CN114260458A - Device and method for preparing superfine high-purity spherical magnesium powder - Google Patents
Device and method for preparing superfine high-purity spherical magnesium powder Download PDFInfo
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Abstract
A superfine high-purity spherical magnesium powder preparation device and method, the device includes gas cylinder, gas storage device, gas mass flowmeter, evaporation gasifier, particle condenser, cyclone dust collector, gas filter and gas cooler connected sequentially; under the action of high-purity inert gas, metal magnesium vapor generated by the evaporation gasification furnace is transferred to a particle condenser along the gas direction, magnesium powder with specific size and shape is formed in a quick suspension condensation mode, and the generated magnesium powder is collected in a cyclone dust collector; argon used in the whole powder making process is purified by a gas filter and then recycled, and a large amount of argon is firstly injected to discharge residual air only when a powder making system is started; solves the technical problems of large particle size, wide particle size distribution range, high impurity content, low sphericity and the like of the existing magnesium powder preparation method, and the introduced high-purity inert gas can be recycled.
Description
Technical Field
The invention relates to the technical field of metal powder preparation, in particular to a device and a method for preparing superfine high-purity spherical magnesium powder.
Background
The metal magnesium powder has the excellent performances of low density, strong reducibility, good biocompatibility and the like, and has the characteristics of flammability and explosiveness, capability of generating dazzling white light during combustion, capability of releasing a large amount of heat and the like, so that the metal magnesium powder is widely applied to the fields of metallurgical reduction, biological medical treatment, energy chemical industry, aerospace, military industry and the like. In the traditional industrial fields of steel making industry, nonferrous metal casting and the like, magnesium powder is often used as a desulfurizing agent, a deoxidizing agent, a reducing agent and the like, the requirements on performance indexes such as the particle size, the particle morphology and the like of the magnesium powder are not high, and in order to avoid the problem of impurity introduction caused by poor-quality magnesium powder, the quality of reduced metal is further improved, and the purity of the metal magnesium powder needs to be improved from the source. In high-end special fields such as aviation, aerospace, navigation, war industry and the like, the high-quality magnesium powder has an important strategic position which is difficult to replace. In order to better satisfy the application of magnesium powder in water-jet engine, bait agent, ignition powder, solid rocket propellant and the like, a new powder preparation technology needs to be developed to obtain superfine magnesium powder with small particle size and narrow distribution. The particle size of the magnesium powder is required to be less than 45 μm, the finer the magnesium powder is, and special requirements on the particle morphology, the active magnesium content and the like of the magnesium powder are also required. In the biomedical field, magnesium powder is used as a powder raw material for powder bed fusion forming (PBF) technology, and the technology has high requirements on powder materials, such as a narrow particle size distribution range, high particle purity, high density, high sphericity, no defects such as air hole inclusion, good fluidity and plasticity, and the like, wherein the smaller particle size distribution range can improve the utilization rate of the powder.
At present, the technical methods for preparing magnesium powder at home and abroad mainly comprise a cutting method, a high-energy ball milling method, an atomization method, a hydrogen plasma direct current arc method and the like, and the existing preparation technology cannot meet the requirements of the fields of metallurgical reduction, biological medical treatment, energy chemical industry, aerospace, military industry and the like on high-quality magnesium powder.
The cutting method is to mechanically cut a large magnesium ingot by adopting physical modes such as cutting, milling, eddy current and the like, the obtained magnesium powder has irregular shape, large particle size and wide distribution range, and impurities are easily introduced in the preparation process.
The high-energy ball milling method is to put a small amount of millimeter-sized magnesium powder and steel milling balls into a ball mill for long-time milling under the protection of inert atmosphere, and by adopting the method, the magnesium powder with relatively fine particle size can be obtained by prolonging the milling time, but because metal magnesium has good ductility, most of magnesium particles are adhered to the milling balls and the wall of the container, so that the milling efficiency is low. As reported in the first publication (Fahimpoor V, Sadrnezhaad S K. magnesium nanopowder for hydrogen adsorption and ammonium perchlorate decomposition [ J ] Materials Letters,2012,85: 128-. The obtained ball-milled sample is a mixture of NaCl and Mg particles, and residual NaCl cannot be completely removed by using a saturated KOH solution, and even magnesium oxide and magnesium hydroxide are generated.
The atomization method for preparing the magnesium powder is an advanced powder preparation technology which is commercially applied at present, but the particle size distribution range of the magnesium powder prepared by the atomization method is wider and is 25-830 mu m, and a step-by-step screening treatment process is required to obtain a magnesium powder product with small particle size and narrow distribution.
The hydrogen plasma DC arc process powder production is that under the vacuum condition, argon mixed gas mixed with H2 or N2 is introduced into an evaporation chamber, metal raw materials are melted and evaporated through DC arc, and the condensation of metal vapor is mainly controlled through inflation pressure and electric power. The method can prepare submicron or even nanoscale magnesium powder, but the prepared magnesium powder mainly takes hexagonal flakes as main materials, the sphericity rate is low, relatively obvious agglomeration and connection phenomena exist among particles, and industrial batch production is difficult to realize. Such as Liu T, Zhang Y, Li X.precursors and characteristics of Ti hydrides and Mg ultra components by hydrogen plasma-metal reaction [ J]Scripta Materialia,2003,48(4): 397-402.) reports Liu et al at 0.1MPa, 100L/min of mixed gas flow (50% Ar + 50% H)2) The prepared magnesium ultrafine particles have the particle size distribution range of 100-2000 nm, the average particle size of 905nm, spherical and hexagonal flaky shapes, and the prepared magnesium ultrafine particles have serious agglomeration and connection phenomena.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a device and a method for preparing superfine high-purity spherical magnesium powder, which realize the rapid suspension condensation of the magnesium powder in an inert gas transmission mode, and the prepared magnesium powder has the characteristics of small particle size, narrow distribution, high sphericity rate and high purity; meanwhile, the method has the advantages of simple preparation process, short preparation time, low energy consumption and low cost, and can solve the problems of uneven particle size distribution, low purity, low sphericity rate and low production efficiency of the magnesium powder produced by the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a superfine high-purity spherical magnesium powder preparation device comprises a gas storage device 1 communicated with a gas cylinder 12, wherein the gas storage device 1 is communicated with the inlet end of an evaporation gasification furnace 3, a boat-shaped graphite crucible 5 is fixed at the temperature equalizing position of the evaporation gasification furnace 3, and a magnesium ingot raw material 4 is placed in the boat-shaped graphite crucible 5; the outlet end of the evaporation gasification furnace 3 is communicated with the inlet end of a particle condenser 6, and the outlet end of the particle condenser 6 is communicated with a powder collecting hopper 8.
The inlet pipeline at the bottom of the gas storage device 1 is sequentially provided with a centrifugal circulating fan 11, a gas cooler 10 and a gas filter 9, and the input end of the gas filter 9 is communicated with the gas output port at the top of the cyclone dust collector 7.
A gas mass flowmeter 2 is communicated between the gas storage device 1 and the evaporation gasification furnace 3.
The evaporation gasification furnace 3 is a horizontal tube furnace, and joints are arranged at two ends of the tube.
The magnesium ingot raw material refers to all forms of metal magnesium, including but not limited to industrial grade magnesium ingot, magnesium powder, and recycled magnesium products.
The particle condenser 6 is tubular, and the external cooling mode includes, but is not limited to, water cooling, ammonia cooling and liquid nitrogen cooling.
The preparation method of the superfine high-purity spherical magnesium powder based on the preparation device utilizes the evaporation-condensation principle, takes industrial magnesium ingots as raw materials, heats the magnesium ingots to an evaporation state in the environment of flowing inert gas at normal pressure, wraps magnesium vapor by the flowing high-purity inert gas to the area of the particle condenser 6 for suspension condensation, and then obtains the superfine high-purity spherical magnesium powder in the powder collecting hopper 8 below the cyclone dust collector 7.
The preparation method comprises the following specific steps:
step one, placing a magnesium raw material in a boat-shaped graphite crucible 5, and placing and fixing the boat-shaped graphite crucible 5 at the uniform temperature area of an evaporation gasification furnace 3;
step two, after the preparation device is connected, continuously introducing inert gas to remove residual air in the powder preparation device;
starting a heating power supply of the evaporation gasification furnace 3, setting the preset evaporation heating temperature to be 700-1300 ℃, adjusting the flow rate of inert gas to be 0.5-5000 LPM, and then preserving heat;
step four, a cooling device outside the particle condenser 6 is opened, so that the temperature of the particle condenser 6 is kept below 400 ℃; the evaporated magnesium vapor collides with inert gas molecules to lose energy, and the magnesium vapor is nucleated and grown in a suspension state to form superfine magnesium powder;
and step five, after the powder making process is finished, taking out the powder collecting hopper 8 below the cyclone dust collector 7, placing the powder collecting hopper 8 in a glove box for storage, finally obtaining high-purity superfine spherical magnesium powder, continuously feeding redundant high-purity inert gas in the cyclone dust collector 7 into a gas filter 9 to remove residual superfine magnesium powder particles, then cooling the magnesium powder by a gas cooler 10, and finally feeding the magnesium powder into the gas storage device 1 by a centrifugal circulating fan 11 to perform the next powder making circulating process.
The purity of the high-purity inert gas is 99.999 percent or more, and the gas types include all gases which do not react with magnesium vapor, including but not limited to argon, helium, neon, krypton, xenon and radon.
And the evaporation heating temperature in the third step is 1000-1300 ℃.
And the flow rate of the inert gas in the third step is 10-500 LPM.
And the heat preservation time in the third step depends on the quality of the raw materials, and is calculated according to the standard that the heat preservation time required by 200g of magnesium ingot raw materials is not less than 40 min.
The temperature of the four-particle condenser 6 in the step is kept at 200-400 ℃.
The invention has the beneficial effects that:
(1) the magnesium powder with different grain diameters is controllably prepared by adjusting the evaporation and gasification temperature and the flow of inert gas; the particle size of the magnesium powder is obviously smaller than that of the magnesium powder prepared by an atomization method, and the distribution range is narrower; the evaporation gasification mode can obtain high-purity magnesium powder without introducing foreign impurities.
(2) Greatly shortens the production period and can be rapidly applied in large scale.
(3) The magnesium powder prepared by the method has small particle size (D)50Less than 10 mu m, narrow particle size distribution range (Span less than 1.50), high purity (more than 99.9%), high sphericity (more than or equal to 95%), large specific surface area (more than 300 m)2Kg), etc.
(4) Simple equipment, simple method and lower cost.
Drawings
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention, in which arrows indicate the direction of gas flow.
FIG. 2 is a scanning electron microscope image of the morphology of the ultra-fine high-purity spherical magnesium powder prepared by the present invention.
FIG. 3 is a particle size distribution curve of the ultra-fine high-purity spherical magnesium powder prepared by the present invention.
FIG. 4 shows the result of X-ray energy spectrum analysis of the ultra-fine high-purity spherical magnesium powder produced by the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Referring to fig. 1, the device for preparing ultrafine high-purity spherical magnesium powder comprises a gas storage device 1 communicated with a gas cylinder 12, wherein the gas storage device 1 is communicated with the inlet (left) end of an evaporation gasification furnace 3 through a gas mass flowmeter 2, a boat-shaped graphite crucible 5 is fixed at the temperature equalizing position of the evaporation gasification furnace 3, and a magnesium ingot raw material 4 is placed in the boat-shaped graphite crucible 5; the outlet end (right) end of the evaporation gasification furnace 3 is communicated with the inlet (left) end of the particle condenser 6, and the outlet end (right) end of the particle condenser 6 is communicated with the powder collecting hopper 8.
The inlet pipeline at the bottom of the gas storage device 1 is sequentially provided with a centrifugal circulating fan 11, a gas cooler 10 and a gas filter 9, and the input end of the gas filter 9 is communicated with the gas output port at the top of the cyclone dust collector 7.
The evaporation gasification furnace 3 is a horizontal tube furnace, the furnace tube is made of 310S stainless steel, the outer diameter is 25mm, the wall thickness is 2mm, and two ends of the furnace tube are designed to be KF25 joints so as to be conveniently connected through KF25 hoops; the maximum heating temperature is 1200 ℃, the power is 3kW, the temperature is controlled by adopting a PID controller and the output of a silicon controlled rectifier, and the overtemperature alarm function is realized.
The boat-shaped graphite crucible 5 has a length of 100mm, an outer diameter of 20mm and a wall thickness of 2mm, is placed at a uniform temperature region inside the 310S stainless steel evaporation gasifier 3, and is provided with a positioning device to prevent the boat-shaped graphite crucible from being blown away from a set position by introduced flowing inert gas.
The industrial grade magnesium raw material is contained in a boat-shaped graphite crucible 5, and the magnesium ingot raw material refers to all forms of metal magnesium, including but not limited to industrial grade magnesium ingots, magnesium powder and recycled magnesium products.
The method is applicable to the preparation of a variety of high purity metal powders including, but not limited to, magnesium powder.
The particle condenser 6 is tubular and made of brass, and the cooling mode of the brass tube comprises but is not limited to water cooling, ammonia cooling, liquid nitrogen cooling and the like.
The gas storage device 1 is provided with a gas valve for regulating the gas flow, and the specific flow value of the high-purity inert gas can be monitored through the gas mass flow meter 2.
Based on the preparation method of the superfine high-purity spherical magnesium powder preparation device, by utilizing an evaporation-condensation principle, an industrial magnesium ingot is used as a raw material, the magnesium ingot is heated to an evaporation state in a normal-pressure flowing inert gas environment, magnesium vapor is wrapped by flowing high-purity inert gas to a particle condenser 6 area for rapid suspension condensation, namely the evaporated magnesium vapor and inert gas molecules collide to lose energy, and the magnesium vapor is nucleated and grown in a suspension state to form superfine magnesium powder; then, superfine high-purity spherical magnesium powder is obtained in a powder collecting hopper 8 below the cyclone dust collector 7, and the devices and the connection sequence of a powder making system refer to the attached figure 1.
The preparation method comprises the following specific steps:
firstly, placing a magnesium raw material in a boat-shaped graphite crucible 5, and placing and fixing the boat-shaped graphite crucible 5 at the uniform temperature area of an evaporation gasification furnace 3;
and step two, connecting a preparation device, and respectively connecting two ends of a stainless steel furnace pipe of the evaporation gasification furnace 3 with the gas mass flow meter 2 and the particle condenser 6 through KF25 joints. As shown in the attached figure 1, a gas cylinder 12, a gas storage device 1, a gas mass flowmeter 2, an evaporation gasification furnace 3, a particle condenser 6, a cyclone dust collector 7, a gas filter 9 and a gas cooler 10 are sequentially connected, and inert gas with the flow rate of 0.5LPM is introduced into one end of a connected device system for more than 5 minutes so as to remove residual air in the powder making device; then, the centrifugal circulating fan 11 is connected into the whole powder making system, so that the system forms a closed loop;
starting a heating power supply of the evaporation gasification furnace 3, setting the preset evaporation heating temperature to be 700-1500 ℃ (preferably 1000-1300 ℃), adjusting the flow rate of the inert gas to be 0.5-5000 LPM (preferably 10-500 LPM), wherein the heat preservation time depends on the quality of the raw materials, generally, the heat preservation time required by 120g of magnesium ingot raw materials is 40min, and the temperature rise rate is 15 ℃/min;
step four, opening a cooling device outside the particle condenser 6, so that the temperature of the particle condenser 6 is kept below 400 ℃ (preferably 200 ℃ - & 400 ℃);
and step five, after the powder making process is finished, taking out the powder collecting hopper 8 below the cyclone dust collector 7, placing the powder collecting hopper 8 in a glove box for storage, finally obtaining the superfine high-purity spherical magnesium powder, continuously feeding redundant high-purity inert gas in the cyclone dust collector 7 into a gas filter 9 to remove residual superfine magnesium powder particles, then cooling the superfine magnesium powder by a gas cooler 10, and finally feeding the superfine magnesium powder into the gas storage device 1 by a centrifugal circulating fan 11 for the next powder making circulating process.
The purity of the high-purity inert gas is 99.999 percent or more, and the gas types include all gases which do not react with magnesium vapor, including but not limited to argon, helium, neon, krypton, xenon, radon and the like.
Example one
Weighing 120g of magnesium ingot raw material, placing the magnesium ingot raw material in a boat-shaped graphite crucible 5, and placing and fixing the boat-shaped graphite crucible 5 at the uniform temperature area of the evaporation gasifier 3;
and step two, connecting two ends of a stainless steel furnace pipe of the evaporation gasification furnace 3 with the gas mass flow meter 2 and the particle condenser 6 respectively through KF25 joints. As shown in the attached figure 1, a gas cylinder 12, a gas storage device 1, a gas mass flow meter 2, an evaporation gasification furnace 3, a particle condenser 6, a cyclone dust collector 7, a gas filter 9 and a gas cooler 10 are sequentially connected, high-purity inert gas is introduced into one end of a connected device system for a proper time, and then a centrifugal circulating fan 11 is connected into the whole powder making system, so that the system forms a closed loop;
starting a heating power supply of the evaporation gasification furnace 3, setting the evaporation gasification temperature to 1000 ℃, the heat preservation time to 40min, the temperature rise rate to 15 ℃/min, and the flow rate of the circulating inert gas in the powder preparation system to 0.7 m/s;
step four, opening a cooling device outside the particle condenser 6, so that the temperature of the particle condenser 6 is kept at 200-400 ℃; the evaporated magnesium vapor collides with inert gas molecules to lose energy, and the magnesium vapor is nucleated and grown in a suspension state to form superfine magnesium powder;
and step five, after the powder making process is finished, taking out the powder collecting hopper 8 below the cyclone dust collector 7, and placing the powder collecting hopper 8 in a glove box for storage to finally obtain the superfine high-purity spherical magnesium powder.
As shown in FIGS. 2, 3 and 4, the magnesium powder obtained by the preparation device and method of the invention has a particle size distribution range of 4-12 μm, a median particle size D50 of 8.16 μm, a particle size Span of 1.25 and a specific surface area of 327.4m2In kg (FIG. 3). The magnesium powder product has good sphericity (figure 2) and almost no other impurity elements, and the X-ray energy spectrum analysis result (figure 4) shows that the magnesium content is 100%.
In the process of the invention, high-purity inert gas enters a gas storage device 1 from a gas cylinder, enters an evaporation gasification furnace 3 through a gas mass flow meter 2, magnesium vapor enriched above a boat-shaped graphite crucible 5 containing magnesium ingot raw materials is wrapped and carried to a particle condenser 6 for suspension condensation, the high-purity inert gas and superfine magnesium powder particles simultaneously enter a cyclone dust collector 7, the superfine magnesium powder particles are collected in a powder collecting hopper 8 positioned below the cyclone dust collector 7, the high-purity inert gas continuously enters a gas filter 9 to remove the residual superfine magnesium powder particles, then is cooled to a proper temperature through a gas cooler 10, finally enters the gas storage device 1 through a centrifugal circulating fan 11, and then is subjected to next circulating process to solve the problems of large particle size, wide particle size distribution range, high impurity content and powder milling of the existing magnesium powder preparation method, Low sphericity and the like, and the introduced high-purity inert gas can be recycled.
Claims (10)
1. A superfine high-purity spherical magnesium powder preparation device is characterized by comprising a gas storage device (1) communicated with a gas cylinder (12), wherein the gas storage device (1) is communicated with the inlet end of an evaporation gasification furnace (3), a boat-shaped graphite crucible (5) is fixed at the temperature equalizing position of the evaporation gasification furnace (3), and a magnesium ingot raw material (4) is placed in the boat-shaped graphite crucible (5); the outlet end of the evaporation gasification furnace (3) is communicated with the inlet end of the particle condenser (6), and the outlet end of the particle condenser (6) is communicated with the powder collecting hopper (8).
2. The apparatus for preparing ultra-fine high-purity spherical magnesium powder according to claim 1, wherein a centrifugal circulating fan (11), a gas cooler (10) and a gas filter (9) are sequentially arranged on the inlet pipeline at the bottom of the gas storage device (1), and the input end of the gas filter (9) is communicated with the gas output port at the top of the cyclone dust collector (7).
3. The apparatus for preparing ultra-fine high-purity spherical magnesium powder as claimed in claim 1, wherein a gas mass flow meter (2) is connected between the gas storage device (1) and the evaporation gasifier (3).
4. The apparatus for preparing ultra-fine high-purity spherical magnesium powder as claimed in claim 1, wherein said evaporation gasification furnace (3) is a horizontal tube furnace, and joints are designed at both ends of the tube.
5. The apparatus for preparing ultra-fine high-purity spherical magnesium powder as claimed in claim 1, wherein the magnesium ingot material refers to all forms of magnesium metal including but not limited to industrial grade magnesium ingot, magnesium powder, and recycled magnesium product.
6. The apparatus for preparing ultrafine high purity magnesium powder in spherical form as claimed in claim 1, wherein said particle condenser (6) is in the form of a tube, and the external cooling means includes, but is not limited to, water cooling, ammonia cooling, and liquid nitrogen cooling.
7. The method for preparing ultra-fine high-purity spherical magnesium powder based on the preparation device of claims 1 to 6 is characterized in that industrial magnesium ingots are used as raw materials, the magnesium ingots are heated to an evaporation state in an atmosphere of flowing inert gas at normal pressure by utilizing the evaporation-condensation principle, magnesium vapor is entrained by the flowing high-purity inert gas to the area of the particle condenser (6) for suspension condensation, and then ultra-fine high-purity spherical magnesium powder is obtained in a powder collecting hopper (8) below a cyclone dust collector (7).
8. The preparation method according to claim 7, comprising the following steps:
firstly, placing a magnesium raw material in a boat-shaped graphite crucible (5), and placing and fixing the boat-shaped graphite crucible (5) at the uniform temperature area of an evaporation gasification furnace (3);
step two, after the preparation device is connected, continuously introducing inert gas to remove residual air in the powder preparation device;
starting a heating power supply of the evaporation gasification furnace (3), setting the preset evaporation heating temperature to be 700-1500 ℃, adjusting the flow rate of inert gas to be 0.5-5000 LPM, and then preserving heat;
step four, a cooling device outside the particle condenser (6) is opened, so that the temperature of the particle condenser (6) is kept below 400 ℃; the evaporated magnesium vapor collides with inert gas molecules to lose energy, and the magnesium vapor is nucleated and grown in a suspension state to form superfine magnesium powder;
and step five, after the powder making process is finished, taking out a powder collecting hopper (8) below the cyclone dust collector (7), placing the powder collecting hopper (8) in a glove box for storage, finally obtaining high-purity superfine spherical magnesium powder, continuously feeding redundant high-purity inert gas in the cyclone dust collector (7) into a gas filter (9) to remove residual superfine magnesium powder particles, then cooling the gas through a gas cooler (10), and finally feeding the gas into a gas storage device (1) through a centrifugal circulating fan (11) to perform the next powder making circulating process.
9. The preparation method according to claim 7, comprising the following steps:
the purity of the high-purity inert gas is 99.999 percent or more, and the gas types include all gases which do not react with magnesium vapor, including but not limited to argon, helium, neon, krypton, xenon and radon.
10. The preparation method according to claim 7, comprising the following steps:
the evaporation heating temperature in the third step is 1000-1300 ℃;
the flow rate of the inert gas in the third step is 10-500 LPM;
the heat preservation time in the third step depends on the quality of the raw materials, and is calculated according to the standard that the heat preservation time required by 200g of magnesium ingot raw materials is not less than 40 min;
the temperature of the four-particle condenser (6) in the step is kept at 200-400 ℃.
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| CN115401206A (en) * | 2022-08-25 | 2022-11-29 | 昆明理工大学 | Equipment and method for preparing high-purity spherical magnesium and/or high-purity magnesium powder |
| CN115647354A (en) * | 2022-11-07 | 2023-01-31 | 郑州机械研究所有限公司 | Powdered zinc-cadmium brazing filler metal and preparation method and device thereof |
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