CN113600822A - Equipment and method for preparing cold storage material spherical particles - Google Patents

Equipment and method for preparing cold storage material spherical particles Download PDF

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Publication number
CN113600822A
CN113600822A CN202110836301.8A CN202110836301A CN113600822A CN 113600822 A CN113600822 A CN 113600822A CN 202110836301 A CN202110836301 A CN 202110836301A CN 113600822 A CN113600822 A CN 113600822A
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China
Prior art keywords
storage material
cold storage
spherical particles
preparing
laser
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CN202110836301.8A
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Chinese (zh)
Inventor
翁子清
金霞
刘平
石磊
金莹
张腾辉
史金光
王彩霞
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Zhejiang Asia General Soldering & Brazing Material Co ltd
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Zhejiang Asia General Soldering & Brazing Material Co ltd
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Priority to CN202110836301.8A priority Critical patent/CN113600822A/en
Publication of CN113600822A publication Critical patent/CN113600822A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/10Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force

Abstract

The invention discloses a device and a method for preparing cold storage material spherical particles. The laser is positioned above the turntable and on one side of the rotating shaft of the turntable; when the particles are prepared, the surface of the cold storage material base material of the rotary disc is melted through the laser, and meanwhile, the rotary disc is driven by the driving motor to drive the cold storage material to horizontally rotate, so that the required spherical cold storage material particles are finally obtained. According to the cold storage material spherical particle preparation equipment and the cold storage material spherical particle preparation method with the optimized design, the cold storage material base material absorbs the high-energy laser beam to be locally and rapidly melted to form a small molten pool, is thrown out to form small liquid drops under the action of centrifugal force, is rapidly cooled to form spherical particles under the action of surface tension, and is used for preparing the needed cold storage material particles, and the cold storage material particles are high in sphericity, concentrated in particle size distribution and controllable in impurity content.

Description

Equipment and method for preparing cold storage material spherical particles
Technical Field
The invention relates to the technical field of cold storage material spherical particle preparation, in particular to cold storage material spherical particle preparation equipment and a cold storage material spherical particle preparation method.
Background
The low temperature technology, as a key technology supporting the development of science and technology, is closely linked with the subjects of physics, machinery, chemical engineering, electronics and the like, and is gradually permeating into more scientific research and high-tech fields. Such as cryogenic materials science, cryogenic physics, cryogenic electronics, cryogenic medicine, gas industry, and aerospace technologies, among others. In various low-temperature refrigeration technologies, a small cold storage type gas refrigerator which has a refrigeration temperature range of 4-20K and generally takes helium as a circulating working medium is widely applied to the low-temperature field due to the characteristics of reliable performance, simple structure, high thermal efficiency and the like, wherein a cold storage material is applied to a cold storage device of the low-temperature refrigerator, and the working principle of the small cold storage type gas refrigerator is that the small cold storage type gas refrigerator is used as an energy storage device and exchanges heat with the working medium in the refrigeration cycle process to store cold. Therefore, the energy accumulator can be ensured to operate efficiently only if the specific heat capacity of the cold storage material is obviously greater than that of the circulating working medium, so that the aim of refrigeration is fulfilled.
The commonly used cold storage materials mainly include intermetallic compounds, oxides, hydrides, and the like composed of rare earth metals. A relatively common cold-storage rare earth intermetallic material considered to be of practical value is Er3Ni、ErNi、ErNi2、ErNi、DyNi2、ErCo2、HoCu、HoCu2And the like. In practical applications of the regenerator material, while ensuring the highest possible filling rate of the regenerator material, the regenerator material should have a large surface area and a regular shape to reduce the flow resistance of the refrigerant in the regenerator, so that the above material is generally processed into spherical particles with a particle size in the range of 154-500 μm. However, the above magnetic cold storage material has a problem that it is difficult to form and process, and researchers in various countries are searching for the materialIs a method suitable for industrial production. Related documents report that Er-Ni and HoCu2 spherical powder is prepared by Blancao, Drangyi and the like of Beijing science and technology university by adopting a rotating disc centrifugal atomization method, and a better effect is obtained preliminarily. The centrifugal atomization of the rotating disc refers to that: the metal liquid flow is collided on a disk rotating at high speed, is smashed by the disk rotating at high speed, is atomized into liquid drops and is rapidly cooled into powder. The method has the following defects: 1) the rotating disc is made of a material with a higher melting point than that of the prepared metal, and is generally suitable for preparing tin-based alloy with a lower melting point (200-500 ℃), while most of magnetic cold storage materials have a higher melting point (generally > 900 ℃), and at the high temperature, the rotating disc can be corroded, softened and melted and is difficult to continuously produce. 2) When the rotating disc atomizes, the metal liquid needs higher superheat degree, and other impurities are inevitably introduced in the smelting process to pollute metal materials. 3) The rare earth has different burning loss phenomena in the alloy rare earth smelting process, the alloy component proportion is difficult to be accurately controlled, and the literature' magnetic cold storage material HoCu2The atomization forming research also mentions that the burning loss phenomenon of the rare earth metal Ho exists. 4) The recovery rate of the spherical particles with the particle size of 500 mu m prepared by the rotary disc centrifugal atomization method is 61.81%, wherein the spherical particles with the particle size of 500 mu m prepared by the rotary disc centrifugal atomization method are non-spherical particles with the particle size of 300 mu m. The quality and yield of the powder are to be further improved.
In addition, a few documents report that the cold storage material particles are prepared by adopting an ultrahigh rotating speed plasma rotating electrode method. The method needs to process the cold accumulation material into a rod-shaped electrode in advance, heat the surface of the rod-shaped electrode by a plasma source to melt and form liquid drops, and rotate the electrode at a high speed to throw out and form cold accumulation material particles. On the one hand, however, since most of the cold storage materials are rare earth intermetallic compounds, the materials are brittle, so that the rod-shaped electrode is difficult to manufacture in a metal machining process; on the other hand, the bar electrode inevitably has vibration, self gravity torque, internal thermal stress and other influence effects in the working process, so that the bar is brittle and broken, and stable and continuous production is not facilitated.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides equipment and a method for preparing cold storage material spherical particles.
The invention provides a cold storage material spherical particle preparation device, which comprises: the device comprises a shell, a base, a turntable, a driving motor and a laser;
the pedestal mounting is in the shell, and the carousel is rotatable to be installed on the base, and driving motor is connected with the carousel and is used for driving carousel horizontal rotation, is equipped with the position that holds that is used for holding cold-storage material substrate on the carousel, and the laser instrument is located the carousel top and is located pivot one side of carousel, and the laser instrument is used for melting hold cold-storage material substrate on the position.
Preferably, a closed preparation cavity is formed inside the shell, an inert gas inlet is formed in the side wall of the closed preparation cavity, and the base and the turntable are located in the closed preparation cavity.
Preferably, still include the cold-storage material substrate, the carousel middle part is equipped with the location axle of vertical setting, is equipped with on the cold-storage material substrate with location axle complex locating hole, the epaxial fastener that is used for fixing the cold-storage material substrate on the carousel that is equipped with of location.
Preferably, the cool storage material base material has a disk structure arranged coaxially with the positioning shaft.
Preferably, a plurality of cold storage material base materials are arranged on the accommodating position in a stacked mode from top to bottom.
Preferably, the surface of the rotating disk is provided with a high-temperature ceramic gasket, and the accommodating part is positioned on the high-temperature ceramic gasket.
The invention also provides a preparation method of the cold storage material spherical particles, which is realized by the cold storage material spherical particle preparation equipment.
Preferably, the cool storage material substrate is fixed on a turntable, the turntable is driven to horizontally rotate by a driving motor, and meanwhile, the surface of the cool storage material substrate is melted by a laser, so that the needed cool storage material particles are finally obtained.
Preferably, an inert gas is previously introduced into the closed preparation chamber.
Preferably, the particle size of the obtained cold storage material spherical particles is controlled by adjusting the beam cross-sectional area of the laser and the rotating speed of the driving motor.
The invention provides equipment and a method for preparing cold storage material spherical particles. The laser is positioned above the turntable and on one side of the rotating shaft of the turntable; when the particles are prepared, the surface of the cold storage material base material of the rotary disc is melted through the laser, and meanwhile, the rotary disc is driven by the driving motor to drive the cold storage material to horizontally rotate, so that the required spherical cold storage material particles are finally obtained. According to the cold storage material spherical particle preparation equipment and the cold storage material spherical particle preparation method with the optimized design, the cold storage material base material absorbs the high-energy laser beam to be locally and rapidly melted to form a small molten pool, is thrown out to form small liquid drops under the action of centrifugal force, is rapidly cooled to form spherical particles under the action of surface tension, and is used for preparing the needed cold storage material particles, and the cold storage material particles are high in sphericity, concentrated in particle size distribution and controllable in impurity content.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing cold storage material spherical particles according to the present invention.
FIG. 2 shows a HoCu prepared by the equipment and method for preparing cold storage material spherical particles provided by the invention2Scanning electron microscope images of spherical particles.
Detailed Description
As shown in fig. 1 and 2, fig. 1 is a schematic structural view of an apparatus for preparing cold storage material spherical particles according to the present invention, and fig. 2 is a schematic structural view of a HoCu prepared by the apparatus and the method for preparing cold storage material spherical particles according to the present invention2Scanning electron microscope images of spherical particles.
Because the cold storage material has the characteristic of high melting point, in the process of preparation by a rotating disc centrifugal atomization method, the metal liquid needs higher superheat degree when the rotating disc is atomized, so that the requirement on the material of the rotating disc is higher, otherwise, other impurities are inevitably introduced in the smelting process to pollute finally prepared material particles.
In order to avoid the above problems, referring to fig. 1, the present invention provides a cold storage material spherical particle manufacturing apparatus, including: the device comprises a shell 1, a base 2, a turntable 3, a driving motor 4 and a laser 5;
the lateral wall of shell 1 is equipped with the inert gas import, and base 2 installs in shell 1, and 3 rotatable installations of carousel are on base 2, and driving motor 4 is connected with carousel 3 and is used for driving 3 horizontal rotations of carousel, is equipped with the position that holds that is used for holding cold-storage material substrate 7 on the carousel 3, and laser 5 is located 3 tops of carousel and is located carousel 3 pivot one side, and laser 5 is used for melting hold cold-storage material substrate 7 on the position.
In the equipment for preparing the spherical particles of the cold storage material provided by the embodiment, the cold storage material which can be used for preparation is Er3Ni、ErNi、ErNi2、ErNi、DyNi2、ErCo2、HoCu、HoCu2And the like.
In order to explain the specific preparation process of the cold storage material spherical particle preparation apparatus in this embodiment in detail, this embodiment also provides a method for preparing cold storage material spherical particles, which is implemented by the cold storage material spherical particle preparation apparatus described above.
In a specific preparation mode, the cold storage material base material 7 is fixed on the rotary table 3, the rotary table 3 is driven to horizontally rotate by the driving motor 4, meanwhile, the surface of the cold storage material base material 7 is melted by the laser 5, and finally, cold storage material particles thrown from the rotary table 3 are obtained around the rotary table 3. In the processing process, the cold storage material absorbs laser energy and is locally and rapidly melted, and high-temperature liquid drops are directly and rotationally thrown out of the cold storage material base material under the action of centrifugal force under the rotation driving of the turntable and are rapidly cooled into spherical particles under the action of surface tension.
During preparation, a high-power laser can be used as an energy source. In a specific control mode, the area where the cold storage material is melted is controlled through the beam cross-sectional area of the laser 5, and the driving motor 4 is matched with a proper rotating speed, so that spherical particles with concentrated particle size distribution can be obtained, and the high yield of the required particle size particles is ensured. Specifically, the smaller the beam cross-sectional area of the laser, the larger the rotation speed of the drive motor, the smaller the particle diameter of the obtained spherical particles, and conversely, the larger the particle diameter of the spherical particles.
In the embodiment, the equipment and the method for preparing the spherical particles of the cold storage material are provided, the side wall of the shell is provided with an inert gas inlet, the turntable is rotatably arranged on the base, the turntable is provided with a containing position for containing a base material of the cold storage material, and the laser is positioned above the turntable and on one side of a rotating shaft of the turntable; when the particles are prepared, the surface of the cold storage material base material of the rotary disc is melted through the laser, and meanwhile, the rotary disc is driven by the driving motor to drive the cold storage material to horizontally rotate, so that the required spherical cold storage material particles are finally obtained. According to the cold storage material spherical particle preparation equipment and the cold storage material spherical particle preparation method with the optimized design, the cold storage material base material absorbs the high-energy laser beam to be locally and rapidly melted to form a small molten pool, is thrown out to form small liquid drops under the action of centrifugal force, is rapidly cooled to form spherical particles under the action of surface tension, and is used for preparing the needed cold storage material particles, and the cold storage material particles are high in sphericity, concentrated in particle size distribution and controllable in impurity content.
In order to avoid the pollution of impurities in the air to the molten cold storage material, in the specific design process of the shell, a closed preparation cavity is formed inside the shell 1, an inert gas inlet is formed in the side wall of the closed preparation cavity, and the base 2 and the rotary disc 3 are located in the closed preparation cavity.
Correspondingly, before preparation, inert gas is led into the closed preparation cavity through the inert gas inlet in advance, and the cold storage material is protected by the inert gas in the preparation process, so that other impurities can be effectively prevented from being introduced.
Compared with the ultrahigh-speed plasma rotating electrode method, the method for preparing the spherical particles of the cold storage material can meet the preparation requirement without special processing of the base material of the cold storage material.
In order to facilitate the fixation of the cold storage material base material, in a specific fixation mode of the cold storage material base material, a positioning shaft 31 which is vertically arranged is arranged in the middle of the rotary table 3, a positioning hole which is matched with the positioning shaft 31 is arranged on the cold storage material base material 7, and a fastener 6 which is used for fixing the cold storage material base material 7 on the rotary table 3 is arranged on the positioning shaft 31; specifically, the fastener can adopt the nut with location axle screw-thread fit, the cold-storage material substrate dismouting of being convenient for.
In the specific structural design of the cool storage material substrate, the cool storage material substrate 7 may be made into an integral cylindrical structure. Preferably, the cool storage material base material 7 may also adopt a disk structure coaxially arranged with the positioning shaft 31, so as to facilitate the fixing of the base material and ensure a continuous and stable preparation process.
Accordingly, when installed, a plurality of cool storage material base materials 7 may be stacked and arranged in order from the top to the bottom on the housing position.
In order to ensure the service life of the rotary table, in a specific design mode of the rotary table, the surface of the rotary table 3 is provided with a high-temperature ceramic gasket 8, and the accommodating position is positioned on the high-temperature ceramic gasket 8. Preferably, the turntable 3 may be made of high-strength alloy steel, and the high-temperature ceramic gasket 8 may be made of alumina, zirconia, or the like.
To explain the apparatus and method for preparing the cold storage material spherical particles of the present embodiment in detail, the following is HoCu2The preparation process of the material is taken as an example.
First, three disk-shaped HoCu are placed2The substrate is mounted to the turntable and is secured to the turntable by fasteners 6. Then, the inside of the housing is evacuated and inert gas is filled into the housing. During preparation, the turntable 3 is driven to rotate horizontally by the driving motor 4, the surface of the cold storage material base material 7 is melted by the laser 5, the rotating speed of the turntable is adjusted, the linear speed of a laser beam irradiating a melting area is kept at 6m/s, the diameter of a laser spot is 1mm, the laser power is 14kW, and HoCu is finally obtained by small liquid drops obtained by laser melting under the action of centrifugal force and surface tension2Particles of the material. The powder obtained is sieved by adopting standard sample sieves with the particle size of 150 mu m and 500 mu m, and the yield of the powder in the section is measured to be 84.6 percent and is greatly improved compared with 61.81 percent of the yield of the atomized powder of the flywheel disc. As can be seen from FIG. 2, the obtained HoCu2The sphericity of the particles is better, the surface is smooth, and the size of the spherical particles is more centralized. In addition, the powder particle size distribution is mainly 150-350 μm as shown by the scale of the picture, which shows that the particle size obtained in this example is uniform.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (10)

1. A cold storage material spherical particle preparation equipment is characterized by comprising: the device comprises a shell (1), a base (2), a turntable (3), a driving motor (4) and a laser (5);
base (2) are installed in shell (1), and carousel (3) is rotatable to be installed on base (2), and driving motor (4) are connected with carousel (3) and are used for driving carousel (3) horizontal rotation, are equipped with the position that holds that is used for holding cold-storage material substrate (7) on carousel (3), and laser instrument (5) are located carousel (3) top and are located pivot one side of carousel (3), and laser instrument (5) are used for melting hold cold-storage material substrate (7) on the position.
2. The apparatus for preparing cold storage material spherical particles according to claim 1, wherein a closed preparation chamber is formed inside the housing (1), the side wall of the closed preparation chamber is provided with an inert gas inlet, and the base (2) and the turntable (3) are positioned in the closed preparation chamber.
3. The equipment for preparing the cold storage material spherical particles according to claim 1, further comprising a cold storage material base material (7), wherein a positioning shaft (31) is vertically arranged in the middle of the rotary table (3), a positioning hole matched with the positioning shaft (31) is arranged on the cold storage material base material (7), and a fastening piece (6) used for fixing the cold storage material base material (7) on the rotary table (3) is arranged on the positioning shaft (31).
4. The apparatus for preparing cold storage material spherical particles according to claim 3, wherein the cold storage material base material (7) has a disk structure arranged coaxially with the positioning shaft (31).
5. The apparatus for preparing cold storage material spherical particles according to claim 4, wherein a plurality of cold storage material base materials (7) are arranged on the receiving position in a stacked manner from top to bottom.
6. The apparatus for preparing cold storage material spherical particles according to claim 1, wherein the surface of the rotary table (3) is provided with a high temperature ceramic gasket (8), and the receiving position is located on the high temperature ceramic gasket (8).
7. A method for preparing cold storage material spherical particles, which is characterized by being realized by the cold storage material spherical particle preparation device according to any one of claims 1 to 6.
8. The method for preparing cold storage material spherical particles according to claim 7, characterized in that the cold storage material substrate (7) is fixed on the turntable (3), the turntable (3) is driven to rotate horizontally by the driving motor (4), and the laser (5) is used for melting the surface of the cold storage material substrate (7) to finally obtain the required cold storage material particles.
9. The method for preparing cold storage material spherical particles according to claim 8, wherein an inert gas is previously introduced into the closed preparation chamber.
10. The method for preparing cold storage material spherical particles according to claim 8 or 9, wherein the particle diameter of the obtained cold storage material spherical particles is controlled by adjusting the beam cross-sectional area of the laser (5) and the rotation speed of the driving motor (4).
CN202110836301.8A 2021-07-23 2021-07-23 Equipment and method for preparing cold storage material spherical particles Pending CN113600822A (en)

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Citations (9)

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GB1294950A (en) * 1969-11-14 1972-11-01
CN2085689U (en) * 1990-12-20 1991-10-02 吉林工业大学 Device for preparation of ultramicron metallic powder by laser illumination
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CN108453264A (en) * 2018-05-22 2018-08-28 航星利华(北京)科技有限公司 A kind of method and device preparing metal powder
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CN2085689U (en) * 1990-12-20 1991-10-02 吉林工业大学 Device for preparation of ultramicron metallic powder by laser illumination
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