CN107116225B - Integrated induction smelting gas atomization powder preparation device and gas atomization powder preparation method - Google Patents

Integrated induction smelting gas atomization powder preparation device and gas atomization powder preparation method Download PDF

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Publication number
CN107116225B
CN107116225B CN201710358256.3A CN201710358256A CN107116225B CN 107116225 B CN107116225 B CN 107116225B CN 201710358256 A CN201710358256 A CN 201710358256A CN 107116225 B CN107116225 B CN 107116225B
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gas
powder
crucible
nozzle
gas atomization
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CN107116225A (en
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计红军
周均博
梁孟
陆骅俊
马舒
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Shenzhen Graduate School Harbin Institute of Technology
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Shenzhen Graduate School Harbin Institute of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0836—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with electric or magnetic field or induction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0888—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0892—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting nozzle; controlling metal stream in or after the casting nozzle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0896—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid particle transport, separation: process and apparatus
    • 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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Abstract

The invention provides an integrated induction smelting gas atomization powder preparation device and a gas atomization powder preparation method, wherein the device comprises a gas atomization powder preparation device, the gas atomization powder preparation device comprises a support frame and a gas atomization crucible, a quartz tube for collecting alloy powder is arranged on the support frame, and one end of the quartz tube is connected with a corundum tube for introducing protective gas; the support frame is provided with an induction coil, the gas atomization crucible is arranged in the induction coil, the bottom of the gas atomization crucible is provided with a nozzle, and the nozzle faces the inside of the quartz tube; the axis of the nozzle of the gas atomization crucible is perpendicular to the axis of the quartz tube; the opening of the corundum tube faces to the outlet of the nozzle; the open end of the quartz tube is sealed by a plug. The device has simple structure, small occupied area and easy assembly, can not cause the phenomenon of blocking nozzles by liquid in the pulverizing process, and can change the flow of the gas to change the particle size distribution ratio of the prepared powder.

Description

Integrated induction smelting gas atomization powder preparation device and gas atomization powder preparation method
Technical Field
The invention relates to an aerosolization powder making device, in particular to an integrated induction smelting aerosolization powder making device and a aerosolization powder making method.
Background
The gas atomization process is a main method for producing metal and alloy powder, and the principle of powder preparation is a process of pulverizing liquid metal flow flowing out of a liquid guide tube into small liquid drops by using high-speed air flow and solidifying the liquid metal flow into powder in the subsequent flight. The gas atomization powder has the advantages of controllable powder granularity, low oxygen content, suitability for the production of various metal and alloy powder, and the like, and becomes the main direction for preparing high-performance and special alloy powder. With the appearance of new materials in the new process of powder metallurgy and the application of powder materials in the industries of chemical industry, electronic device preparation, surface engineering, military and the like, the requirements on the purity, the fineness, the sphericity and the like of the powder are continuously improved, so that the development of the powder gas atomization method preparation technology is further promoted.
The metal melt is atomized by high-pressure air flow and becomes small liquid drops, and the small liquid drops are continuously cooled and solidified into powder in the downward flight. The oxygen content and shape of the powder are constantly changing during solidification, and when the conditions allow, the oxygen content of the powder can reach a lower level, and the shape is spherical. It is generally believed that powders with high sphericity and low oxygen content need to be prepared under vacuum conditions and are generally difficult to prepare under non-vacuum conditions. However, the vacuum atomization pulverizing device has a complex structure and high manufacturing and maintenance cost, and the produced powder has no cost advantage. Further research and practice have shown that the structural and functional configuration of the atomizing device is closely related to controlling the oxygen content and shape of the powder, and that the non-vacuum atomizing device can realize the preparation of the powder with high sphericity and low oxygen content.
At present, the traditional gas atomization powder making equipment is separated from a flow-limiting pouring system, so that the gas atomization powder making equipment is in certain contact with oxygen in the powder preparation process, so that the prepared powder has high oxygen content or the easily oxidized metal is completely oxidized, and the usability of the powder is reduced. Some gas atomization powder making equipment is of a smelting and pouring integrated structure, but most of the equipment has high vacuum requirements, is excessively complex in structure, is troublesome to operate and difficult to maintain, is high in price, and is unfavorable for atmosphere control because the volume of an atomization chamber of a non-vacuum gas atomization device is generally larger. Meanwhile, at present, a non-limiting atomizing nozzle is generally adopted in China, the particle size of prepared powder is difficult to be miniaturized, and the design of some special nozzles is also available, but the structure is relatively complex. In the gas atomization process, high-pressure gas is mostly adopted to spray the metal solution from an atomization chamber to form powder particles, and a nozzle is easy to block.
Disclosure of Invention
Aiming at the technical problems, the invention discloses an integrated induction smelting gas atomization powder making device and a gas atomization powder making method, which have the advantages of simple structure, small occupied area, easy assembly and no nozzle blockage phenomenon caused by liquid in the powder making process, and can change the flow rate of gas to change the particle size distribution ratio of prepared powder.
In this regard, the invention adopts the following technical scheme:
an integrated induction smelting gas atomization powder making device comprises a gas atomization powder making device, wherein the smelting device is arranged in induction heating equipment; the gas atomization powder preparation device comprises a support frame and a gas atomization crucible, wherein a quartz tube for collecting alloy powder is arranged on the support frame, and one end of the quartz tube is connected with a corundum tube for introducing protective gas; the support frame is provided with an induction coil, the gas atomization crucible is arranged in the induction coil, the bottom of the gas atomization crucible is provided with a nozzle, and the nozzle faces the inside of the quartz tube; the axis of the nozzle of the gas atomization crucible is perpendicular to the axis of the quartz tube; the opening of the corundum tube faces to the outlet of the nozzle; the opening end of the quartz tube is sealed by a plug; the gas atomization crucible is provided with a gas inlet connected with an external gas cylinder.
By adopting the technical scheme, the gas atomization crucible with the nozzle and the air inlet is used for realizing the dripping of alloy liquid, the opening ends at the two ends are used for realizing the collection of atomized powder through the quartz tube sealed by the plugs, the small crucible for keeping molten metal is tightly connected with the quartz tube, the atomization chamber and the preliminary screening chamber are both arranged in the quartz tube, and the vertical atomization design is adopted for carrying out the gas atomization preparation of the powder. The axis of the nozzle of the gas atomization crucible is perpendicular to the axis of the quartz tube, so that vertical atomization is realized, and the purpose of enabling atomized powder to perform horizontal throwing motion can be realized, so that spherical powder with larger particle size is closer to the nozzle, and spherical powder with smaller particle size is farther from the nozzle, so that preliminary screening of the powder is realized.
As a further improvement of the invention, the nozzle is of an inverted cone structure, and the angle of the cone angle of the nozzle is 75-85 degrees. With this angle of nozzle, the molten metal is atomized by allowing the molten metal to stay in the nozzle for a while due to the surface tension and by allowing the molten metal to rapidly flow into the atomizing chamber when the flow rate of the gas introduced into the nozzle is increased.
Further, the gas atomization crucible in the atomization device is provided with a cylindrical gas inlet connected with an external gas cylinder, and protective gas is introduced in the atomization process.
As a further development of the invention, the angle of the cone angle of the nozzle is 80 °. The nozzle at the bottom of the gas atomization crucible adopts an 80-DEG conical design, the angle is 80 DEG, so that molten metal can stay in the nozzle for a period of time due to the action of surface tension, and when the gas flow rate introduced into the nozzle is increased, the molten metal can quickly flow into the atomization chamber for atomization, the bottom of the small crucible is compactly connected with a circular through hole on one side of the quartz tube, the axis of the small crucible is ensured to be perpendicular to the axis of the quartz tube, and vertical atomization is realized.
Furthermore, the gas atomization crucible is provided with a crucible cover which is in interference fit with the crucible, a layer of plasticine is coated at the well-matched joint, and a circular ring is arranged at the upper part of the crucible cover for convenient taking; the small crucible and the supporting frame coil are mechanically fixed, and the periphery is only provided with an induction coil for melting alloy.
As a further improvement of the invention, the corundum tube is connected with the gas cylinder through a pneumatic valve; the gas atomization crucible is connected with an external gas cylinder through a gas flowmeter.
As a further improvement of the invention, at least two semi-cylindrical quartz baffle plates are arranged in the quartz tube.
As a further improvement of the invention, 4 semi-cylindrical quartz baffle plates are arranged in the quartz tube, and the preliminary screening of the powder with different spherical diameters can be realized by adjusting the distance between the two quartz baffle plates.
As a further improvement of the invention, the corundum tube is a porous corundum tube; the mouth of the quartz tube is provided with a punching solid silica gel plug, and the punching solid silica gel plug is in interference fit with the quartz tube.
As a further improvement of the invention, it comprises a smelting device, which is placed in the induction heating apparatus; the smelting device comprises a first smelting container and a smelting container cover, and a second smelting container is arranged in the first smelting container; the melting container cover is provided with a protective gas inlet and a protective gas outlet; a heat insulation layer is arranged between the first smelting container and the second smelting container, and the heat insulation layer is made of aluminum silicate cotton. The cover of the melting container is provided with a protective gas inlet and a protective gas outlet, so that the contact between the alloy and oxygen in the melting process is avoided, and the oxygen content of the final alloy powder is reduced. The induction heating device is an induction coil.
Further, the first smelting container is a quartz cup with a cylindrical hole, the second smelting container is a smelting ceramic crucible, and the quartz cup is matched with a quartz cover with the cylindrical hole.
As a further improvement of the invention, the support frame adopts a telescopic structure.
As a further improvement of the present invention, the opening of the quartz tube is in close contact with the nozzle opening;
as a further improvement of the invention, the corundum tube is aligned to the outlet of the nozzle of the aerosolizing crucible, and a solid silica gel plug is glued to the quartz tube with tape.
As a further improvement of the invention, the joint of the quartz cup and the quartz cover of the smelting device is provided with an O-shaped ring when the quartz cup and the quartz cover are closed, and simultaneously, the sealing of the device is realized by fastening the joint by using a hexagonal bolt and a hexagonal nut.
The quartz cup and the quartz cover of the smelting device are provided with cylindrical holes which are respectively used as an inlet and an outlet of protective gas when smelting alloy, so that the contact between the alloy and oxygen in the smelting process is avoided, and the oxygen content of the final alloy powder is reduced.
Furthermore, an aluminum silicate cotton layer with good heat insulation effect is adopted between the outer wall of the smelting ceramic crucible and the inner wall of the quartz tube, so that the quartz cup on the outer layer is prevented from being melted due to overhigh crucible temperature in the smelting process.
Further, the complete smelting device is placed in the induction heating coil, and alloy smelting can be rapidly achieved by adjusting the current.
Further, solid silica gel plugs with middle openings are plugged at two ends of a quartz tube in the atomizing device, and interference fit is adopted between the two plugs; the porous corundum pipes are inserted into the openings of the solid silica gel plugs and fastened by sealant, and the porous corundum pipes are fastened with the peripheral silica gel pipes by hoops, so that inflow and outflow of protective gas are realized.
Further, the gas flowmeter in the atomizing device is mechanically fixed on the supporting frame and connected between the gas cylinder and the gas inlet of the atomizing device, and the quantized gas flow is used for controlling the particle size ratio of atomized alloy powder.
Further, a coil is arranged on a supporting frame in the atomizing device and can be used for fixing an air atomizing crucible; the height of the support frame can be adjusted through bolts by the four stainless steel pipes with screw thread openings at one side; a groove is arranged in the middle for fixing the quartz tube.
The invention discloses a method for preparing powder by adopting the integrated induction smelting gas atomization powder preparation device, which comprises the following steps:
step S1, placing metal with a certain proportion into a smelting device for sealing, introducing protective gas, starting induction heating equipment for heating, closing the induction heating equipment and cooling to a fully solidified state when the alloy is in a fully molten state, repeating the steps for three times, cooling to room temperature, and closing the gas; taking out the master alloy and cutting;
s2, placing the alloy obtained in the step S1 into an aerosolization crucible, covering the aerosolization crucible cover, controlling the flow of gas entering the aerosolization crucible to protect the master alloy from oxidation in the melting process, and controlling the air pressure entering a corundum tube to enable the air pressure to reach an aerosolization pressure value; preferably, the gas flow rate into the aerosolizing crucible is controlled to be 0.1m 3 /h。
And step S3, electrifying the induction coil to heat, melting the master alloy in the gas atomization crucible, and increasing the gas flow entering the gas atomization crucible after 5-10S to realize atomization powder preparation.
According to the technical scheme, the flow of the gas can be changed to change the particle size distribution ratio of the prepared powder.
As a further improvement of the invention, semi-cylindrical quartz baffle plates are arranged in the quartz tube, and a space is arranged between the semi-cylindrical quartz baffle plates; the method for preparing the powder by gas atomization further comprises the following steps:
s4, after atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolization crucible, opening a silica gel plug on the right side of a quartz tube, pouring powder in the quartz tube into a standard sample sieve with the size larger than 800 meshes, and screening for more than 3 times to obtain the finest required powder; then taking down a semi-cylindrical quartz baffle plate farthest from the nozzle, pouring the powder into a 400-800-mesh standard sample sieve, and screening for more than 3 times to obtain finer required powder; and then sequentially taking down semi-cylindrical quartz baffle plates far from the nozzle opening, pouring the powder into standard sieves with corresponding meshes, and sequentially sieving the powder with larger spherical diameter. That is, the semi-cylindrical quartz baffle plates which are closer to the nozzle are sequentially removed, the powder is poured into a standard sieve with a corresponding smaller mesh number, and the powder with a larger spherical diameter is sequentially screened.
Furthermore, 4 semi-cylindrical quartz baffle plates are placed in a quartz tube in the atomizing device, and the primary screening of powder with different spherical diameters can be realized by adjusting the distance between the two quartz baffle plates.
Further, the semi-cylindrical quartz baffle plates are 140cm, 90cm, 50cm and 20cm from the opening of the nozzle in sequence.
Further, in the case of continuous atomization, the step S2 and the step S3 are repeated after the cover of the aerosolizing crucible is opened.
Compared with the prior art, the invention has the beneficial effects that:
firstly, by adopting the technical scheme of the invention, the device has the advantages of simple and light structure, suitability for carrying, long service life, low atomization pressure, convenient disassembly and assembly, small occupied area, low energy consumption and environmental protection by adopting induction heating, low manufacturing cost and good pulverizing effect, is very suitable for research and development experiments and exploration application, and reduces the cost in the experimental stage; the device realizes the preliminary screening of the powder with different spherical diameters, and realizes the integration of keeping the small crucible, the atomizing chamber and the collecting chamber of the molten alloy.
Secondly, by adopting the technical scheme of the invention, the device can be used only by introducing protective gas (such as nitrogen), and the use condition is looser compared with that of some equipment strictly ensured vacuum conditions; the device can control the particle size distribution of the prepared powder by adjusting the gas flow by adding a gas flowmeter.
Thirdly, by adopting the technical scheme of the invention, the device adopts the 80-degree conical nozzle, adopts the vertical atomization design, reduces the gas atomization pressure, enhances the dispersion of alloy liquid drops, avoids the blockage of the nozzle, ensures fine and uniform preparation powder, can improve the cooling speed, and can realize the efficient preparation of alloy powder and amorphous alloy powder.
Fourth, adopt the technical scheme of the invention, every part used in the device obtains conveniently, connect simply each other, trouble appears in any place in the application process, needn't professional, can debug or change of the relevant spare part very fast, greatly reduce the maintenance time, raise the powder process efficiency.
Drawings
Fig. 1 is a front view of an induction melting device in an integrated induction melting gas atomization pulverizing device according to the present invention.
Fig. 2 is a top view of an induction melting apparatus in an integrated induction melting aerosolized pulverizing apparatus according to the present invention.
Fig. 3 is a front view of an aerosolized powder process unit in an integrated induction melting aerosolized powder process unit according to the present invention.
Fig. 4 is a top view of an aerosolized powder process unit in an integrated induction melting aerosolized powder process unit according to the present invention.
Fig. 5 is a left side view of an aerosolized powder process unit in an integrated induction melting aerosolized powder process unit according to the present invention.
FIG. 6 is a cross-sectional view of a small crucible and a crucible cover in an aerosolized powder process unit in an integrated induction melting aerosolized powder process unit according to the present invention.
Fig. 7 is an SEM image of Cu-Sn alloy powder prepared by an integrated induction melting aerosolized pulverizing apparatus according to the present invention.
The reference numerals include: 1-hexagonal bolts, 2-hexagonal nuts, 3-smelting quartz covers, 4-smelting quartz cups, 5-O-shaped rings, 6-aluminum silicate cotton, 7-smelting crucibles, 8-gas atomization small crucible covers, 9-gas atomization small crucibles, 10-corundum pipes, 11-silica gel plugs, 12-quartz pipes, 13-supporting frames, 14-screws, 15-gas flow meters, 16-semi-cylindrical quartz baffle plates, 17-nozzles and 18-cylindrical gas inlets.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
An integrated induction smelting gas atomization powder making device comprises an induction smelting device and a gas atomization powder making device.
Referring to fig. 1-2, the induction smelting device comprises a smelting quartz cup 4 and a smelting quartz cover 3, wherein the smelting quartz cup 4 and the smelting quartz cover are hermetically combined through an O-shaped ring 5, a hexagonal bolt 1 and a hexagonal nut 2, a smelting crucible 7 is arranged in the smelting quartz cup 4 and is separated from the inner wall of the smelting quartz cup 4 through an aluminum silicate cotton 6, an induction coil is coated on the outer wall of the smelting quartz cup 4, and the alloy is heated and smelted.
Referring to fig. 3-5, the aerosolized powder making device comprises a supporting frame 13, wherein the height of the supporting frame 13 is adjusted by stretching and contracting an internal steel pipe and matching with a screw 14; the quartz tube 12 with the two ends plugged with the perforated solid silica gel plugs 11 by interference fit is arranged in a groove of the support frame and is used for collecting alloy powder; the corundum tube 10 is inserted into holes at two ends of the silica gel plug 11 and is fastened by sealant, and the corundum tube 10 can be connected with a rubber tube of an external gas cylinder to realize the circulation of protective gas; the gas flowmeter 15 is mechanically fixed on the support frame 13 and is used for adjusting the flow of the introduced gas; the gas atomization small crucible 9 is mechanically fixed in a coil at the left upper part of the supporting frame 13, a layer of induction coil is coated on the periphery of the gas atomization small crucible, the internal alloy is heated, the gas atomization small crucible cover 8 is connected with the gas atomization small crucible 9 in an interference fit manner, and a layer of plasticine is coated at the joint in practical application, so that good air tightness is ensured; the bottom nozzle 17 of the gas atomization small crucible 9 is inserted into the opening at the left end of the quartz tube 12, and the vertical atomization is realized by ensuring that the axis of the crucible is vertical to the axis of the quartz tube 12; a semi-cylindrical quartz baffle 16 is placed at intervals inside the quartz tube 12 to achieve preliminary screening of powders of different spherical diameters.
The small gas atomization crucible 9 in the gas atomization powder preparation device is provided with a cylindrical gas inlet 18 connected with an external gas cylinder, and protective gas is introduced in the atomization process; as shown in FIG. 6, the nozzle 17 at the bottom of the aerosolizing small crucible 9 is of 80℃conical design. The angle of the nozzle 17 is also compared, when the angle is 85 degrees, the residence time of the molten metal in the nozzle is uncontrollable, the gas pressure introduced into the nozzle 17 after melting is not completely applied and flows out of the nozzle quickly, so that the sphericity of the prepared powder is poor and cannot meet the requirements, when the angle is 75 degrees, the contact area between the molten metal and the gas above the same volume is increased, the pressure of the applied gas is reduced, the residence time of the molten metal in the nozzle is increased, the risk of oxidization is increased, and meanwhile, the molten metal needs to be introduced into an atomization chamber by relatively large gas flow, so that the production investment is increased, and the atomization effect and efficiency are not ideal. When the angle is 80 DEG, molten metal can stay in the nozzle 17 for a period of time due to the comprehensive actions of surface tension, gas pressure and self gravity, and when the gas flow rate introduced into the nozzle 17 is increased, the molten metal can quickly flow into an atomizing chamber for atomizing, so that the practical application is well satisfied, the bottom of the gas atomizing small crucible 9 is compactly connected with a circular through hole on one side of a quartz tube, the axis of the gas atomizing small crucible 9 is ensured to be perpendicular to the axis of the quartz tube 12, and vertical atomization is realized, and the purpose of enabling atomized powder to perform a flat throwing motion is realized, so that spherical powder with larger particle size is closer to the nozzle 17 and spherical powder with smaller particle size is farther from the nozzle 17, and preliminary screening of the powder is realized; the gas atomization small crucible 9 is provided with a crucible cover which is in interference fit with the crucible, a layer of plasticine is coated at the matched joint, and a circular ring is arranged at the upper part of the crucible cover for convenient taking; the gas atomization small crucible 9 and the supporting frame coil are mechanically fixed, and the periphery is only provided with an induction coil for melting alloy.
As shown in fig. 1 to 6, the working principle and the using method of the integrated induction smelting gas atomization powder making device are as follows:
step S1: putting a metal (100 g) with a certain proportion into a smelting crucible 7, screwing a hexagonal nut 2, and introducing Ar gas or N into a smelting quartz cup 4 2 The air outlet of the smelting quartz cup 4 is connected with an external water tank through a tetrafluoro pipe so as to ensure better tightness. The induction heating equipment is started, the induction heating equipment is closed and cooled to a fully solidified state when the alloy is in a fully molten state, the process is repeated three times, the alloy is cooled to room temperature, the gas is closed, and the master alloy is taken out and cut to be within 10 multiplied by 20 mm.
Step S2: the screw 14 is unscrewed, the small hole formed in the quartz tube 12 is tightly contacted with the nozzle 17 of the aerosolizing small crucible 9 by adjusting the height of the supporting frame 13, the solid silica gel plug 11 is rotated to align the hole of the porous corundum tube 10 with the outlet of the nozzle 17 of the aerosolizing small crucible 9, the solid silica gel plug 11 is firmly adhered to the quartz tube 12 by using an adhesive tape, and the solid silica gel plug which is perforated and is connected with the porous corundum tube in an interference fit in the hole is also firmly adhered to the quartz tube 12 by using the adhesive tape.
Step S3: placing a small piece of cut master alloy into an aerosolizing small crucible 9, covering the aerosolizing small crucible with an aerosolizing small crucible cover 8, compacting by an iron wire, and controlling the flow rate of gas entering the aerosolizing small crucible 9 to be 0.1m by a gas flowmeter 15 3 And/h, controlling the air pressure entering the porous corundum tube 10 to reach an air atomization pressure value through an air pressure valve.
Step S4: the induction heating switch is turned on, the master alloy is melted in the gas atomization small crucible 9, the surface tension is large, molten metal cannot flow out of the nozzle 17 of the gas atomization small crucible 9 immediately, and the gas flow entering the gas atomization small crucible 9 is increased immediately after 5-10 s, so that atomization powder preparation is realized.
If continuous atomization is required, the two steps of the step S3 and the step S4 are repeated after the gas atomization small crucible cover 8 is opened.
After atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolized small crucible 9, opening a right solid silica gel plug 11, pouring powder in a quartz tube 12 into a standard sample sieve with larger mesh number (more than 800 meshes), and screening for more than 3 times to obtain the finest required powder; then taking off a semi-cylindrical quartz baffle plate farthest from the atomizing nozzle 17, pouring the powder into a standard sample sieve (400-800 meshes) with a slightly larger mesh number, and screening for more than 3 times to obtain finer required powder; and then sequentially taking down semi-cylindrical quartz baffle plates which are closer to the nozzle, pouring the powder into a standard sieve with a corresponding smaller mesh number, and sequentially sieving the powder with a larger spherical diameter.
Example 2
The apparatus and method of example 1 were used to prepare elemental Sn metal powders. Pure Sn was cut to within 10 x 20 x mm dimensions. As shown in fig. 1 to 6, the following steps are adopted:
step S1: as shown in fig. 1 to 6, the screw 14 is unscrewed, the small hole formed in the quartz tube 12 is tightly contacted with the nozzle 17 of the aerosolizing small crucible 9 by adjusting the height of the supporting frame 13, the solid silica gel plug 11 is rotated, the porous corundum tube 10 is made to be in air alignment with the outlet of the nozzle 17 of the aerosolizing small crucible 9, the solid silica gel plug 11 is firmly adhered to the quartz tube 12 by using an adhesive tape, and the solid silica gel plug 11 which is perforated and is connected with the porous corundum tube in an interference fit in the hole is also firmly adhered to the quartz tube 12 by using an adhesive tape.
Step S2: placing a small block of cut Sn into an aerosolizing small crucible 9, covering the aerosolizing small crucible with an aerosolizing small crucible cover 8, compacting by an iron wire, and controlling the flow rate of the gas entering the aerosolizing small crucible 9 to be 0.1m by a gas flowmeter 15 3 And/h, controlling the air pressure entering the porous corundum tube 10 to reach an air atomization pressure value of 0.15 MPa through an air pressure valve.
Step S3: when the induction heating switch is turned on, sn is melted in the small aerosolizing crucible 9, the surface tension is larger, molten metal does not flow out of the nozzle 17 of the small aerosolizing crucible 9 immediately, and after 5 s, the flow rate of gas entering the small aerosolizing crucible 9 is increased to 0.5 m immediately 3 And/h, atomizing and pulverizing.
Continuously atomizing, and repeating the steps S2-S3 after opening the gas atomization small crucible cover 8.
After atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolized small crucible 9, opening a solid silica gel plug 11, pouring powder in a quartz tube 12 into a standard sample sieve with larger mesh number (more than 800 meshes), and screening for more than 3 times to obtain the finest required powder; then taking off a semi-cylindrical quartz baffle plate farthest from the atomizing nozzle 17, pouring the powder into a standard sample sieve (400-800 meshes) with a slightly larger mesh number, and screening for more than 3 times to obtain finer required powder; and sequentially taking down semi-cylindrical quartz baffle plates which are closer to the nozzle, pouring the powder into a standard sieve with a corresponding smaller mesh number, and sequentially sieving the powder with larger spherical diameter to obtain Sn powder with different spherical diameters.
Example 3
The apparatus and method of example 1 were used to prepare Cu-based cu—sn alloy powders, as shown in fig. 1 to 6, using the following steps:
step S1: 39.1g of pure Cu and 60.9g of pure Sn are placed in a smelting crucible 7, a hexagonal nut 2 is screwed, ar gas is introduced into a smelting quartz cup 4, and an air outlet of the smelting quartz cup 4 is connected with an external water tank through a tetrafluoro pipe so as to ensure better tightness. The induction heating equipment is started, the induction heating equipment is closed and cooled to a fully solidified state when the alloy is in a fully molten state, the process is repeated three times, the alloy is cooled to room temperature, the gas is closed, and the master alloy is taken out and cut to be within 10 multiplied by 20 mm.
Step S2: the screw 14 is unscrewed, the small hole formed in the quartz tube 12 is tightly contacted with the nozzle 17 of the aerosolizing small crucible 9 by adjusting the height of the supporting frame 13, the solid silica gel plug 11 is rotated, the porous corundum tube 10 is enabled to be in air alignment with the outlet of the nozzle 17 of the aerosolizing small crucible 9, the solid silica gel plug 11 is firmly adhered to the quartz tube 12 by using an adhesive tape, and the solid silica gel plug 11 which is perforated and is connected with the porous corundum tube in an interference fit in the hole is also firmly adhered to the quartz tube 12 by using the adhesive tape.
Step S3: placing a small piece of cut master alloy into an aerosolizing small crucible 9, covering the aerosolizing small crucible with an aerosolizing small crucible cover 8, compacting by an iron wire, and controlling the flow rate of gas entering the aerosolizing small crucible 9 to be 0.1m by a gas flowmeter 15 3 And/h, controlling the air pressure entering the porous corundum tube 10 to reach an air atomization pressure value of 0.15 MPa through an air pressure valve.
Step S4: the induction heating switch is started, the master alloy is melted in the gas atomization small crucible 9, the surface tension is larger, the molten metal does not flow out of the nozzle 17 of the gas atomization small crucible 9 immediately, and the gas flow entering the gas atomization small crucible 9 is increased to 0.5 m immediately after 5 s 3 And/h, atomizing and pulverizing.
Continuously atomizing, and repeating the two steps of the step S3 and the step S4 after opening the gas atomization small crucible cover 8.
After atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolized small crucible 9, opening a solid silica gel plug 11, pouring powder in a quartz tube 12 into a standard sample sieve with larger mesh number (more than 800 meshes), and screening for more than 3 times to obtain the finest required powder; then taking off a semi-cylindrical quartz baffle plate farthest from the atomizing nozzle 17, pouring the powder into a standard sample sieve (400-800 meshes) with a slightly larger mesh number, and screening for more than 3 times to obtain finer required powder; and sequentially taking down semi-cylindrical quartz baffle plates which are closer to the nozzle, pouring the powder into a standard sieve with a corresponding smaller mesh number, and sequentially sieving the powder with larger spherical diameters to obtain Cu-Sn alloy powder with different spherical diameters, wherein an SEM (scanning electron microscope) diagram is shown in FIG. 7, and the particle sizes of the powder are uniform as seen in FIG. 7.
Example 4
The apparatus and method of example 1 were used to prepare amorphous alloy powder, as shown in fig. 1 to 6, using the following steps:
step S1: 38.1g of pure Cu, 53.6g of pure Zr, 1.6g of pure Al and 5.8g of pure Y are placed in a smelting crucible 7, a hexagonal nut 2 is screwed, ar gas is introduced into a smelting quartz cup 4, and an air outlet of the smelting quartz cup 4 is connected with an external water tank through a tetrafluoro pipe so as to ensure better tightness. The induction heating equipment is started, the induction heating equipment is closed and cooled to a fully solidified state when the alloy is in a fully molten state, the process is repeated three times, the alloy is cooled to room temperature, the gas is closed, and the master alloy is taken out and cut to be within 10 multiplied by 20 mm.
Step S2: the screw 14 is unscrewed, the small hole formed in the quartz tube 12 is tightly contacted with the nozzle 17 of the aerosolizing small crucible 9 by adjusting the height of the supporting frame 13, the solid silica gel plug 11 is rotated, the porous corundum tube 10 is made to be in air alignment with the outlet of the nozzle 17 of the aerosolizing small crucible 9, the solid silica gel plug 11 is firmly adhered to the quartz tube 12 by using an adhesive tape, and the solid silica gel plug 11 which is perforated and is connected with the porous corundum tube in an interference fit in the hole is also firmly adhered to the quartz tube 12 by using the adhesive tape.
Step S3: placing a small piece of cut master alloy into an aerosolizing small crucible 9, covering the aerosolizing small crucible with an aerosolizing small crucible cover 8, compacting by an iron wire, and controlling the flow rate of gas entering the aerosolizing small crucible 9 to be 0.1m by a gas flowmeter 15 3 And/h, controlling the air pressure entering the porous corundum tube 10 to reach an air atomization pressure value of 0.15 MPa through an air pressure valve.
Step S4: the induction heating switch is started, the master alloy is melted in the gas atomization small crucible 9, the surface tension is larger, the molten metal does not flow out of the nozzle 17 of the gas atomization small crucible 9 immediately, and the gas flow entering the gas atomization small crucible 9 is increased to 0.5 m immediately after 5 s 3 And/h, atomizing and pulverizing.
Continuously atomizing, and repeating the two steps of the step S3 and the step S4 after opening the gas atomization small crucible cover 8.
After atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolized small crucible 9, opening a solid silica gel plug 11, pouring powder in a quartz tube 12 into a standard sample sieve with larger mesh number (more than 800 meshes), and screening for more than 3 times to obtain the finest required powder; then taking off a semi-cylindrical quartz baffle plate farthest from the atomizing nozzle 17, pouring the powder into a standard sample sieve (400-800 meshes) with a slightly larger mesh number, and screening for more than 3 times to obtain finer required powder; sequentially removing semicylindrical quartz baffle plates which are closer to the nozzle, pouring the powder into a standard sieve with a corresponding smaller mesh number, and sequentially sieving the powder with larger spherical diameter to obtain Cu with different spherical diameters 46 Zr 45 A l7 Y 5 Amorphous alloy powder.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.

Claims (7)

1. An integral type induction melting gas atomization powder process device which characterized in that: the device comprises an aerosolization powder preparation device, wherein the aerosolization powder preparation device comprises a support frame and an aerosolization crucible, a quartz tube used for collecting alloy powder is arranged on the support frame, and one end of the quartz tube is connected with a corundum tube which is filled with protective gas; the support frame is provided with an induction coil, the gas atomization crucible is arranged in the induction coil, the bottom of the gas atomization crucible is provided with a nozzle, and the nozzle faces the inside of the quartz tube; the axis of the nozzle of the gas atomization crucible is perpendicular to the axis of the quartz tube; the opening of the corundum tube faces to the outlet of the nozzle; the opening end of the quartz tube is sealed by a plug; the gas atomization crucible is provided with a gas inlet connected with an external gas cylinder; the nozzle is of a reverse cone structure, and the angle of the cone angle of the nozzle is 80 degrees; the corundum pipe is connected with the gas cylinder through a pneumatic valve; the gas atomization crucible is connected with an external gas cylinder through a gas flowmeter.
2. The integrated induction melting aerosolized pulverizing apparatus of claim 1, wherein: and at least two semi-cylindrical quartz baffle plates are arranged in the quartz tube.
3. The integrated induction melting aerosolized pulverizing apparatus of claim 2, wherein: 4 semi-cylindrical quartz baffle plates are arranged in the quartz tube, and the primary screening of the powder with different spherical diameters can be realized by adjusting the distance between the two quartz baffle plates.
4. The integrated induction melting aerosolized pulverizing apparatus of claim 1, wherein: the corundum tube is a porous corundum tube; the mouth of the quartz tube is provided with a punching solid silica gel plug, and the punching solid silica gel plug is in interference fit with the quartz tube.
5. The integrated induction melting aerosolization pulverizing apparatus of any one of claims 1-4, wherein: the device comprises a smelting device, wherein the smelting device is arranged in induction heating equipment; the smelting device comprises a first smelting container and a smelting container cover, and a second smelting container is arranged in the first smelting container; the melting container cover is provided with a protective gas inlet and a protective gas outlet; a heat insulation layer is arranged between the first smelting container and the second smelting container, and the heat insulation layer is made of aluminum silicate cotton.
6. A method for making powder by gas atomization by adopting the integrated induction smelting gas atomization powder making device as defined in any one of claims 1-5, which is characterized in that: the method comprises the following steps:
step S1, placing metal with a certain proportion into a smelting device for sealing, introducing protective gas, starting induction heating equipment for heating, closing the induction heating equipment and cooling to a fully solidified state when the alloy is in a fully molten state, repeating the steps for three times, cooling to room temperature, and closing the gas; taking out the master alloy and cutting;
s2, placing the alloy obtained in the step S1 into an aerosolization crucible, covering the aerosolization crucible cover, controlling the flow of gas entering the aerosolization crucible to protect the master alloy from oxidization in the process of melting, and controlling the pressure of the gas entering a corundum tube to enable the gas to reach an aerosolization pressure value;
and step S3, electrifying the induction coil to heat, melting the master alloy in the gas atomization crucible, and increasing the gas flow entering the gas atomization crucible after 5-10S to realize atomization powder preparation.
7. The aerosolized milling process of claim 6, wherein: semi-cylindrical quartz baffle plates are arranged in the quartz tube, and a space is reserved between the semi-cylindrical quartz baffle plates; the method for preparing the powder by gas atomization further comprises the following steps:
s4, after atomization is finished, closing an induction heating switch, closing gas, taking out an aerosolizing crucible, opening a silica gel plug on the right side of a quartz tube, pouring powder in the quartz tube into a standard sample sieve with the size larger than 800 meshes, and screening for more than 3 times to obtain required powder; then taking down a semi-cylindrical quartz baffle plate farthest from the nozzle, pouring the powder into a 400-800-mesh standard sample sieve, and screening for more than 3 times to obtain the required powder; and then sequentially taking down semi-cylindrical quartz baffle plates far from the nozzle opening, pouring the powder into standard sieves with corresponding meshes, and sequentially sieving the powder with larger spherical diameter.
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