CN111590083B - Preparation method of spherical nanocrystalline alloy powder - Google Patents
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Abstract
The invention discloses a preparation method of spherical nanocrystalline alloy powder, which comprises the following steps: s1: melting the raw materials to obtain alloy melt; s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate; s3: the alloy powder intermediate enters a cooling zone for cooling to obtain spherical amorphous alloy powder; s4: and annealing the spherical amorphous alloy powder to obtain the spherical nanocrystalline alloy powder. The superfine, spherical and low-oxygen nanocrystalline powder is prepared by the preparation method.
Description
Technical Field
The invention belongs to the technical field of atomization powder preparation, and particularly relates to a method for preparing spherical nanocrystalline alloy powder by adopting an air atomization water cooling process.
Background
Atomization milling is a powder preparation process in which a rapidly moving atomizing medium (typically high pressure water or gas) is used to break up a metal or alloy liquid into fine droplets, followed by condensation into a solid powder. The shape of the powder obtained varies greatly, due to the method by which the powder is produced.
Along with the rapid layout, intelligent manufacturing and new energy automobile key support plan of 5G communication, nanocrystalline atomized powder becomes the soft magnetic material with the most competitive power of the molded inductor. The nanocrystalline magnetic powder prepared by the atomization method has better sphericity, is favorable for coating powder particles and has more excellent high-frequency application characteristics. The nanocrystalline magnetic powder has high saturation magnetic flux density, can reduce the volume of devices, and provides larger space for circuit design.
Nanocrystalline powders are generally obtained by preparing amorphous powders and then heat-treating the powders. Currently, the industrialized nanocrystalline powder preparation method in the market is to prepare the material into amorphous strips in advance, then mechanically crush or crush the amorphous strips by air flow, and then heat treat the amorphous strips to obtain nanocrystalline powder. The shape of the broken powder is sheet-shaped or block-shaped, has sharp angle protrusions, is unfavorable for insulating coating, and has thicker granularity.
With the development of high frequency and miniaturization of electronic devices, the market demands for soft magnetic powder with high magnetic permeability and low loss at high frequency are also becoming more and more demanding. Some manufacturers have increasingly higher requirements on the grain size, sphericity and the like of nanocrystalline powder, and D50 of the powder is required: 3 to 5 μm, which is difficult to achieve by the crushing method. Therefore, the atomization method for preparing spherical low-oxygen nanocrystalline powder becomes a key for solving the problem.
At present, there are two main ways of preparing nanocrystalline soft magnetic powder: (1) a belt crushing method; (2) atomization method. The material is firstly prepared into amorphous powder, and then the amorphous powder is treated by a proper heat treatment process, so that the nanocrystalline powder is obtained. The nanocrystalline powder prepared by adopting the amorphous strip crushing method is easy to puncture an insulating layer coated on the surface of the powder due to a plurality of powder edges, so that the market expansion of the nanocrystalline powder is limited. A photograph of the nanocrystalline powder produced by the ribbon crushing process is shown in fig. 1.
Disclosure of Invention
The invention aims to find a preparation method for preparing spherical low-oxygen nanocrystalline powder, which solves the requirements of high-permeability low-loss nanocrystalline powder at high frequency of electronic devices.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the first aspect of the invention provides a preparation method of spherical nanocrystalline alloy powder, which comprises the following steps:
s1: melting the raw materials to obtain alloy melt;
s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate;
s3: the alloy powder intermediate enters a cooling zone for cooling to obtain the spherical amorphous alloy powder;
s4: and annealing the spherical amorphous alloy powder to obtain the spherical nanocrystalline alloy.
In some embodiments, the components of the raw materials include, in mass percent: si:1-14%, B:7-15%, C: less than or equal to 4 percent, cu: less than or equal to 3 percent, nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and unavoidable impurities.
In some embodiments, the FeSiB-based alloy is NP01, NP02 or NP03 alloy;
the NP01 alloy comprises the following chemical components in percentage by mass: cu:1%, nb:3%, si:13.5%, B:9%, fe: the balance and unavoidable impurities;
the NP02 alloy comprises the following chemical components in percentage by mass: cu:1%, nb:1%, si:4%, B:9%, C:0.3%, fe: the balance and unavoidable impurities;
the NP03 alloy comprises the following chemical components in percentage by mass: cu:1.2%, si:2%, B:12%, P:2%, fe: the balance and unavoidable impurities.
In some embodiments, in step S1, the raw material is melted at a temperature 50 to 250 ℃ higher than the melting point of the raw material to obtain the alloy melt.
In some embodiments, in step S1, the raw material is melted at 150 to 200 ℃ above the melting point of the raw material to obtain the alloy melt.
In some embodiments, in the step S2, the atomizing gas pressure is 2 to 6Mpa during the atomizing treatment.
In some embodiments, the vacuum degree at the time of the atomization treatment is controlled to 10Pa or less.
In some embodiments, in step S2, the inert atomizing gas is nitrogen or argon.
In some embodiments, in step S3, the rate of cooling is 10 6 K/s or more.
In some embodiments, the cooling rate is 10 6 -10 7 K/s。
In some embodiments, in step S4, the soak temperature of the anneal is 400-700 ℃.
In some embodiments, the incubation time is 20 to 120 minutes.
In some embodiments, the annealing is performed in a reducing gas or an inert gas;
in some embodiments, the reducing gas is hydrogen or carbon monoxide; the inert gas is nitrogen or argon.
In some embodiments, the spherical amorphous alloy powder is prepared by an apparatus comprising:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
the liquid cooling device is positioned below the gas atomizer and arranged at the periphery of the gas flow nozzle of the gas atomizer, and is used for cooling the alloy powder intermediate after the gas atomizer is broken to form spherical amorphous alloy powder.
In some embodiments, the apparatus for preparing spherical amorphous alloy powder further comprises a catheter connecting a tundish containing the alloy melt and the aerosolizer;
in some embodiments, the catheter upper end communicates with the tundish.
In some embodiments, the catheter lower end seats against a corresponding socket of the aerosolizer.
In some embodiments, the inner cavity of the catheter is in an inverted cone shape from top to bottom, and the cone angle is 0-15 degrees;
in some embodiments, the lumen of the catheter transitions from a reverse taper to a cylindrical shape with a taper angle of 1-15 °.
In some embodiments, an air inlet pipe for introducing the atomizing gas into the gas atomizer is arranged on the side wall of the gas atomizer.
In some embodiments, an air flow nozzle for crushing the alloy melt is arranged around the alloy melt outlet at the lower part of the air atomizer;
in some embodiments, the air flow nozzles are arranged in a ring.
In some embodiments, the direction of the air flow ejected by the air flow nozzle forms an included angle of 40-50 degrees with the vertical direction.
In some embodiments, the liquid cooling device is annularly arranged at the periphery of the airflow nozzle and is used for forming an annular cooling area for cooling the alloy powder intermediate.
In some embodiments, the liquid cooling device is a cylindrical structure with double walls, and a cooling liquid outlet is arranged on the lower bottom surface of the liquid cooling device and is used for enabling cooling liquid to flow downwards to form a cooling liquid curtain, and the cooling liquid curtain forms an annular cooling zone for cooling the alloy powder intermediate.
In some embodiments, the cooling fluid is water.
In some embodiments, the liquid cooling device is a cylindrical structure having double walls, the space between the double walls being filled with a cooling liquid, and the hollow region of the cylindrical structure is an annular cooling region for cooling the alloy powder intermediate, more preferably the cooling liquid is liquid nitrogen.
In some embodiments, the liquid cooling device is secured to a lower bottom surface of the aerosolizer.
In some embodiments, a liquid inlet pipe for injecting cooling liquid into the liquid cooling device is arranged on the side wall of the liquid cooling device.
In a second aspect, the present invention provides a spherical nanocrystalline alloy powder produced according to the production method of the first aspect of the present invention.
In some embodiments, the spherical nanocrystalline powder has a particle size D50 of 5 to 30 μm.
In some embodiments, the spherical nanocrystalline powder has an oxygen content of 200-1000ppm.
The technical features of the preparation device according to the invention can be used in any possible combination.
The invention has the advantages that the method for preparing spherical low-oxygen amorphous powder is found by improving the atomizer structure, and the spherical nanocrystalline powder is prepared by heat treatment of the amorphous powder. The loss of the superfine, spherical and low-oxygen nanocrystalline powder is greatly reduced, and the nano-powder can be widely applied to the field of high-frequency and miniaturized electronic devices and has good market prospect.
Drawings
FIG. 1 is a photograph of nanocrystalline powder produced by a ribbon crushing process of the prior art.
Fig. 2 is a schematic structural diagram of a prior art spherical amorphous alloy powder preparation apparatus.
Fig. 3 is a schematic structural view of a spherical amorphous alloy powder preparation apparatus according to some embodiments of the present invention.
FIG. 4 is a schematic diagram showing the structure and the use state of the apparatus for preparing spherical amorphous alloy powder shown in FIG. 3.
FIG. 5 is an SEM photograph of amorphous alloy powder prepared in step (3) of example 1 of the present invention.
FIG. 6 is a comparison of XRD patterns of the alloy powder prepared in example 1 of the present invention, in which the lower curve is the XRD pattern of the alloy powder of step (3) and the upper curve is the XRD pattern of the alloy powder of step (4).
Fig. 7 is an SEM scanning electron micrograph of the alloy powder prepared in comparative example 1.
Fig. 8 is an XRD pattern of the alloy powder prepared in comparative example 1.
FIG. 9 is an SEM photograph of amorphous alloy powder prepared in step (3) of example 2 of the present invention.
FIG. 10 is an SEM photograph of the alloy powder prepared in the step (5) of example 2 of the present invention.
FIG. 11 is a comparison of XRD patterns of the alloy powder prepared in example 2 of the present invention, in which the lower curve is the XRD pattern of the alloy powder of step (3) and the upper curve is the XRD pattern of the alloy powder of step (4).
Fig. 12 is an SEM scanning electron micrograph of the alloy powder prepared in comparative example 2.
Fig. 13 is an XRD pattern of the alloy powder prepared in comparative example 2.
FIG. 14 is an SEM photograph of amorphous alloy powder prepared in step (3) of example 3 of the present invention.
FIG. 15 is a comparison of XRD patterns of the alloy powder prepared in example 3 of the present invention, wherein the lower curve is the XRD pattern of the alloy powder of step (3), and the upper curve is the XRD pattern of the alloy powder of step (4).
FIG. 16 is an SEM photograph of the alloy powder prepared in comparative example 3 of the present invention.
FIG. 17 is an XRD pattern of alloy powder prepared in comparative example 3 of the present invention.
The device comprises a 1-gas atomizer, a 2-gas inlet pipe, a 3-gas flow nozzle, a 4-liquid guide pipe, a 5-melt nozzle, a 6-water cooling device, a 7-water inlet pipe, an 8-alloy melt liquid flow, 9-sprayed atomized gas, a 10-cooling water curtain and 11-amorphous alloy powder.
The XRD patterns of fig. 6, 8, 10, 12, 14, 16 have an abscissa of 2θ (twice the incident angle of x-rays) and an ordinate of diffraction intensity.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
The nanocrystalline powder prepared by the prior tape crushing method has coarse powder granularity, usually D50 of tens to hundreds of micrometers, and more powder edges and corners, and is easy to puncture an insulating layer coated on the surface of the powder, thus limiting the expansion of the application of the nanocrystalline powder. The nano-crystal powder prepared by water atomization has poor sphericity and high oxygen content, and the oxygen content can reach about 2000 ppm. The sphericity and oxygen content of the powder are improved by the gas atomization process, but the difficulty of obtaining amorphous powder is increased, especially some powder particles with larger size are more difficult to form amorphous because the cooling speed of the powder is slow by the gas atomization process. The invention aims to solve the technical problem of finding an atomization powder preparation method which can obtain ultrafine, spherical and low-oxygen amorphous powder and obtain nanocrystalline powder by selecting a proper heat treatment process.
The invention relates to a preparation method of spherical nanocrystalline powder, which combines and optimizes the powder preparation modes of gas atomization and water atomization, so that the prepared powder has the advantages of low oxygen and spherical powder preparation by gas atomization, amorphous powder can be obtained by rapid cooling of water, and then the amorphous powder is subjected to heat treatment to obtain nanocrystalline powder. The granularity range D50 of the spherical nanocrystalline powder is 5-30 mu m, the oxygen content is less than 1000ppm, such as 200-1000ppm, the metal raw material is put into a vacuum medium frequency induction furnace for heating and melting, the temperature of molten steel is generally heated to 1300-1600 ℃ according to the material difference (the temperature is preferably 150-200 ℃ above the melting point of alloy), the vacuum degree is less than 10Pa, and the atomization pressure is 2-6 Mpa (the proper pressure is selected according to the granularity requirement). Through redesigning the atomizer structure, after the atomizer is improved, can make alloy solution pass through high-pressure gas and strike the breakage, the metal droplet forms spherical granule under the effect of surface tension, and the granule is cooled off fast through the cooling water curtain to obtain spherical, low oxygen amorphous powder. The method comprises the following specific steps: an annular water cooling device is added below the atomizer, and the annular water cooling device is positioned at the outer side of the nozzle. The alloy solution flows down through the liquid guide pipe at the bottom of the tundish, after the alloy solution is beaten and broken into small metal liquid drops by high-pressure gas, the cooling speed of the gas is far lower than that of water, so that the metal liquid drops form spherical powder particles under the action of surface tension, the powder particles are sprayed out through the water curtain of the annular water cooling device below the atomizer in the falling process, and the spherical particles are rapidly cooled to obtain amorphous powder. And (3) annealing the prepared spherical amorphous powder at the annealing temperature of 450-650 ℃ for 30-90 min in reducing or inert gas to obtain spherical nanocrystalline powder.
The prior device for preparing amorphous powder by an atomization method is shown in fig. 2, and comprises an atomizer 1, an air inlet pipe 2, an air flow nozzle 3, a liquid guide pipe 4 and a melt nozzle 5.
The spherical amorphous alloy powder preparation device provided by the invention is characterized in that the existing gas atomization equipment is subjected to simple and easy-to-implement structural transformation, alloy melt can be subjected to high-pressure gas striking and crushing, metal liquid drops form spherical particles under the action of surface tension, and the particles are rapidly cooled by a cooling area formed by a cooling liquid (water) curtain, so that spherical and low-oxygen amorphous powder is obtained. Referring to fig. 2 to 4, the preparation apparatus of the present invention includes an air atomizer 1 and a liquid cooling apparatus disposed below the air atomizer 1 and disposed at the periphery of an air flow nozzle of the air atomizer, and of course, the preparation apparatus of the present invention may further include a melting furnace for melting alloy, a tundish for holding alloy melt, a vacuum pump, an apparatus for supplying atomized gas, an apparatus for collecting powder, and the like for realizing atomized pulverization, and since these apparatuses are all conventional apparatuses for atomized pulverization, they will not be described in detail herein, and only the portions closely related to the realization of the object of the present invention will be described in detail below.
The gas atomizer 1 breaks up the alloy melt from the tundish using atomizing gas. The gas atomizer 1 used in the present invention may be a conventional apparatus used in the field of atomizing pulverization, and in the embodiment of the present invention, the gas atomizer 1 includes: the body is used for being inserted into a corresponding socket of the liquid guide pipe 4, is used for being connected with the air inlet pipe 2 of atomizing air, is used for spraying out the air flow nozzle 3 of atomizing air, the liquid guide pipe 4 is used for connecting a tundish filled with alloy melt and the air atomizer 1, the inner cavity of the liquid guide pipe 4 is in an inverted cone shape from top to bottom, the cone angle is 0-15 degrees, preferably, the inner cavity of the liquid guide pipe 4 is in a cylindrical shape in a transition mode from top to bottom from the inverted cone shape, the cone angle of the inverted cone is 1-15 degrees (such as 2 degrees, 5 degrees, 7 degrees, 10 degrees, 12 degrees and 14 degrees), and the cone structure can ensure that the alloy melt flow 8 has enough flow and pressure, so that the air atomization is facilitated. The direction of the air flow sprayed by the air flow nozzle 3 forms an included angle of 40-50 degrees (such as 41 degrees, 43 degrees, 45 degrees, 47 degrees and 49 degrees) with the vertical direction (namely the axial direction of the liquid guide tube) so as to ensure the atomizing powder making effect and granularity.
In the preferred embodiment of the invention, the upper end of the liquid guide pipe 4 is communicated with the tundish, the lower end part of the liquid guide pipe 4 is arranged at the corresponding socket of the gas atomizer 1, therefore, alloy melt can be sprayed out from the bottom spraying outlet of the liquid guide pipe 4 to form a downward alloy melt flow 8, the inner cavity of the liquid guide pipe 4 is transited from the reverse taper shape to the cylindrical shape from top to bottom, the taper angle of the reverse taper shape is 10 degrees, and the taper structure can ensure that the alloy melt flow 8 has enough flow and pressure, thereby being beneficial to gas atomization. The side wall of the gas atomizer 1 is provided with an air inlet pipe 2 for introducing atomizing gas into the gas atomizer 1, the lower part of the gas atomizer is provided with a plurality of gas flow nozzles 3 for crushing the alloy melt liquid flow 8 around an alloy melt outlet (namely, a bottom ejection port of the liquid guide pipe 4), the plurality of gas flow nozzles 3 are uniformly arranged on the lower bottom surface of the gas atomizer 1 and around the bottom ejection port of the liquid guide pipe 4, the plurality of gas flow nozzles 3 are annularly arranged, the direction of the gas flow ejected by the gas flow nozzles 3 is 45 degrees with the vertical direction (namely, the axial direction of the liquid guide pipe), the atomizing gas entering from the air inlet pipe 2 reaches the gas flow nozzles 3, and the alloy melt liquid flow is crushed by the atomizing gas 9 ejected by the nozzles.
The liquid cooling device is positioned below the gas atomizer 1 and arranged at the periphery of the gas flow nozzle 3 of the gas atomizer 1, and is used for cooling the alloy powder intermediate after the gas atomizer 1 is broken to form spherical amorphous alloy powder. The liquid cooling device of the present invention is any cooling device that can provide a sufficient cooling rate for the crushed alloy powder intermediate, such as: the cooling device can form a cooling area surrounded by cooling liquid sprayed from a cooling liquid outlet, the alloy powder intermediate just passes through the cooling area, the cooling liquid can be water, and the cooling device can be of a double-wall cylindrical structure with the lower bottom surface provided with the cooling liquid outlet in the circumferential direction; or the cooling device is made of good heat transfer material, the cooling device can be a cylindrical or quadrangular cylinder or a hexagonal cylinder and the like, the cylinder wall is double-layer hollow, the space between the double-layer walls is filled with cooling liquid such as liquid nitrogen and the like, the lower bottom surface of the cooling device is not provided with a cooling liquid outlet, and the area in the middle of the cylinder of the cylindrical cooling device is a cooling area for cooling the alloy powder intermediate. The first cooling device forming a cooling water curtain has a vertical height that is smaller than that of the second cooling device. The liquid cooling device is annularly arranged on the periphery of the air flow nozzle 3, and the upper end of the liquid cooling device can be fixed on the lower bottom surface of the air atomizer 1 or can be arranged independently of the air atomizer 1. Preferably, the wall surface is smooth or coated with a lubricious coating so that the powder particles do not adhere to the wall.
In a preferred embodiment of the present invention, the liquid cooling device is annularly disposed on the periphery of the air flow nozzle 3, the upper end of the liquid cooling device is fixed on the lower bottom surface of the air atomizer 1, the lower bottom surface of the liquid cooling device is provided with a cooling liquid outlet, and the cooling liquid adopts water, so the cooling device is also called a water cooling device 6, the water cooling device 6 further comprises a water inlet pipe 7 for water inlet, which is disposed on the side wall of the water cooling device 6, so as to supply cooling water to the inside of the water cooling device, the cooling water flows downwards from the cooling liquid outlet to form an annular cooling water curtain 10, and the inside of the cooling water curtain 10 is a cooling area for cooling the alloy powder intermediate to form amorphous alloy powder 11. According to the invention, an annular water cooling device 6 is added below the air atomizer, the annular water cooling device 6 is positioned at the outer side of the air flow nozzle 3, and cooling water can flow downwards or be sprayed out from the water cooling device 6, so that a cooling area surrounded by an annular water curtain is ensured to have proper temperature, and alloy small liquid drops passing through the cooling area are cooled to form amorphous powder. When the alloy melt is sprayed out through the spraying port at the bottom of the liquid guide pipe 4 and is beaten and broken into small metal liquid drops by high-pressure gas, the gas cooling speed is far lower than that of water, so that the metal liquid drops form spherical powder particles under the action of surface tension, the powder particles pass through the cooling water curtain 10 sprayed out by the annular water cooling device below the atomizer in the falling process, and the spherical particles are rapidly cooled to obtain amorphous alloy powder 11.
The spherical amorphous alloy powder preparation device is suitable for preparing various amorphous alloy powders, and is particularly suitable for preparing FeSiB amorphous alloy powders; preferably, the amorphous alloy powder comprises the following components in percentage by mass: si:1-14%, B:7-15%, C: less than or equal to 4 percent, cu: less than or equal to 3 percent, nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and unavoidable impurities; for example, the FeSiB amorphous alloy powder is NP01, NP02 or NP03 alloy powder; the NP01 alloy powder comprises the following chemical components in percentage by mass: cu:1%, nb:3%, si:13.5%, B:9%, fe: the balance and unavoidable impurities; the NP02 alloy comprises the following chemical components in percentage by mass: cu:1%, nb:1%, si:4%, B:9%, C:0.3%, fe: the balance and unavoidable impurities; the NP03 alloy comprises the following chemical components in percentage by mass: cu:1.2%, si:2%, B:12%, P:2%, fe: the balance and unavoidable impurities.
The invention also comprises an annealing furnace for annealing the spherical amorphous alloy powder prepared by the spherical amorphous alloy powder preparation device to form spherical nanocrystalline alloy powder. The annealing furnace of the present invention may be selected from conventional annealing furnaces in the field of alloy powder preparation.
The invention also provides a preparation method of the spherical nanocrystalline alloy powder, which comprises the following steps:
s1: heating and melting metal raw materials in a vacuum intermediate frequency induction furnace, wherein the temperature of molten steel is selected according to different materials; heating to 1300-1600 deg.c, preferably to 50-250 deg.c, and more preferably 150-200 deg.c higher than the melting point of the material, and vacuum degree below 10Pa (9 Pa, 7Pa, 6Pa, 1Pa, 0.1 Pa) to obtain molten alloy;
s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate;
preferably, during the atomization treatment, an appropriate atomization pressure is selected according to the granularity requirement, and the pressure of an atomization gas (namely, the spraying pressure of the gas for atomization) is 2-6 Mpa (such as 2.5Pa, 3Pa, 4Pa, 5Pa and 5.5 Pa); the vacuum degree during the atomization treatment is controlled to be less than 10Pa (such as 9Pa, 7Pa, 6Pa, 1Pa, and 0.1 Pa); the inert atomizing gas is nitrogen or argon.
S3: the alloy powder intermediate enters a cooling zone for cooling to obtain the spherical amorphous alloy powder; preferably the cooling rate is 10 6 K/s or more (e.g. 2 x 10 6 K/s、4*10 6 K/s、6*10 6 K/s、8*10 6 K/s、9*10 6 K/s、2*10 7 K/s、4*10 7 K/s、6*10 7 K/s、8*10 7 K/s、9*10 7 K/s); more preferably the cooling rate is 10 6 -10 7 K/s。
S4: annealing the spherical amorphous alloy powder, wherein the annealing temperature is 400-700 ℃ (such as 420 ℃, 460 ℃, 480 ℃, 500 ℃, 520 ℃, 540 ℃, 560 ℃, 580 ℃, 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃) and the spherical amorphous alloy powder is subjected to heat preservation in reducing or inert gas for 20-120 min (such as 40min, 60min, 80min and 100 min) to obtain the spherical nanocrystalline alloy powder.
The preparation method of the present invention is further described by the following examples, which all use the preparation apparatus of the present invention, wherein the direction of the air flow ejected from the air flow nozzle 3 forms 45 ° with the vertical direction (i.e. the axial direction of the catheter), the inner cavity of the catheter 4 transitions from the inverted cone shape to the cylindrical shape from top to bottom, the cone angle of the inverted cone shape is 10 °, the cooling liquid is water, and the liquid cooling apparatus can form a cooling water curtain.
Example 1
The NP01 nanocrystalline powder is prepared in this example, and the chemical components (according to mass percent) are: cu:1%, nb:3%, si:13.5%, B:9%, fe: the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) Heating the raw materials to 1325 ℃ under the atmosphere of 5Pa of vacuum degree to melt to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 5Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (i.e. the temperature of alloy melt in a tundish) is 1320 ℃, and the pressure of the atomization gas is 2.2MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 Obtaining amorphous alloy powder at a speed of K/s or above;
(4) And (3) annealing and preserving the heat of the amorphous alloy powder at 550 ℃ under the hydrogen atmosphere for 60min, and collecting the spherical nanocrystalline alloy powder.
The alloy powder prepared in the step (3) was observed by a Scanning Electron Microscope (SEM) and a photograph is shown in FIG. 5, from which it is understood that the alloy powder prepared by the method of the present invention has very good sphericity and a particle size D50: 28. Mu.m. The oxygen content of the alloy powder was 319ppm.
The alloy powder obtained in step (4) was tested for particle size D50 of 28 μm and oxygen content of 367ppm.
The XRD patterns of the alloy powders obtained in step (3) and step (4) were analyzed by X-ray diffraction, respectively, and as can be seen from fig. 6, the measured powder of step (3) has no significant diffraction peak, and the powder of step (4) has significant diffraction peak, and is a crystalline alloy powder.
Comparative example 1
This comparative example 1, in which the existing gas atomization apparatus was used for pulverizing, was identical to example 1 in both raw materials and the first two processes, and omitted the cooling step of step (3) and the annealing step of step (4). The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 7, the sphericity of the powder was deteriorated due to the decrease in cooling rate. The particle size D50 was 23. Mu.m, and the oxygen content was 613ppm.
XRD patterns were obtained by X-ray diffraction analysis, see figure 8. As can be seen from the figure, the alloy powder prepared in this comparative example has already exhibited diffraction peaks and crystallization of the powder is started.
Example 2:
the NP02 nanocrystalline alloy powder is prepared in the embodiment, and the chemical components (according to mass percent) are as follows: cu:1%, nb:1%, si:4%, B:9%, C:0.3%, fe: the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) Heating the raw materials to 1425 ℃ under the ambient atmosphere with the vacuum degree of 8Pa, and melting to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 8Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (namely the temperature of alloy melt in a tundish) is 1420 ℃, and the pressure of the atomization gas is 6MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 Obtaining amorphous alloy powder at a speed of K/s or above;
(4) And (3) annealing and preserving the heat of the amorphous alloy powder for 90 minutes at 450 ℃ in a hydrogen atmosphere, and collecting spherical nanocrystalline alloy powder.
(5) And carrying out air current classification treatment on the spherical nanocrystalline alloy powder to obtain alloy powder.
The alloy powder prepared in the step (3) was observed by a Scanning Electron Microscope (SEM), and the photograph was seen in FIG. 9, from which it is understood that the alloy powder prepared by the method of the present invention has very good sphericity and a particle size D50: 10. Mu.m. The oxygen content of the alloy powder was 503ppm.
The alloy powder obtained in the step (4) was tested to have a particle size D50 of 10 μm and an oxygen content of 931ppm.
The alloy powder obtained in the step (5) was observed by a Scanning Electron Microscope (SEM), and the photograph thereof was shown in FIG. 10, and the alloy powder obtained in the step (5) had a particle size D50 of 3. Mu.m.
The XRD patterns of the alloy powders obtained in step (3) and step (4) were analyzed by X-ray diffraction, respectively, and as can be seen from fig. 11, the measured powder of step (3) had no significant diffraction peak, and the powder of step (4) had significant diffraction peak, and was crystalline alloy powder.
Comparative example 2
In this comparative example 2, the existing gas atomization apparatus (i.e., without a liquid cooling device) was used for pulverizing, and the raw materials and the former two steps were the same as those in example 2, and the cooling step in step (3) and the annealing step in step (4) were omitted in this comparative example. The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 12, irregularly shaped particles in the powder significantly increased and sphericity deteriorated due to a decrease in cooling rate. The particle size D50 was 11. Mu.m, and the oxygen content was 762ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as can be seen from fig. 13, the alloy powder prepared in this comparative example had developed diffraction peaks and the powder started to crystallize.
Example 3:
the NP03 nanocrystalline alloy powder is prepared in the embodiment, and the chemical components (according to mass percent) are as follows: cu:1.2%, si:2%, B:12%, P:2%, fe: the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) Heating the raw materials to 1385 ℃ under the atmosphere of 3Pa of vacuum degree to melt to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 3Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (namely the temperature of alloy melt in a tundish) is 1380 ℃, and the pressure of the atomization gas is 3.6MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 Obtaining amorphous alloy powder at a speed of K/s or above;
(4) And (3) annealing and preserving the heat of the amorphous alloy powder for 30min at 650 ℃ in a hydrogen atmosphere, and collecting spherical nanocrystalline alloy powder.
As can be seen from the observation of the powder prepared in step (3) by a Scanning Electron Microscope (SEM), referring to FIG. 14, the alloy powder prepared by the method of the present invention has very good sphericity and a particle size D50: 17. Mu.m. The oxygen content of the alloy powder was 361ppm.
The alloy powder obtained in the step (4) has the granularity D50 of 17 mu m and the oxygen content of 502ppm.
The XRD patterns of the alloy powders obtained in step (3) and step (4) were analyzed by X-ray diffraction, respectively, and as can be seen from fig. 15, the measured powder of step (3) had no significant diffraction peak, and the powder of step (4) had significant diffraction peak, and was crystalline alloy powder.
Comparative example 3
This comparative example 3, in which the existing aerosolization apparatus was used for pulverizing, was identical to example 3 in both the raw material and the first two steps, and omitted the cooling step of step (3) and the annealing step of step (4). The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 16, irregularly shaped particles in the powder significantly increased and sphericity deteriorated due to a decrease in cooling rate. The particle size D50 was 18. Mu.m, and the oxygen content was 537ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as can be seen from fig. 17, the alloy powder prepared in this comparative example had developed diffraction peaks and the powder started to crystallize.
Knot (S)
The powder obtained in step (3) of examples 1 to 3 had no significant diffraction peak, and was amorphous alloy powder, and the powder in step (4) had significant diffraction peak, and was crystalline alloy powder. The powder obtained in comparative examples 1 to 3 had a significant diffraction peak, and crystallization occurred in the powder, and the nanocrystalline powder was usually prepared by first preparing amorphous powder, and then heat-treating the alloy obtained in comparative examples 1 to 3 to obtain nanocrystalline powder, without forming amorphous, with insufficient cooling rate, resulting in crystallization of the powder, and non-uniformity in crystal distribution. The application properties of this material are poor. Therefore, the atomization powder preparation method can obtain superfine, spherical and low-oxygen nanocrystalline powder.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.
Claims (13)
1. A preparation method of spherical nanocrystalline alloy powder, which is characterized by comprising the following steps:
s1: melting the raw materials to obtain alloy melt; the raw material is FeSiB alloy; the raw materials comprise the following components in percentage by mass: si:1-14%, B:7-15%, C: less than or equal to 4 percent, cu: less than or equal to 3 percent, nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and unavoidable impurities;
s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate; during atomization treatment, the pressure of atomization gas is 2-6 mpa; the vacuum degree during atomization treatment is controlled to be below 10 Pa;
s3: the alloy powder intermediate enters a cooling zone for cooling to obtain spherical amorphous alloy powder; the cooling rate is 10 6 K/s or more;
s4: annealing the spherical amorphous alloy powder, wherein the annealing temperature is 400-700 ℃; the heat preservation time is 20-120 min, and the spherical nanocrystalline alloy powder is obtained; the granularity D50 of the spherical nanocrystalline alloy powder is 5-30 mu m, and the oxygen content of the spherical nanocrystalline alloy powder is 200-1000ppm;
the spherical amorphous alloy powder is prepared by an apparatus comprising:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
the liquid cooling device is positioned below the gas atomizer and arranged at the periphery of the gas flow nozzle of the gas atomizer, and is used for cooling the alloy powder intermediate crushed by the gas atomizer to form spherical amorphous alloy powder; the liquid cooling device is annularly arranged at the periphery of the airflow nozzle and is used for forming an annular cooling area for cooling the alloy powder intermediate; the liquid cooling device is of a cylindrical structure with double walls, a cooling liquid outlet is formed in the lower bottom surface of the liquid cooling device and used for enabling cooling liquid to flow downwards to form a cooling liquid curtain, the cooling liquid curtain forms an annular cooling area for cooling the alloy powder intermediate, and the cooling liquid is water.
2. The method of claim 1, wherein the FeSiB-based alloy is NP01, NP02 or NP03 alloy; the NP01 alloy comprises the following chemical components in percentage by mass: cu:1%, nb:3%, si:13.5%, B:9%, fe: the balance and unavoidable impurities;
the NP02 alloy comprises the following chemical components in percentage by mass: cu:1%, nb:1%, si:4%, B:9%, C:0.3%, fe: the balance and unavoidable impurities;
the NP03 alloy comprises the following chemical components in percentage by mass: cu:1.2%, si:2%, B:12%, P:2%, fe: the balance and unavoidable impurities.
3. The method according to claim 1, wherein in step S1, the raw material is melted at a temperature 50 to 250 ℃ higher than the melting point of the raw material to obtain the alloy melt.
4. The method according to claim 3, wherein in step S1, the raw material is melted at 150 to 200 ℃ higher than the melting point of the raw material to obtain the alloy melt.
5. The method of claim 1, wherein in step S2, the inert atomizing gas is nitrogen or argon.
6. The method of claim 1, wherein in step S3, the cooling rate is 10 6 -10 7 K/s。
7. The method of claim 1, wherein the annealing is performed in a reducing gas or an inert gas; the reducing gas is hydrogen or carbon monoxide; the inert gas is nitrogen or argon.
8. The production method according to claim 1, wherein the production apparatus of the spherical amorphous alloy powder further comprises a liquid guide tube connecting a tundish containing the alloy melt and the gas atomizer.
9. The method of manufacture of claim 8, wherein the catheter upper end is in communication with the tundish; the lower end part of the liquid guide pipe is arranged on a corresponding socket of the air atomizer; the inner cavity of the catheter is in an inverted cone shape from top to bottom, and the cone angle is 0-15 degrees.
10. The method of claim 8, wherein the lumen of the catheter transitions from a reverse taper to a cylindrical shape with a taper angle of 1-15 °.
11. The production method according to claim 1, wherein an air inlet pipe for introducing the atomizing gas into the gas atomizer is provided on a side wall of the gas atomizer.
12. The production method according to claim 1, wherein an air flow nozzle for crushing the alloy melt is provided around the alloy melt outlet in the lower part of the air atomizer; the air flow nozzles are annularly arranged; the direction of the airflow sprayed by the airflow nozzle forms an included angle of 40-50 degrees with the vertical direction.
13. The method of claim 1, wherein the liquid cooling device is fixed to a lower bottom surface of the atomizer; the side wall of the liquid cooling device is provided with a liquid inlet pipe for injecting cooling liquid into the liquid cooling device.
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| CN112475307A (en) * | 2020-11-26 | 2021-03-12 | 成都慧磁电子材料有限公司 | Method for preparing metal material powder by gas atomization and metal powder atomization device |
| CN114147212A (en) * | 2020-11-30 | 2022-03-08 | 佛山市中研非晶科技股份有限公司 | Amorphous nanocrystalline atomized powder and preparation method thereof |
| CN113106358B (en) * | 2021-04-02 | 2022-08-12 | 天津大学 | Iron-based amorphous alloy/graphene wave-absorbing material and preparation method thereof |
| CN114653956A (en) * | 2022-03-24 | 2022-06-24 | 安徽大学绿色产业创新研究院 | Preparation method of spherical nanocrystalline magnetically soft alloy powder |
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