is an acronym Scanning Electron Microscope, meaning scanning electron microscopy.
Detailed Description
The present application is described in further detail below in conjunction with the various figures.
Wt% in the present document means mass% and min means time unit minutes.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-fine tin-based alloy welding powder as shown in fig. 1 to 5, the apparatus comprises a primary centrifugal apparatus, a condensing apparatus and a secondary centrifugal apparatus; the primary centrifugal device comprises a centrifugal cup and an outer cup; both the centrifugal cup and the outer cup are hollow; the centrifugal cup is connected with the centrifugal motor M1 for centrifugal rotation, and the outer cup is fixed; the wall of the centrifugal cup is provided with a centrifugal cup through hole for centrifuging the mixed solution; the diameter of the outer cup is larger than that of the centrifugal cup, and the outer cup is sleeved on the periphery of the centrifugal cup; the cup wall of the outer cup is provided with an outer cup rectangular hole; the rectangular hole of the outer cup is communicated with the condensing device; the condensing device is communicated with the secondary centrifugal device.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, a centrifugal cup is used for accommodating a mixed solution of high-temperature medium oil and alloy liquid; the centrifugal cup can be driven by an external motor to rotate and drive the mixed solution in the centrifugal cup to rotate; under the action of centrifugal force, the mixed solution flows into the outer circular cup through the through hole of the centrifugal cup; the mixed solution in the outer cup enters a condensing device through the rectangular hole of the outer cup; cooling the centrifuged mixed solution through a condensing device, and cooling tiny suspended particles in the mixed solution into alloy powder; the mixed solution containing the medium oil and the alloy powder enters a secondary centrifugal device to separate the medium oil and the alloy powder.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, a primary centrifugal apparatus includes a centrifugal cup and an outer cup coaxially disposed; the cross sections of the outer circular cup and the centrifugal cup have the same center; the diameter of the centrifugal cup ranges from 50 mm to 300 mm; the wall thickness of the centrifugal cup ranges from 1 mm to 5 mm; the diameter of the through hole of the centrifugal cup ranges from 0.02 mm to 0.5 mm.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, the width of the rectangular hole of the outer cup ranges from 2 mm to 5 mm; the length of the rectangular hole of the outer cup ranges from 10 mm to 50 mm.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, an outer cup rectangular hole provided on a cup wall of an outer cup includes an outer cup rectangular hole a and an outer cup rectangular hole B; the center-to-center spacing between the rectangular hole A and the rectangular hole B is 5 mm to 10 mm.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, the centrifugal motor M1 is a high-speed motor, and the motor rotation speed ranges from 1000rpm to 10000rpm.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, the condensing apparatus includes a rectangular circular receiving pipe and a condensing pipe; the condensing tube is used for cooling the alloy liquid in the mixed liquid into alloy powder; a pipe sleeve is arranged outside the condensing pipe, and cooling oil is arranged between the pipe sleeve and the outer wall of the condensing pipe; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid flowing out of the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is communicated with one end of the condensing pipe; the other end of the condensing tube is communicated with the secondary centrifugal device.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder as shown in fig. 6, a condensing apparatus comprises a rectangular rounded receiving pipe, a valve, a condensing pipe a and a condensing pipe B; the condensing pipe A and the condensing pipe B are used for cooling alloy liquid in the mixed liquid into alloy powder; the outside of the condensing pipe A and the condensing pipe B are respectively provided with a pipe sleeve, and cooling oil is arranged between the pipe sleeves and the outer wall of the condensing pipe A; cooling oil is arranged between the pipe sleeve and the condensing pipe B; the secondary centrifugal device comprises a secondary centrifugal device A and a secondary centrifugal device B; the condensing pipe A is communicated with the secondary centrifugal device A; the condensing pipe B is communicated with the secondary centrifugal device B; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid flowing out of the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is connected with a valve, and the valve controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe A or controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe B. The valve is not shown in the drawings.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-fine tin-based alloy welding powder as shown in fig. 1 to 5, further comprising a melting furnace and a return pipe; the melting furnace is used for melting the solid alloy into the liquid alloy; one end of the melting furnace is communicated with the hollow centrifugal cup and is used for feeding the mixed solution of the high-temperature medium oil and the alloy liquid into the centrifugal cup; one end of the return pipe is communicated with a medium oil outlet of the secondary centrifugal device, and the other end of the return pipe is communicated with the smelting furnace; the return pipe is used for returning the medium oil flowing out of the secondary centrifugal device to the smelting furnace.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing ultra-micro tin-based alloy welding powder as shown in fig. 1 to 5, a flow rate adjusting device is further provided between the melting furnace and the centrifugal cup; the flow regulating device comprises a flow meter A and a flow regulating valve A; a reflux flow regulating device is also arranged between the reflux pipe and the melting furnace; the reflux flow regulating device comprises a reflux flow meter B and a reflux flow regulating valve B.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing an ultra-fine tin-based alloy welding powder as shown in fig. 1 to 5, a secondary centrifugal apparatus includes a hollow secondary centrifugal apparatus body; the secondary centrifugal device main body is used for receiving the medium oil and alloy powder mixed solution output from the condensing device; the medium oil outlet of the secondary centrifugal device is arranged at the upper part of one side of the main body of the secondary centrifugal device; the secondary centrifugal device main body is internally provided with a powder-liquid separation basket for bearing alloy powder; the powder-liquid separation basket comprises a filter paper or a non-woven cloth hanging basket.
In an embodiment of a centrifugal liquid phase forming apparatus for preparing ultra-fine tin-based alloy welding powder, not shown in some drawings, the centrifugal cup and the outer cup are made of any one or more materials of zirconia, alumina and titanium alloy.
In an embodiment of a centrifugal liquid phase forming method for preparing an ultra-fine tin-based alloy welding powder, not shown in some drawings, a centrifugal liquid phase forming apparatus for preparing an ultra-fine tin-based alloy welding powder is based on the above; the method comprises the following steps of: melting the solid alloy into liquid alloy, and placing the liquid alloy solution into medium oil with the temperature higher than the melting point of the alloy; and (B) step (B): continuously injecting the mixed solution of the molten liquid alloy and the medium oil into a centrifugal cup of a primary centrifugal device; centrifugal mixing is carried out in a centrifugal cup; the rotational speed of the centrifugal cup is 1000rpm to 10000rpm (rpm is revolutions per minute); step C: the mixed solution of the liquid alloy and the medium oil overflowed from the rectangular hole of the outer cup enters a condensing device for cooling; the cooling temperature ranges from (T-20) DEG C to (T-50) DEG C, wherein T is the alloy liquid phase temperature; step D: c, allowing the cooled mixed solution of the alloy powder and the medium oil to enter a secondary centrifugal device for centrifugal separation of the alloy powder and the medium oil; step E: and (D) collecting the alloy powder obtained in the step (D), and cleaning the collected alloy powder. In the step E, the cleaning agent used for cleaning is a degreasing solvent, and comprises any one or more of acetone ethanol, isopropanol, dichloromethane and trichloroethylene. Step F: collecting the medium oil obtained in the step D, and returning the medium oil to the step A.
The mixed solution of the molten liquid alloy and the medium oil comprises a dispersing agent; the dispersant comprises any one or more of paraffin wax, polyamide wax, hydrogenated castor oil and petroleum sulfonate.
The saidLiquid alloyIs a tin-based alloy, and contains any one or more elements of Sb, bi, cu, ag, ni, co, in, ge, au.
The saidLiquid alloyIs a tin-based alloy; the tin-based alloy includes any one of SnAgCu, snAg, snCu, snSb, snBi, snBiAg, snBiCu, snAu, snIn.
The medium oil is vegetable oil, including any one of olive oil, peanut oil, soybean oil, castor oil and rapeseed oil.
In fig. 1 to 6, reference numeral 10 is a melting furnace, i.e., a tin furnace, and reference numeral 15 is a flow rate adjusting device, in which a flow rate meter a and a flow rate adjusting valve a are not shown; reference numeral 63 denotes a reflux flow rate adjusting device, and the reflux flow meter B and the reflux flow rate adjusting valve B are not shown in the drawings. The alloy designated 11 is in a solid state upon being placed in the furnace and is melted into a liquid alloy in the furnace 10; the liquid alloy 11 is centrifugally dispersed in a centrifugal cup, condensed by a condensing device and enters a secondary centrifugal device to separate alloy and medium oil. The temperature of the medium oil 12 in the furnace is above the alloy melting temperature; the temperature of the medium oil 12 in the condensing unit and the secondary centrifuging unit is lower than the alloy melting temperature.
In the embodiment 1 of the tin-base alloy welding powder prepared by the centrifugal liquid phase forming method of the ultra-micro tin-base alloy welding powder, SAC305 tin-base alloy is placed in a tin furnace, namely a smelting furnace, high-temperature medium oil is added, alloy liquid is melted, the temperature is set to 270 ℃, the tin-base alloy solution flows into a rotating centrifugal cup along with the high-temperature medium oil, the diameter of the rotating centrifugal cup is 100 mm, the wall thickness of the rotating centrifugal cup is 5 mm, the thickness of the wall of the rotating centrifugal cup is regularly perforated by 0.1 mm, the rotating centrifugal cup rotates at a high speed of 4000rpm, the tin-base alloy solution throws out tiny metal drops with equal diameter and the like from a through hole of the centrifugal cup on the rotating centrifugal cup and a rectangular hole of an outer cup of a concentric outer cup in a pulse mode, the tin-base alloy solution falls into a rectangular circular receiving pipe, the tin-base alloy receiving pipe enters a condensing pipe under the driving of liquid oil medium, and the spherical drops are cooled below the liquidus of the tin-base alloy, and the spherical drops are solidified into spherical powder to be dispersed in the medium oil. The metal solution flows out from the through holes of the centrifugal cup to present a metal liquid flow with equal diameter, the metal liquid flow is cut off into ultrafine metal liquid drops with a small section by the rectangular holes of the outer cup of the concentric outer cup, and the through holes are arranged in an array, so that the through holes of the centrifugal cup flow out a row of metal liquid flow at regular intervals and are continuously cut off by the rectangular holes of the cup, and then the ultrafine metal liquid drops with equal diameter and equal size are thrown out in a pulse mode.
The rear end of the condensing tube is connected with a centrifugal machine, and the centrifugal machine is one or more than two centrifugal machines which are connected in parallel. The medium oil suspended with the ultra-micro welding powder is introduced into a centrifugal machine, a layer of filter paper is attached to the inner side of the centrifugal machine, the centrifugal machine rotates at a high speed under the drive of a rotating motor, metal particles with high specific gravity in suspension are dispersed on the filter paper on the inner wall of the centrifugal machine under the action of centrifugal force and self gravity, and medium oil with low specific gravity is discharged from a medium oil outlet on the centrifugal machine and is introduced into a tin furnace through a connecting pipe. After the superfine welding powder separated on the filter paper reaches a certain amount, the feeding valve of the centrifuge is closed, and the suspension is led into another centrifuge connected in parallel for continuous separation operation. And during the process, the first centrifugal machine is used for collecting the superfine welding powder and preparing for separating again, so that continuous circulation production of the superfine welding powder centrifugal liquid phase forming is realized. After the collected ultra-micro welding powder is cleaned by a cleaning agent and is protected by nitrogen and dried, the ultra-micro tin-based welding powder 1 is obtained, the particle ratio of the test particle size T7 (2 to 11 um) is 92%, the oxygen content is 420ppm, the sphericity is good, the powder surface is smooth, the technical index of the electronic industry standard is met, and the ultra-micro welding powder SEM is shown in figure 7.
In the embodiment 2 of the tin-base alloy welding powder prepared by the centrifugal liquid phase forming method of the ultra-micro tin-base alloy welding powder, the Sn90Sb10 tin-base alloy is added with high-temperature medium oil in a tin furnace, namely a melting furnace, the molten alloy is set at 280 ℃, the tin-base alloy solution flows into a rotating centrifugal cup along with the high-temperature medium oil, the diameter of the rotating centrifugal cup is 200 mm, the wall thickness of the rotating centrifugal cup is 3 mm, holes are regularly formed by 0.05 mm, the rotating centrifugal cup rotates at a high speed of 4000rpm, the production process is the same as that of the embodiment 1, the ultra-micro tin-base welding powder 2 is obtained, the particle ratio of the obtained particle size T8 (2-8 um) after testing is more than 95%, the oxygen content is 490ppm, the sphericity is good, the powder surface is smooth, the technical index of the electron industry standard is met, and the ultra-micro welding powder SEM is shown in figure 8.
In the embodiment 3 of the tin-base alloy welding powder prepared by the centrifugal liquid phase forming method of the ultra-micro tin-base alloy welding powder, the Sn42Bi57.6Ag0.4tin-base alloy is added into a tin furnace 1, namely a smelting furnace, high-temperature medium oil is added, alloy liquid is melted, the temperature is set to 190 ℃, the tin-base alloy solution flows into a rotating centrifugal cup along with the high-temperature medium oil, the diameter of the rotating centrifugal cup is 300 mm, the wall thickness of the rotating centrifugal cup is 1 mm, holes are regularly formed by 0.03 mm, the rotating centrifugal cup rotates at a speed of 1300rpm at a high speed, the production process is the same as in the embodiment 1, the ultra-micro tin-base welding powder 3 is obtained, the particle ratio of the obtained particle size T6 (5-15 um) after testing is 93%, the oxygen content is 220ppm, the sphericity is good, the powder surface is smooth, the technical index of the electron industry standard is met, and the ultra-micro welding powder SEM is shown in figure 9.
In the embodiment 4 of the tin-base alloy welding powder prepared by the centrifugal liquid phase forming method of the ultra-micro tin-base alloy welding powder, sn96.5Ag3Cu0.5 tin-base alloy is added into a tin furnace 1, namely a smelting furnace, high-temperature medium oil is added, alloy liquid is melted, the temperature is set to 270 ℃, the tin-base alloy solution flows into a rotating centrifugal cup along with the high-temperature medium oil, the diameter of the rotating centrifugal cup is 400 mm, the wall thickness of the rotating centrifugal cup is 5 mm, holes are regularly formed by 0.02 mm, the rotating centrifugal cup rotates at a high speed of 2000rpm, the production process is the same as in the embodiment 1, ultra-micro tin-base welding powder 4 is obtained, the particle ratio of the obtained particle size T9 (1-5 um) after testing is 92%, the oxygen content is 750ppm, the sphericity is good, the powder surface is smooth, the technical index of the electron industry standard is met, and the ultra-micro welding powder SEM is shown in figure 10.
In the embodiment 5 of the tin-base alloy welding powder prepared by the centrifugal liquid phase forming method of the ultra-micro tin-base alloy welding powder, sn90.5Ag3Cu0.5Bi6 tin-base alloy is added into a tin furnace 1, namely a smelting furnace, high-temperature medium oil is added, molten alloy liquid is melted, the temperature is set to 270 ℃, the tin-base alloy solution flows into a rotating centrifugal cup along with the high-temperature medium oil, the diameter of the rotating centrifugal cup is 500 mm, the wall thickness of the rotating centrifugal cup is 8 mm, holes are regularly formed by 0.02 mm, the rotating centrifugal cup rotates at a high speed of 2000m/s, the production process is the same as that of the embodiment 1, the ultra-micro tin-base welding powder 5 is obtained, the particle ratio of the particle with the particle size T10 (1-3 um) is 90 percent, the oxygen content is 960ppm, the sphericity is good, the powder surface is smooth, the technical index of the electron industry standard is met, and the ultra-micro welding powder SEM is shown in figure 11.
Comparative example 1: the method is characterized in that ultra-micro welding powder SAC 305T 6 of a foreign commercial centrifugal process is adopted, the particle ratio of the particle size distribution (5-15 um) is tested to be 90%, the surface of tin powder is obviously damaged when observed by a scanning electron microscope, and a large number of irregular special-shaped particles exist, and the SEM image 12 is shown.
Comparative example 2: the commercial ultra-micro welding powder SAC 305T 7 with the liquid phase forming process is adopted, the particle ratio of the particle with the particle size distribution (2-11 um) is tested to be 91%, and the scanning electron microscope is used for observing the surface damage of the tin powder, and the surface damage has the rugged state, as shown in an SEM (scanning electron microscope) figure 13.
Comparative example 3: and taking superfine welding powder SAC 305T 7 of a centrifugal atomization airflow separation process sold in the market, wherein the particle ratio of the test particle size distribution (2-11 um) is 92%, and observing that the surface of the tin powder is irregular and special-shaped particles by a scanning electron microscope, and the surface of the tin powder is not smooth and flat. See SEM fig. 14.
Comparative example 4: the ultra-micro welding powder SAC 305T 9 of the foreign market gas atomization gas flow separation process is adopted, the particle ratio of the particle with the particle size distribution (1-5 um) is 77%, the surface of the tin powder is obviously damaged when observed by a scanning electron microscope, and a small amount of irregular special-shaped particles exist, and the SEM image 15 is shown.
A centrifugal liquid phase forming device and method for preparing ultra-micro tin-based alloy welding powder are provided. The high-efficiency centrifugal atomization technology and the high-product-quality liquid phase forming technology are combined together, so that the continuous and high-quality ultra-micro welding powder is prepared efficiently, meanwhile, medium auxiliary materials in the production process can be recycled, the production cost is saved, and the production efficiency is improved.
The foregoing description is only exemplary embodiments of the present application, and is not intended to limit the scope of the patent application, but rather, the patent application is intended to cover any equivalents of the structures or equivalent processes described by the specification and drawings, or any other related application, directly or indirectly.
Claims (10)
1. A centrifugal liquid phase forming device for preparing ultra-micro tin-base alloy welding powder is characterized in that
Comprises a primary centrifugal device, a condensing device and a secondary centrifugal device;
the primary centrifugal device comprises a centrifugal cup and an outer cup; both the centrifugal cup and the outer cup are hollow; the centrifugal cup is connected with the centrifugal motor M1 for centrifugal rotation, and the outer cup is fixed;
the wall of the centrifugal cup is provided with a centrifugal cup through hole for flowing out the mixed solution; the diameter of the outer cup is larger than that of the centrifugal cup, and the outer cup is sleeved on the periphery of the centrifugal cup; the cup wall of the outer cup is provided with an outer cup rectangular hole; the rectangular hole of the outer cup is communicated with the condensing device; the condensing device is communicated with the secondary centrifugal device.
2. The centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder according to claim 1, wherein,
the primary centrifugal device comprises a centrifugal cup and an outer circular cup which are coaxially arranged; the cross sections of the outer circular cup and the centrifugal cup have the same center;
the diameter of the centrifugal cup ranges from 50 mm to 300 mm; the wall thickness of the centrifugal cup ranges from 1 mm to 5 mm; the diameter of the through hole of the centrifugal cup ranges from 0.02 mm to 0.5 mm.
3. The centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder according to claim 1, wherein,
the width of the rectangular hole of the outer circular cup ranges from 2 mm to 5 mm; the length of the rectangular hole of the outer cup ranges from 10 mm to 50 mm.
4. The centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder according to claim 1, wherein,
the outer cup rectangular hole formed in the cup wall of the outer cup comprises an outer cup rectangular hole A and an outer cup rectangular hole B; the center-to-center distance between the rectangular hole A of the outer cup and the rectangular hole B of the outer cup is 5 mm to 10 mm;
a heat preservation device is arranged outside the outer cup and is used for keeping the temperature balance of the centrifugal cup and the outer cup;
the centrifugal motor M1 is a high-speed motor, and the motor rotation speed ranges from 1000rpm to 10000rpm.
5. The centrifugal liquid phase forming apparatus for preparing an ultra-micro tin-based alloy welding powder according to claim 1, wherein,
the condensing device comprises a rectangular circular receiving pipe and a condensing pipe; the condensing pipe is used for cooling the alloy liquid drops in the mixed liquid into alloy powder; a pipe sleeve is arranged outside the condensing pipe, and cooling oil is arranged between the pipe sleeve and the outer wall of the condensing pipe; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid flowing out of the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is communicated with one end of the condensing pipe; the other end of the condensing tube is communicated with the secondary centrifugal device;
or the condensing device comprises a rectangular circular receiving pipe, a valve, a condensing pipe A and a condensing pipe B; the condensing pipe A and the condensing pipe B are used for cooling alloy liquid in the mixed liquid into alloy powder; the outside of the condensing pipe A and the condensing pipe B are respectively provided with a pipe sleeve, and cooling oil is arranged between the pipe sleeves and the outer wall of the condensing pipe A; cooling oil is arranged between the pipe sleeve and the condensing pipe B; the secondary centrifugal device comprises a secondary centrifugal device A and a secondary centrifugal device B; the condensing pipe A is communicated with the secondary centrifugal device A; the condensing pipe B is communicated with the secondary centrifugal device B; one end of the rectangular-shaped circular receiving pipe is communicated with an outer cup rectangular hole on the outer cup and is used for receiving mixed liquid flowing out of the outer cup rectangular hole; the other end of the rectangular circular receiving pipe is connected with a valve, and the valve controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe A or controls the other end of the rectangular circular receiving pipe to be communicated with the condensing pipe B;
the centrifugal liquid phase forming device for preparing the ultra-micro tin-base alloy welding powder also comprises a melting furnace and a return pipe; the outside or bottom of the melting furnace is provided with a heating and heat-preserving device which can be used for melting solid alloy into liquid alloy; one end of the melting furnace is communicated with the hollow centrifugal cup and is used for feeding the mixed solution of the high-temperature medium oil and the alloy liquid into the centrifugal cup; one end of the return pipe is communicated with a medium oil outlet of the secondary centrifugal device, and the other end of the return pipe is communicated with the smelting furnace; the return pipe is used for returning the medium oil flowing out of the secondary centrifugal device to the smelting furnace; a flow regulating device is also arranged between the melting furnace and the centrifugal cup; the flow regulating device comprises a flow meter A and a flow regulating valve A; a reflux flow regulating device is also arranged between the reflux pipe and the melting furnace; the reflux flow regulating device comprises a reflux flow meter B and a reflux flow regulating valve B;
the secondary centrifugal device comprises a hollow secondary centrifugal device main body; the secondary centrifugal device main body is used for receiving the medium oil and alloy powder mixed solution output from the condensing device; the medium oil outlet of the secondary centrifugal device is arranged at the upper part of one side of the main body of the secondary centrifugal device; the secondary centrifugal device main body is internally provided with a powder-liquid separation basket for bearing alloy welding powder; the powder-liquid separation basket comprises a filter paper or a non-woven cloth hanging basket; the powder-liquid separation basket is driven by a motor M2 to rotate at a high speed, a filtering small hole is drilled on the outer circle of the powder-liquid separation basket, the aperture of the filtering small hole is 3-5 mm, the rotation speed of the motor M2 is 600-1000 rpm, a concentric barrel, namely a secondary centrifugal device main body, is sleeved outside the powder-liquid separation basket, oil suspension in the powder-liquid separation basket overflows from the outer circular hole of the powder-liquid separation basket under the action of centrifugal force, and powder of alloy welding powder is left in a filter paper or non-woven cloth hanging basket;
the centrifugal cup and the outer cup are made of any one or more materials of zirconia, alumina and titanium alloy.
6. A centrifugal liquid phase forming method for preparing ultra-micro tin-base alloy welding powder is characterized in that
A centrifugal liquid phase forming apparatus for producing an ultra-fine tin-based alloy welding powder according to any one of claims 1 to 5;
comprises the steps of,
and (B) step (B): continuously injecting the mixed solution of the molten liquid alloy and the medium oil into a centrifugal cup of a primary centrifugal device; centrifugal mixing is carried out in a centrifugal cup; the rotational linear velocity of the centrifugal cup is 5 m/s to 50 m/s; or the rotational speed of the centrifugal cup is in the range of 1000rpm to 10000rpm;
step C: the mixed solution of the liquid alloy and the medium oil which are centrifuged out from the rectangular hole of the outer circular cup enters a condensing device for cooling; the cooling temperature ranges from (T-20) DEG C to (T-50) DEG C, wherein T is the alloy liquid phase temperature;
step D: and C, cooling the mixed solution of the alloy powder and the medium oil in the step, and feeding the mixed solution into a secondary centrifugal device for centrifugal separation of the alloy powder and the medium oil.
7. The centrifugal liquid phase forming method for preparing an ultra-micro tin-based alloy welding powder according to claim 6, wherein,
further comprising step E: collecting the alloy powder obtained in the step D, cleaning the collected alloy powder, and drying in a nitrogen protection atmosphere;
in the step E, the cleaning agent used for cleaning is a degreasing solvent, and comprises any one or more of acetone ethanol, isopropanol, dichloromethane and trichloroethylene.
8. The centrifugal liquid phase forming method for preparing an ultra-micro tin-based alloy welding powder according to claim 6, wherein,
the mixed solution of the molten liquid alloy and the medium oil comprises a dispersing agent; the dispersant comprises any one or more of paraffin wax, polyamide wax, hydrogenated castor oil and petroleum sulfonate.
9. The centrifugal liquid phase forming method for preparing an ultra-micro tin-based alloy welding powder according to claim 6, wherein,
step B is preceded by step A: melting the solid alloy into liquid alloy, and placing the liquid alloy solution into medium oil with the temperature higher than the melting point of the alloy; the medium oil is vegetable oil, including any one of olive oil, peanut oil, soybean oil, castor oil and rapeseed oil;
further comprising step F: collecting the medium oil obtained in the step D, and returning the medium oil to the step A.
10. The centrifugal liquid phase forming method for preparing an ultra-micro tin-based alloy welding powder according to claim 6, wherein,
the saidLiquid alloyIs a tin-based alloy, and contains any one or more elements of Sb, bi, cu, ag, ni, co, in, ge, au;
or saidLiquid alloyIs a tin-based alloy; the tin-based alloy includes any one of SnAgCu, snAg, snCu, snSb, snBi, snBiAg, snBiCu, snAu, snIn.
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