CN115647377B - Iron-nickel-molybdenum metal alloy powder and preparation device and method thereof, and magnetic powder core and preparation method thereof - Google Patents
Iron-nickel-molybdenum metal alloy powder and preparation device and method thereof, and magnetic powder core and preparation method thereof Download PDFInfo
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Abstract
The invention provides iron-nickel-molybdenum metal alloy powder and a preparation device and method thereof, and a magnetic powder core and a preparation method thereof. The preparation device and the preparation method of the invention use nitrogen as a medium, and set the switching time of the pulse electromagnetic valve through the PLC control system so as to input pulse type high-speed nitrogen flow to the circular seam nozzle component; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam arranged on a central horizontal annular plane of the inner annular cavity wall of the pulse type high-speed nitrogen flow to form a horizontal pulse type high-speed nitrogen flow spraying surface, and the molten metal flow is cut off to form rod-shaped iron-nickel-molybdenum metal alloy powder. The rod-shaped iron-nickel-molybdenum powder prepared by the method has a large axial-diameter ratio, can reduce demagnetization factors in the long axis direction of the powder, improves the effective magnetic permeability in the long axis direction of the powder, and realizes the improvement of the effective magnetic permeability of the finally prepared iron-nickel-molybdenum magnetic powder core. The rod-shaped iron-nickel-molybdenum alloy powder prepared by the method is combined with a conventional cladding pressing heat treatment process to prepare an iron-nickel-molybdenum metal magnetic powder core sample with the magnetic conductivity of more than 500.
Description
Technical Field
The invention relates to the technical field of alloy powder preparation, in particular to preparation of iron-nickel-molybdenum metal alloy powder, and particularly relates to iron-nickel-molybdenum metal alloy powder and a preparation device and method thereof, and a magnetic powder core and a preparation method thereof.
Background
Along with the development of high frequency, high power density and miniaturization of electronic components, higher and higher requirements are provided for the performance of the metal magnetic powder core, and the novel magnetic powder core has the characteristics of high saturation magnetic induction intensity, low loss, good temperature stability and the like. The iron-nickel-molybdenum metal magnetic powder core belongs to a high-end magnetic powder core, has the lowest loss and temperature coefficient, and is widely applied to the fields of military industry and high-end precision instruments. At present, the technical level of iron-nickel-molybdenum metal magnetic powder core manufacturers is uneven, the magnetic conductivity of iron-nickel-molybdenum products like those of magnetic powder cores in America abroad reaches 300, and the magnetic conductivity is obviously superior to that of iron-nickel-molybdenum products 160 of domestic manufacturers. The iron-nickel-molybdenum metal magnetic powder core is usually obtained by pressing and molding iron-nickel-molybdenum metal alloy powder, so the performance, the microscopic form, the particle size and the like of the iron-nickel-molybdenum metal alloy powder also determine the magnetic conductivity of the prepared iron-nickel-molybdenum metal magnetic powder core to a great extent.
Chinese patent publication No. CN107578873A discloses "a method for preparing an iron-nickel-molybdenum metal magnetic powder core with magnetic permeability μ = 400", in which a gas atomization method is first used to prepare iron-nickel-molybdenum metal alloy powder, and then 2 times of insulation coating treatment are performed to obtain iron-nickel-molybdenum core material magnetic powder with magnetic permeability near 400. Although the iron-nickel-molybdenum metal alloy powder prepared by adopting the gas atomization method is subjected to subsequent 2-time insulation coating treatment, a first phosphoric acid and chromate composite layer is generated on the surface of the powder prepared by gas atomization, so that the surface resistance is increased, and the insulativity of a magnetic core is improved; and then, a second coating layer is generated by adding an aluminate and water glass aqueous solution, so that the magnetic permeability of the finally pressed magnetic core can reach about 400. However, the shape of the iron-nickel-molybdenum alloy powder prepared by the gas atomization method in the scheme is a spherical or spheroidal structure, and the magnetic permeability of the magnetic powder core prepared from the spherical or spheroidal powder with a three-dimensional structure has the characteristic of anisotropy, so that the improvement of the magnetic permeability of the magnetic core prepared subsequently is limited.
Therefore, it is urgently needed to develop a method and an apparatus for preparing iron-nickel-molybdenum metal alloy powder with high yield and a rod-like two-dimensional structure, so as to improve the effective magnetic permeability of the iron-nickel-molybdenum magnetic powder core in the long axis direction of the rod-like structure.
Disclosure of Invention
The invention aims to provide iron-nickel-molybdenum metal alloy powder, a preparation device and a preparation method thereof, a magnetic powder core and a preparation method thereof, so as to prepare the iron-nickel-molybdenum metal alloy powder with high yield and a rod-shaped structure, and improve the effective magnetic conductivity of the rod-shaped structure of the iron-nickel-molybdenum magnetic powder core in the long axis direction.
In order to solve the technical problems, the invention adopts the following technical scheme:
in a first aspect, the invention provides a device for preparing iron-nickel-molybdenum metal alloy powder, which mainly comprises a smelting part and a powder making part, wherein the powder making part is provided with a first chamber surrounded by a first shell; the smelting part is provided with a second chamber enclosed by a second shell and the top of the first shell;
a smelting furnace is arranged in the second chamber, a tundish is fixedly arranged at the top of the first shell, and the tundish is used for receiving molten metal liquid poured by the smelting furnace; the tundish is of a hollow structure with openings at two ends, the bottom of the tundish is embedded in a first plate, the first plate is fixed at the top of the first shell, and the top of the first shell is provided with a first through hole with the same size as the outer diameter of the tundish; a plurality of through flow guide holes are equidistantly arranged on the first plate, the inlet end of each flow guide hole is provided with a first flow guide opening, the outlet end of each flow guide hole is provided with a second flow guide opening, and the inner diameter of each first flow guide opening is larger than that of each second flow guide opening; the tundish in the fixed state is aligned with the first through hole, so that the molten liquid poured in the tundish can flow into the first cavity through the flow guide hole;
the first cavity is internally provided with a circular seam nozzle assembly, the circular seam nozzle assembly is arranged below the corresponding diversion hole, the circular seam nozzle assembly is a circular pipe fitting which is formed by a hollow pipe and is provided with a hollow inner annular cavity, and the molten liquid flowing out of the diversion hole can fall into the range of the hollow inner annular cavity; the central horizontal ring plane of the inner ring cavity wall is provided with a jet circular seam, the circular ring pipe fitting is also provided with a first input port which is used for being connected with an external first nitrogen gas storage device, a connecting pipeline of the circular ring pipe fitting is provided with a pressure pump and a pulse electromagnetic valve, and the pulse electromagnetic valve is connected with a PLC control system and used for setting the switching time of the pulse electromagnetic valve so as to input pulse type high-speed nitrogen gas flow into a hollow pipe of the circular seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through the spraying annular seam to form a horizontal pulse type high-speed nitrogen flow spraying surface which is used for intercepting the continuous metal flow flowing out of the flow guide holes to prepare the iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure;
the bottom of the first shell of the powder making part is connected with a detachable discharging barrel for collecting the prepared iron-nickel-molybdenum alloy powder; the detachable charging basket is connected with a cooling device and used for cooling the prepared powder; the powder process portion still is equipped with first exhaust port, connects outside first exhaust duct for the nitrogen gas that the discharge let in. Preferably, the middle section of the first exhaust pipeline is provided with a dust removal cloth bag for adsorbing a small amount of fine particle powder wrapped in the discharged nitrogen. When the nitrogen dust removal device works, a small amount of fine particle powder wrapped by nitrogen gas upwards enters the nitrogen gas discharge pipe, the fine particle powder is adsorbed on the dust removal cloth bag, and the nitrogen gas is discharged from gaps of the dust removal cloth bag.
Furthermore, a groove is formed in the first plate, the bottom of the tundish is embedded in the groove, and the flow guide hole is formed in the groove; the middle bag is sleeved with a third plate, the third plate is provided with a second through hole which is consistent with the outer diameter of the middle bag, the third plate penetrates through the middle bag cover and is arranged on the first plate, the first plate extends outwards along the outer edge of the groove of the first plate to form an outer edge, the periphery of the third plate is provided with a plurality of first bolt holes, a plurality of second bolt holes which are coaxial with the first bolt holes are arranged at the corresponding positions of the top plate of the device body, and the third plate is fixed at the top of the first shell through fixing bolts.
Furthermore, the tundish is provided with a high-frequency induction heater for continuously heating the tundish during pouring, so that the phenomenon that the molten mass is not overheated enough and solidifies to block the tundish at the flow guide port is avoided.
Further, the air conditioner is provided with a fan,
the cooling device is a water-cooling circulating cooling device and comprises a buffer pool and a sedimentation pool; the bottom of a first shell of the powder making part is provided with filter cloth, a circulating water outlet is arranged at the position below the filter cloth on the first shell, and a circulating water inlet is arranged at the position above the filter cloth on one side of the first shell opposite to the circulating water outlet; a first motor is arranged on a connecting pipeline between the circulating water outlet and the buffer tank, a second motor is arranged on a connecting pipeline between the buffer tank and the sedimentation tank, and a third motor is arranged on a connecting pipeline between the sedimentation tank and the circulating water inlet; during operation, all put water in removable unloading bucket, buffer pool, the sedimentation tank, form the circulation water route and cool off the iron-nickel-molybdenum powder that makes. According to the invention, the filter cloth is arranged at the bottom of the first shell of the powder making part, so that on one hand, the buffer effect can be achieved, the powder is prevented from directly falling into the bottom of the detachable discharging barrel, and the rod-shaped powder is prevented from being broken; on the other hand, for filtering rod-like powders in circulating water.
Furthermore, a second exhaust port is arranged in a second chamber of the smelting part and connected with an external second exhaust pipeline, and a fourth motor is arranged on the second exhaust pipeline and used for exhausting and vacuumizing; the second chamber is also provided with a nitrogen gas input port which is connected with an external second nitrogen gas storage device and used for inputting nitrogen gas protection into the second chamber and enabling the molten liquid poured into the tundish to better flow into the powder making part from the flow guide holes under the gas pressure.
Furthermore, the annular seam-shaped nozzle assembly is fixed through a plurality of steel frames arranged on the inner wall of the device body. Preferably, the number of steel frames is 4.
Preferably, the width of the spray annular seam of the annular seam nozzle assembly is 0.1 to 0.2mm.
In a second aspect, the invention further provides a method for preparing iron-nickel-molybdenum metal alloy powder by using the preparation device, which specifically comprises the following steps:
(1) Feeding pure metals of iron, nickel and molybdenum into a smelting furnace according to a preset proportion, heating and smelting, continuing to heat after the pure metals of iron, nickel and molybdenum are changed into molten liquid metal liquid, overheating to 150-200 ℃, pouring into a tundish, and meanwhile, continuously heating the tundish by using a high-frequency induction heater;
(2) The molten liquid poured into the tundish flows out to a circumferential seam nozzle assembly below the molten liquid through a plurality of through flow guide holes arranged on a first plate at the bottom of the molten liquid, and the PLC control system is used for controlling the on-off time of a pulse electromagnetic valve arranged on a nitrogen input pipeline so as to input pulse type high-speed nitrogen flow to the circumferential seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam arranged on a central horizontal annular plane of the inner annular cavity wall of the pulse type high-speed nitrogen flow to form a horizontal pulse type high-speed nitrogen flow spraying surface, and the continuous metal flow flowing out of the flow guide holes is cut off to obtain iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure;
(3) Simultaneously, the powder that makes falls into in the removable bucket of unloading that holds water in powder process portion bottom, cools off through water-cooling circulation.
Further, the method comprises the steps of: (4) And after the molten liquid completely flows out of the diversion holes, emptying water in a detachable bucket at the bottom, putting the iron-nickel-molybdenum slurry covered on the filter cloth into a vacuum mixer, and drying at the temperature of 60-80 ℃ for 30-60min to obtain dry iron-nickel-molybdenum powder.
Further, the method comprises the steps of: (5) And placing the dried iron-nickel-molybdenum powder on a 300-mesh sieve in an ultrasonic sieving machine for sieving, wherein the 300-mesh sieve is qualified iron-nickel-molybdenum powder, the qualified iron-nickel-molybdenum powder enters a plastic barrel with a built-in woven bag through a soft rubber pipe connected with the ultrasonic sieving machine, and a foam layer with the thickness of 2-3cm is placed between the woven bag and the plastic barrel to play a role in buffering. The purpose of the 300 mesh sieve is to remove broken chip powder and obtain qualified rod-shaped powder. The foam layer is placed to the intermediate layer of braided bag and plastic drum can further prevent the rupture of bar-shaped powder.
Preferably, in the step (2), the switching time of the pulse electromagnetic valve is set to be 5ms and 10ms after nitrogen is introduced in every 15ms period, and the rod-shaped powder with a certain axial-diameter ratio is prepared by combining the inner diameter of the second diversion port at the outlet end of the diversion hole. Such as: the inner diameter of the first flow guide opening is 0.2-0.3 mm, and the inner diameter of the second flow guide opening is 0.05-0.1mm.
Furthermore, before heating and smelting, the fourth motor is started to exhaust the second chamber of the smelting part and vacuumize the second chamber to 20-50pa, then nitrogen is input into the second chamber through a nitrogen input port for protection, nitrogen is supplemented to 90-100Kpa, the input nitrogen can form certain pressure in the second chamber, a downward positive pressure is provided for the tundish, and therefore the molten liquid poured into the tundish can better flow into the powder making part from the flow guide holes. Because the aperture of the flow guide hole is smaller, and the upper part of the flow guide hole is wide and the lower part of the flow guide hole is narrow, the flow guide hole can better flow into the powder making part under the pressure action of nitrogen flushed from the nitrogen input port of the second cavity, and the problem of hole blockage can be avoided. After vacuum pumping, the quality of the product in the smelting process can be ensured under the nitrogen protection atmosphere.
The nitrogen medium is discharged upwards through a second exhaust port at the top of the powder making part.
In a third aspect, the invention further provides iron-nickel-molybdenum metal alloy powder prepared by the preparation device or the method, wherein the iron-nickel-molybdenum metal alloy powder has a rod-shaped micro morphology.
In a fourth aspect, the invention further provides a high-permeability iron-nickel-molybdenum magnetic powder core, wherein the high-permeability iron-nickel-molybdenum magnetic powder core is prepared from the iron-nickel-molybdenum metal alloy powder, and the permeability of the iron-nickel-molybdenum magnetic powder core can reach more than 500.
In a fifth aspect, the invention further provides a preparation method of the iron-nickel-molybdenum magnetic powder core with high magnetic permeability, which specifically comprises the following steps:
(1) Insulating and coating: putting the iron-nickel-molybdenum magnetic powder prepared by the device or the method into a coating solution for chemical film forming for 0.5 to 1h; the coating solution is formed by dissolving a coating agent in a coating solvent, the coating agent is a mixture of silicon dioxide, organic silicon and phosphoric acid, and the mass ratio of the silicon dioxide to the organic silicon to the phosphoric acid is 1:2:1; the coating solvent is absolute ethyl alcohol; the addition amount of the coating agent is 1 per mill to 5 per mill of the weight of the mixed magnetic powder; the adding amount of the coating solvent is 3-5% of the weight of the mixed magnetic powder;
(3) And (3) pressing and forming: adding 0.1-0.4 wt% of zinc stearate and 0.1-0.5 wt% of K resin into the insulated and coated magnetic powder, feeding the magnetic powder into a die cavity of a forming press under the pressure of 100-300T, and performing compression forming by ultrasonic vibration for 1-2s to obtain a blank magnetic core; the powder fed into the die cavity can ensure that the rod-shaped powder is laid in the die cavity in a full horizontal mode after ultrasonic vibration, and the phenomenon that the powder is crushed in the pressing forming process to influence the performance of the magnetic powder core is avoided.
(4) Annealing: placing the blank magnetic core in a vacuum sintering furnace, and annealing under the mixed gas of reducing atmosphere and inert atmosphere at the annealing temperature of 650-750 ℃ for 0.8-1.2h; the reducing atmosphere is H 2 The inert atmosphere is Ar or N 2 (ii) a The volume ratio of the reducing atmosphere to the inert atmosphere is 7-6:3-4;
(5) Impregnation treatment: adding the annealed blank magnetic core into an acetone solution containing epoxy resin with the mass percentage concentration of 0.8-1.2%, soaking for 30-60min, taking out, cleaning, and then baking at 80-120 ℃;
(6) Powder coating and sorting.
The invention has the beneficial effects that:
1. the preparation process of the iron-nickel-molybdenum alloy powder provided by the invention takes nitrogen as a medium, sets the switching time of a pulse electromagnetic valve through a PLC control system, and opens the electromagnetic valve in a pulse period to input pulse type high-speed nitrogen flow to a circular seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam arranged on a central horizontal annular plane of the inner annular cavity wall of the pulse type high-speed nitrogen flow to form a horizontal pulse type high-speed nitrogen flow spraying surface, and the continuous metal flow flowing out of the flow guide holes is cut off to obtain the iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure.
The rod-shaped iron-nickel-molybdenum powder prepared by the method has a large axial-diameter ratio (the ratio of the axial length to the axial diameter), can reduce the demagnetization factor of the powder in the long axis direction, improves the effective magnetic conductivity of the powder in the long axis direction, and realizes the improvement of the effective magnetic conductivity of the finally prepared iron-nickel-molybdenum magnetic powder core. The rod-shaped iron-nickel-molybdenum alloy powder prepared by the method can be combined with the conventional coating pressing heat treatment process to prepare the iron-nickel-molybdenum metal magnetic powder core with the magnetic conductivity of more than 500.
2. The preparation device and the preparation method of the iron-nickel-molybdenum alloy powder provided by the invention have the advantages that the yield is high, and the particle size of the prepared powder is uniform.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a manufacturing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic view of an installation structure of a tundish of the manufacturing apparatus according to the embodiment of the present invention;
FIG. 3 is a schematic view of a circular seam nozzle assembly according to an embodiment of the present invention;
FIG. 4 isbase:Sub>A cross-sectional view taken along line A-A of FIG. 3;
FIG. 5 is a SEM image of the micro-morphology of an iron-nickel-molybdenum alloy powder sample prepared in example 2 of the invention;
FIG. 6 is a SEM image of the microstructure of an iron-nickel-molybdenum alloy powder sample prepared by a conventional atomization powder preparation process in a comparative example of the invention.
Description of the reference numerals
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that all the directional indicators (such as upper, lower, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the motion situation, and the like in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "plurality" or "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
Example 1
As shown in fig. 1-4, the present embodiment provides a device for preparing iron-nickel-molybdenum metal alloy powder, which mainly comprises a melting section and a powder-making section, wherein the powder-making section has a first chamber surrounded by a first shell 11; the melting section has a second chamber enclosed by a second housing 13 and the top of the first housing 11. In the present embodiment, the melting section and the pulverizing section are both cylindrical as a preferred embodiment.
The second chamber is internally provided with a smelting furnace 1, the top of the first shell 11 is fixedly provided with a tundish 2, and the tundish 2 is used for receiving metal molten liquid poured by the smelting furnace 1. As an implementable manner, a driving mechanism and a turnover mechanism are arranged on the smelting furnace 1, and the turnover mechanism can be driven by the driving mechanism to turn over so as to pour the molten liquid in the smelting furnace into a tundish. In a preferred embodiment, a high-frequency induction heater (not shown) is arranged on the tundish 2 and used for continuously heating the tundish during pouring to prevent the molten metal from being overheated insufficiently and solidifying in the flow guide hole to block the tundish.
In the embodiment, the tundish 2 is a hollow structure with two open ends, the bottom of the tundish is embedded in the first plate 3, the first plate 3 is fixed on the top of the first shell 11, and the top of the first shell 11 is provided with a first through hole 11-3 with the same size as the outer diameter of the tundish 2; a plurality of through flow guide holes 3-2 are equidistantly arranged on the first plate 3, the inlet end of each flow guide hole 3-2 is provided with a first flow guide opening, the outlet end of each flow guide hole 3-2 is provided with a second flow guide opening, and the inner diameter of each first flow guide opening is larger than that of each second flow guide opening; the tundish 2 in the fixed state is aligned with the first through hole 11-3 so that the melt poured into the tundish 2 can flow into the first chamber through the guide hole 3-2.
As a preferred embodiment, the first plate 3 in the embodiment is provided with a groove 3-1, the bottom of the tundish 2 is embedded in the groove 3-1, and the diversion hole 3-2 is arranged in the groove 3-1; in order to prevent the metal melt in the tundish 2 from seeping out from the gap of the groove 3-1 of the first plate 3, the jogged joint is sealed by refractory material. A third plate 4 is sleeved outside the tundish 2, the third plate 4 is provided with a second through hole 4-1 which is consistent with the outer diameter of the tundish 2, the third plate 4 penetrates through the tundish 2 to cover the first plate 3, the first plate 3 extends outwards along the outer edge of the groove 3-1 to form an outer edge, the periphery of the third plate 4 is provided with a plurality of first bolt holes 4-2, a plurality of second bolt holes 11-2 which are coaxial with the first bolt holes 4-2 are arranged at the corresponding position of the top plate 11-1 of the first shell 11, and the third plate 4 is used for fixing the first plate 3 on the top plate 11-1 by fixing bolts 5.
As a preferable embodiment, the inner diameter of the first diversion opening of the diversion hole 3-2 in the embodiment is 0.2 to 0.3mm, and the inner diameter of the second diversion opening is 0.05 to 0.1mm. During pouring, the molten liquid alloy flows into the second flow guide port from the first flow guide port, and the flow guide hole structure with the wide upper part and the narrow lower part can accelerate the flow speed of the molten liquid flow at the second flow guide port at the outlet end, so that blockage is prevented, the diameter of the melt can be reduced, the axial diameter ratio of the prepared rodlike powder is improved, and the yield of the rodlike powder with the large diameter-thickness ratio is improved. The flow guide holes 3-2 in this embodiment are uniformly arranged in multiple layers in an annular array with the center of the circle of the circular first plate 3 as the center.
As a preferred embodiment, the first plate 3 in this embodiment is a boron nitride ceramic plate; the tundish 2 is a cylinder with two open ends, correspondingly, the groove 3-1 on the first plate 3 is circular, the first plate 3 extends outwards along the outer edge of the groove 3-1 to form an outer edge, and the outer edge is circular and coaxial with the groove 3-1. Preferably, the extension width of the outer edge is 4 to 5cm. The third plate 4 is a metal cover plate, which is square in shape.
In this embodiment, the tundish 2 is made into a structure with two open ends, the bottom of the tundish is embedded in the first plate 3 (boron nitride ceramic round plate), and the first plate 3 (boron nitride ceramic round plate) is fixed at the top of the powder making part through the third plate 4, so that the boron nitride ceramic round plate is convenient to replace. Generally, a boron nitride ceramic circular plate is replaced every time a furnace is smelted; and the boron nitride ceramic plate is insulating and high-temperature resistant, so that impurities can be prevented from being doped in the powder preparation process, and the quality of the product is ensured.
In this embodiment, a circular seam nozzle assembly 6 is arranged in the first chamber, the circular seam nozzle assembly 6 is arranged below the guide hole 3-2, the circular seam nozzle assembly 6 is a circular pipe fitting formed by a hollow pipe 6-1 and provided with a hollow inner annular cavity 6-3, and the molten liquid flowing out of the guide hole 3-2 can fall into the hollow inner annular cavity 6-3; a central horizontal ring plane of the inner ring cavity wall is provided with a jet circular seam 6-2, the circular ring pipe fitting is also provided with a first input port which is generally arranged on the outer ring wall and is used for being connected with an external first nitrogen gas storage device 10, a connecting pipeline of the circular ring pipe fitting is provided with a booster pump 8 and a pulse electromagnetic valve 7, and the pulse electromagnetic valve 7 is connected with a PLC (programmable logic controller) control system 9 and is used for setting the switching time of the pulse electromagnetic valve 7 so as to input pulse type high-speed nitrogen gas flow into a hollow pipe 6-1 of the circular seam nozzle assembly 6; the pulse type high-speed nitrogen flow can be sprayed out through the spraying annular seam 6-2 to form a horizontal pulse type high-speed nitrogen flow spraying surface which is used for cutting off continuous metal liquid flow flowing out of the flow guide holes 3-2 to prepare the rod-shaped iron-nickel-molybdenum metal alloy powder with the micro-morphology structure.
In the preferred embodiment, the width of the injection circumferential weld 6-2 of the circumferential weld nozzle assembly 6 is 0.1 to 0.2mm. Preferably, the circular slit nozzle assembly 6 is fixed by 4 steel frames 16 provided on the inner wall of the first housing 11.
The bottom of the first shell 11 of the powder making part of the device is connected with a detachable charging basket 17, and preferably, a sealing ring 18 is arranged at the joint of the first shell and the detachable charging basket and is used for collecting the prepared iron-nickel-molybdenum alloy powder.
The detachable charging basket 17 is connected with a cooling device for cooling the prepared powder. As a preferred embodiment, the cooling device in this embodiment is a water-cooling circulation cooling device, and includes a buffer tank 20, a sedimentation tank 21; the bottom of a first shell 11 of the powder making part is provided with a filter cloth 19, a circulating water outlet is arranged at the position below the filter cloth 19 on the first shell 11, and a circulating water inlet is arranged at one side of the position above the filter cloth 19 on the first shell 11, which is opposite to the circulating water outlet; a first motor 23 is arranged on a connecting pipeline between the circulating water outlet and the buffer tank 20, a second motor 24 is arranged on a connecting pipeline between the buffer tank 20 and the sedimentation tank 21, and a third motor 25 is arranged on a connecting pipeline between the sedimentation tank 21 and the circulating water inlet; when the device works, water is placed in the detachable charging basket 17, the buffer pool 20 and the sedimentation pool 21 to form a circulating water path to cool the prepared iron-nickel-molybdenum powder. According to the invention, the filter cloth 19 is arranged at the bottom of the first shell 11 of the powder making part, so that on one hand, the buffering effect can be achieved, the powder is prevented from directly falling into the bottom of the detachable charging basket 17, and the rod-shaped powder is prevented from being broken; on the other hand, for filtering rod-like powders in circulating water. In order to further filter the powder in the circulating water, a filter screen 22 is also arranged on the connecting pipeline of the circulating water outlet.
The top of powder process portion is equipped with first exhaust port, connects outside first exhaust duct for the nitrogen gas that the discharge let in. Preferably, the middle section of the first exhaust pipeline is provided with a dust removal cloth bag 15 for adsorbing a small amount of fine particle powder wrapped in the discharged nitrogen. When the nitrogen dust removal device works, a small amount of fine particle powder wrapped by nitrogen gas upwards enters the nitrogen gas discharge pipe, the fine particle powder is adsorbed on the dust removal cloth bag 15, and the nitrogen gas is discharged from gaps of the dust removal cloth bag 15.
A second exhaust port is formed in a second chamber of the smelting part in the embodiment and is connected with an external second exhaust pipeline, and a fourth motor 12 is arranged on the second exhaust pipeline and is used for exhausting and vacuumizing; the second chamber is also provided with a nitrogen gas input port which is connected with an external second nitrogen gas storage device 14 and used for inputting nitrogen gas protection into the second chamber, and the melt liquid poured into the tundish can better flow into the powder making part from the flow guide holes under the gas pressure.
Example 2
The embodiment provides a method for preparing iron-nickel-molybdenum metal alloy powder by using the preparation device in the embodiment 1, which specifically comprises the following steps:
(1) Weighing pure metal iron, nickel and molybdenum according to the following proportion: 80-85wt% of nickel, 2-5wt% of molybdenum and the balance of iron are placed in a smelting furnace 1 for heating and smelting, the molten metal is continuously heated after being changed into molten liquid metal liquid, the molten liquid metal liquid is overheated to 150-200 ℃, then the molten liquid metal liquid is poured into a tundish 2, and meanwhile, the tundish 2 is continuously heated by a high-frequency induction heater, so that the phenomenon that the superheat degree of a solution is insufficient and the solution is solidified in a guide hole to block the tundish is avoided. Before heating and smelting, the fourth motor 12 is started to exhaust the second chamber of the smelting part and vacuumize the second chamber to 20-50pa, then nitrogen is input into the second chamber through a nitrogen input port for protection, nitrogen is supplemented to 90-100Kpa, the input nitrogen can form certain pressure in the second chamber, a downward positive pressure is provided for the tundish 2, and therefore the molten liquid poured into the tundish 2 can better flow into the powder making part from the flow guide holes 3-2. The aperture of the flow guide hole is smaller, the upper part of the flow guide hole is wide, and the lower part of the flow guide hole is narrow, so that the flow guide hole can better flow into the powder making part from the flow guide hole 3-2 under the pressure action of nitrogen flushed from the nitrogen inlet of the second cavity, and the problem of hole blockage can be avoided. After vacuum pumping, the quality of the product in the smelting process can be ensured under the nitrogen protection atmosphere.
(2) The molten metal liquid poured into the tundish 2 flows out to a circumferential seam nozzle assembly 6 below the molten metal liquid through a plurality of through flow guide holes 3-2 which are wide at the top and narrow at the bottom and are arranged on a first plate 3 at the bottom of the molten metal liquid, and the PLC control system 9 is used for controlling the switching time of a pulse electromagnetic valve 7 arranged on a nitrogen input pipeline so as to input pulse high-speed nitrogen flow to the circumferential seam nozzle assembly 6; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam 6-2 arranged on a central horizontal annular plane of the inner annular cavity wall to form a horizontal pulse type high-speed nitrogen flow spraying surface, and continuous metal liquid flow flowing out of the flow guide holes 3-2 is cut off to obtain iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure. In the preferred embodiment, the switching time of the pulse electromagnetic valve 7 is controlled to open 5ms and stop 10ms every 15ms period to cut off the metal liquid flow by nitrogen gas to form the iron-nickel-molybdenum metal alloy powder with a bar-shaped microstructure, and the obtained bar-shaped powder has a length of about 6mm and is easy to break due to overlong length. And combining the inner diameter (0.05-0.1mm) of the second diversion port at the outlet end of the diversion hole to prepare the rod-shaped powder with a certain axial-diameter ratio, wherein the axial-diameter ratio of the rod-shaped powder prepared in the embodiment is 60-120.
(3) Meanwhile, the prepared powder falls into a detachable charging basket 17 filled with water at the bottom of the powder preparation part and is cooled through water cooling circulation. The nitrogen medium is discharged upwards through a second exhaust port at the top of the powder making part.
(4) After the molten liquid completely flows out of the diversion holes, draining the water in the detachable charging basket 17 at the bottom, putting the iron-nickel-molybdenum slurry covered on the filter cloth 19 into a vacuum mixer, drying at the temperature of 60-80 ℃ for 30-60min to obtain dry iron-nickel-molybdenum powder;
(5) And placing the dried iron-nickel-molybdenum powder on a 300-mesh screen in an ultrasonic screening machine for screening, wherein the 300-mesh screen is qualified iron-nickel-molybdenum powder, the qualified iron-nickel-molybdenum powder enters a plastic barrel with a woven bag arranged inside through a soft rubber tube connected with the ultrasonic screening machine, and a foam layer plays a role in buffering after the woven bag and the plastic barrel are placed for 2-3cm in an interlayer. The purpose of the 300 mesh sieve is to remove broken chip powder and obtain qualified rod-shaped powder. The foam layer is placed to the intermediate layer of braided bag and plastic drum can further prevent bar-like powder rupture.
Taking the sample of the iron-nickel-molybdenum metal alloy powder prepared by the method of this embodiment, the SEM image is shown in fig. 5, and it can be seen that the microstructure of the iron-nickel-molybdenum metal alloy powder prepared by the method of the present invention is a rod-like structure.
In contrast, in the embodiment of the present invention, the iron-nickel-molybdenum metal alloy powder is prepared by referring to the conventional gas atomization powder preparation method disclosed in chinese patent publication No. CN109317688a in the prior art, and an SEM image of the iron-nickel-molybdenum metal alloy powder is shown in fig. 6.
Example 3
The embodiment provides a method for preparing an iron-nickel-molybdenum magnetic powder core by using the rod-shaped iron-nickel-molybdenum metal alloy powder prepared by the method in the embodiment 2, which specifically comprises the following steps:
(1) Insulating and coating: placing the iron-nickel-molybdenum metal alloy powder in a coating solution to carry out chemical film forming treatment, wherein the film forming time is 0.5 to 1h; the coating solution is formed by dissolving a coating agent in a coating solvent, the coating agent is a mixture of silicon dioxide, organic silicon and phosphoric acid, and the mass ratio of the silicon dioxide to the organic silicon to the phosphoric acid is 1:2:1; the coating solvent is absolute ethyl alcohol; the addition amount of the coating agent is 1 per mill to 5 per mill of the weight of the mixed magnetic powder; the adding amount of the coating solvent is 3-5% of the weight of the mixed magnetic powder;
(3) And (3) pressing and forming: adding 0.1-0.4 wt% of zinc stearate and 0.1-0.5 wt% of K resin into the insulated and coated magnetic powder, feeding the magnetic powder into a die cavity of a forming press under the pressure of 100-300T, and performing compression forming by ultrasonic vibration for 1-2s to obtain a blank magnetic core; the powder fed into the die cavity can ensure that the rod-shaped powder is laid in the die cavity in a full horizontal mode after ultrasonic vibration, and the phenomenon that the powder is crushed in the pressing forming process to influence the performance of the magnetic powder core is avoided.
(4) Annealing: placing the blank magnetic core in a vacuum sintering furnace, and annealing under the mixed gas of reducing atmosphere and inert atmosphere at the annealing temperature of 650-750 ℃ for 0.8-1.2h; the reducing atmosphere is H 2 The inert atmosphere is Ar or N 2 (ii) a The volume ratio of the reducing atmosphere to the inert atmosphere is 7-6:3-4;
(5) Impregnation treatment: adding the annealed blank magnetic core into an acetone solution containing epoxy resin with the mass percentage concentration of 0.8-1.2%, soaking for 30-60min, taking out, cleaning, and then baking at 80-120 ℃;
(6) And performing powder coating and sorting to obtain the iron-nickel-molybdenum magnetic powder core.
As a comparison, the spherical Fe-Ni-Mo metal alloy powder obtained by the conventional gas atomization powder preparation method of the comparative example of example 2 was subjected to the same process as described above to obtain an Fe-Ni-Mo magnetic powder core of the same size. The magnetic performance of two magnetic powder core samples is detected according to the following method:
(1) Effective magnetic permeability: measuring inductance L of a metal magnetic powder core by using a TH2816B precision LCR digital bridge device, and obtaining magnetic core permeability L =4 pi mu N Ae/le by using a formula, wherein: l is inductance (H), mu is magnetic core permeability, N is turns, ae is magnetic core sectional area (cm), le is magnetic core magnetic path length (cm);
(2) Power loss: testing the power loss of the magnetic powder core by adopting a WL3866E wide high-power signal source, wherein Pc = W/V; (W is power (kW), V is volume cm 3 ）
3) Direct current superposition characteristics: detecting by using a TH1778A direct current power supply bias tester with DC = Ls/L 0 Wherein: DC is direct current superposition, ls is inductance under a certain current value; l0 is the initial inductance with a current value of zero.
The detection results are shown in table 1;
in conclusion: the preparation process of the iron-nickel-molybdenum alloy powder provided by the invention takes nitrogen as a medium, sets the switching time of a pulse electromagnetic valve through a PLC control system, and opens the electromagnetic valve in a pulse period to input pulse type high-speed nitrogen flow to a circular seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam arranged on a central horizontal annular plane of the inner annular cavity wall of the pulse type high-speed nitrogen flow to form a horizontal pulse type high-speed nitrogen flow spraying surface, and the continuous metal flow flowing out of the flow guide holes is cut off to obtain the iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure.
The rod-shaped iron-nickel-molybdenum powder prepared by the method has a large axial-diameter ratio (the ratio of the axial length to the axial diameter), can reduce the demagnetization factor of the powder in the long axis direction, improves the effective magnetic conductivity of the powder in the long axis direction, and realizes the improvement of the effective magnetic conductivity of the finally prepared iron-nickel-molybdenum magnetic powder core. The rod-shaped iron-nickel-molybdenum alloy powder prepared by the method can be combined with the conventional coating pressing heat treatment process to prepare the iron-nickel-molybdenum metal magnetic powder core with the magnetic conductivity of more than 500.
The preparation device and the preparation method of the iron-nickel-molybdenum alloy powder provided by the invention have the advantages that the yield is high, and the particle size of the prepared powder is uniform.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The device for preparing the iron-nickel-molybdenum metal alloy powder is characterized by mainly comprising a smelting part and a powder making part, wherein the powder making part is provided with a first chamber surrounded by a first shell; the smelting part is provided with a second chamber enclosed by a second shell and the top of the first shell;
a smelting furnace is arranged in the second cavity, a tundish is fixedly arranged at the top of the first shell, and the tundish is used for receiving molten metal liquid poured by the smelting furnace; the tundish is of a hollow structure with openings at two ends, the bottom of the tundish is embedded in a first plate, the first plate is fixed at the top of the first shell, and the top of the first shell is provided with a first through hole with the same size as the outer diameter of the tundish; a plurality of through flow guide holes are equidistantly arranged on the first plate, a first flow guide port is arranged at the inlet end of each flow guide hole, a second flow guide port is arranged at the outlet end of each flow guide hole, and the inner diameter of each first flow guide port is larger than that of each second flow guide port; the tundish in the fixed state is aligned with the first through hole, so that the molten liquid poured in the tundish can flow into the first cavity through the flow guide hole;
the first cavity is internally provided with a circular seam nozzle assembly, the circular seam nozzle assembly is arranged below the corresponding diversion hole, the circular seam nozzle assembly is a circular pipe fitting which is formed by a hollow pipe and is provided with a hollow inner annular cavity, and the molten liquid flowing out of the diversion hole can fall into the range of the hollow inner annular cavity; the central horizontal ring plane of the inner ring cavity wall is provided with a jet circular seam, the circular ring pipe fitting is also provided with a first input port which is used for being connected with an external first nitrogen gas storage device, a connecting pipeline of the circular ring pipe fitting is provided with a booster pump and a pulse electromagnetic valve, and the pulse electromagnetic valve is connected with a PLC control system and used for setting the switching time of the pulse electromagnetic valve so as to input pulse type high-speed nitrogen gas flow into a hollow pipe of the circular seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through the spraying annular seam to form a horizontal pulse type high-speed nitrogen flow spraying surface which is used for intercepting continuous metal liquid flow flowing out of the flow guide holes to prepare iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure;
the bottom of the first shell of the powder making part is connected with a detachable discharging barrel for collecting the prepared iron-nickel-molybdenum alloy powder; the detachable charging bucket is connected with a cooling device for cooling the collected powder; the powder making part is also provided with a first exhaust port which is connected with an external first exhaust pipeline and used for exhausting introduced nitrogen;
the first plate is provided with a groove, the bottom of the tundish is embedded in the groove, and the flow guide hole is arranged in the groove; the middle package overcoat is equipped with the third plate, and the third plate is equipped with the second through-hole unanimous with middle package external diameter size, and the third plate passes middle package lid and establishes on first plate, and first plate is along the outer fringe of its recess and outwards extends and form the outer fringe, and the periphery of third plate is equipped with a plurality of first bolt holes, and the corresponding position of device body roof is equipped with a plurality of second bolt holes coaxial with first bolt hole, adopts fixing bolt to fix first plate at the top of first casing through the third plate.
2. The apparatus for producing iron-nickel-molybdenum metal alloy powder according to claim 1,
the tundish is provided with a high-frequency induction heater for continuously heating the tundish during pouring.
3. The apparatus for producing iron-nickel-molybdenum metal alloy powder according to claim 1 or 2,
the cooling device is a water-cooling circulating cooling device and comprises a buffer pool and a sedimentation pool; the bottom of a first shell of the powder making part is provided with filter cloth, a circulating water outlet is arranged at the position below the filter cloth on the first shell, and a circulating water inlet is arranged at the position above the filter cloth on one side of the first shell opposite to the circulating water outlet; a first motor is arranged on a connecting pipeline between the circulating water outlet and the buffer tank, a second motor is arranged on a connecting pipeline between the buffer tank and the sedimentation tank, and a third motor is arranged on a connecting pipeline between the sedimentation tank and the circulating water inlet; during operation, all put water in removable unloading bucket, buffer pool, the sedimentation tank, form the circulation water route and cool off the iron-nickel-molybdenum powder that makes.
4. The apparatus for producing iron-nickel-molybdenum metal alloy powder according to claim 1 or 2,
a second exhaust port is formed in a second chamber of the smelting part and connected with an external second exhaust pipeline, and a fourth motor is arranged on the second exhaust pipeline and used for exhausting and vacuumizing; the second chamber is also provided with a nitrogen input port which is connected with an external second nitrogen storage device and used for inputting nitrogen protection to the second chamber, and the melt liquid poured into the tundish can better flow into the powder making part from the flow guide holes under the gas pressure.
5. The apparatus for producing iron-nickel-molybdenum metal alloy powder according to claim 1 or 2,
the annular-slit-shaped nozzle assembly is fixed through a plurality of steel frames arranged on the inner wall of the first shell; the width of the jet circular seam is 0.1 to 0.2mm.
6. The method for preparing iron-nickel-molybdenum metal alloy powder by using the preparation device as claimed in any one of claims 1 to 5, comprising the following steps:
(1) Feeding pure metals of iron, nickel and molybdenum into a smelting furnace according to a preset proportion, heating and smelting, continuing to heat after the pure metals of iron, nickel and molybdenum are changed into molten liquid metal liquid, overheating to 150-200 ℃, pouring into a tundish, and meanwhile, continuously heating the tundish by using a high-frequency induction heater; before smelting, vacuumizing the second chamber to 20-50pa through the first exhaust port, and then inputting nitrogen into the second chamber through a nitrogen input port for protection, and supplementing nitrogen to 90-100Kpa;
(2) The molten liquid poured into the tundish flows out to a circumferential seam nozzle assembly below the molten liquid through a plurality of through flow guide holes arranged on a first plate at the bottom of the molten liquid, and the PLC control system is used for controlling the on-off time of a pulse electromagnetic valve arranged on a nitrogen input pipeline so as to input pulse type high-speed nitrogen flow to the circumferential seam nozzle assembly; the pulse type high-speed nitrogen flow can be sprayed out through a spraying annular seam arranged on a central horizontal annular plane of the inner annular cavity wall of the pulse type high-speed nitrogen flow to form a horizontal pulse type high-speed nitrogen flow spraying surface, and the continuous metal flow flowing out of the flow guide holes is cut off to obtain iron-nickel-molybdenum metal alloy powder with a rod-shaped microstructure;
(3) The prepared powder falls into a detachable material barrel filled with water at the bottom of the powder preparation part and is cooled through water cooling circulation; the nitrogen medium is discharged upwards through a second exhaust port at the top of the powder making part;
(4) After the molten liquid completely flows out of the diversion holes, emptying the water in the detachable discharging barrel, putting the iron-nickel-molybdenum slurry covered on the filter cloth into a vacuum mixer, drying at the temperature of 60-80 ℃ for 30-60min;
(5) And (3) placing the dried iron-nickel-molybdenum powder on a 300-mesh sieve in an ultrasonic sieving machine for sieving, wherein the 300-mesh oversize product is qualified iron-nickel-molybdenum powder, the qualified iron-nickel-molybdenum powder enters a plastic barrel with a built-in woven bag through a soft rubber pipe connected with the ultrasonic sieving machine, and a foam layer with the thickness of 2-3cm is placed between the woven bag and the plastic barrel.
7. The manufacturing apparatus of any one of claims 1 to 5 or the method of claim 6, wherein the iron-nickel-molybdenum metal alloy powder has a rod-like micro-morphology.
8. A high permeability Fe-Ni-Mo magnetic powder core prepared by using the Fe-Ni-Mo metal alloy powder according to claim 7.
9. The method for preparing the high-permeability Fe-Ni-Mo magnetic powder core as claimed in claim 8, characterized by comprising the following steps:
(1) Insulating and coating: placing the iron-nickel-molybdenum magnetic powder prepared by the preparation device of any one of claims 1 to 5 or the method of claim 6 in a coating solution for chemical film forming for 0.5 to 1h; the coating solution is formed by dissolving a coating agent in a coating solvent, the coating agent is a mixture of silicon dioxide, organic silicon and phosphoric acid, and the mass ratio of the silicon dioxide to the organic silicon to the phosphoric acid is 1:2:1; the coating solvent is absolute ethyl alcohol; the addition amount of the coating agent is 1 of the weight of the mixed magnetic powder‰-5Permillage; the adding amount of the coating solvent is 3-5% of the weight of the mixed magnetic powder;
(2) And (3) pressing and forming: adding 0.1-0.4 wt% of zinc stearate and 0.1-0.5 wt% of K resin into the insulated and coated magnetic powder, feeding the magnetic powder into a die cavity of a forming press under the pressure of 100-300T, and performing compression forming by ultrasonic vibration for 1-2s to obtain a blank magnetic core;
(3) Annealing: placing the blank magnetic core in a vacuum sintering furnace, and annealing under the mixed gas of a reducing atmosphere and an inert atmosphere at the annealing temperature of 650 to 750 ℃ for 0.8 to 1.2h; the reducing atmosphere is H 2 The inert atmosphere is Ar or N 2 (ii) a The volume ratio of the reducing atmosphere to the inert atmosphere is 7-6:3-4;
(4) Impregnation treatment: adding the annealed blank magnetic core into an acetone solution containing epoxy resin with the mass percentage concentration of 0.8-1.2%, soaking for 30-60min, taking out, cleaning, and then baking at 80-120 ℃;
(5) Powder coating and sorting.
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| CN103611942B (en) * | 2013-12-10 | 2015-10-14 | 河北联合大学 | The method of high pressure melting atomization nitrogen quenching device and production samarium Fe-N Alloys powder thereof |
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