CN111390187A - Preparation method of permanent magnet powder by applying double-sided wet-warm oxidation treatment - Google Patents

Preparation method of permanent magnet powder by applying double-sided wet-warm oxidation treatment Download PDF

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CN111390187A
CN111390187A CN202010168459.8A CN202010168459A CN111390187A CN 111390187 A CN111390187 A CN 111390187A CN 202010168459 A CN202010168459 A CN 202010168459A CN 111390187 A CN111390187 A CN 111390187A
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郁成斌
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Jiangsu Juxin Magnet Co ltd
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Abstract

The invention discloses a method for preparing permanent magnetic powder by applying double-sided wet-warm oxidation treatment, which belongs to the technical field of magnetic composite materials, can realize that a certain content of Nb and Zr is added in a raw material formula in a compounding way, the crystallization temperature of alloy is improved, the nucleation rate is increased, crystal grains can be obviously refined, the coercive force is obviously improved, the comprehensive performance of magnetic powder preparation is improved through process optimization, particularly the accurate control of time, temperature, grain diameter and the like during crystallization treatment is reflected, a magnetic powder sample is poured into a double-sided wet-warm treatment device for high-wet treatment after crystallization treatment, simultaneously high-temperature treatment with two gradients is carried out, and a special interval humidification and contact type drying method is adopted, so that crystals can be effectively oxidized and eliminated, and the internal stress structure of the magnetic powder can be improved to fully ensure the whole surface property and uniformity of the magnetic powder sample oxidation treatment, improve the comprehensive performance of the magnetic powder product and prolong the service life.

Description

Preparation method of permanent magnet powder by applying double-sided wet-warm oxidation treatment
Technical Field
The invention relates to the technical field of magnetic composite materials, in particular to a preparation method of permanent magnetic powder by applying double-sided wet-warm oxidation treatment.
Background
With the rapid development of high-tech industries, the neodymium iron boron permanent magnet powder is widely applied to the fields of aviation, aerospace, navigation, automobiles, various precision instruments, small and medium-sized, miniature high-efficiency motors, computers, IT technical equipment, office automation equipment, numerous household appliances and the like, and is continuously expanding. However, the electronic information industry and the identification bar code printing industry for highly anti-counterfeiting products and commodities have new requirements on the use of neodymium iron boron permanent magnet powder.
The existing neodymium iron boron permanent magnetic powder has higher cost during preparation, the comprehensive magnetic performance of the prepared magnetic powder is poorer, the aging phenomenon is easy to occur after the magnetic powder is used for a period of time, a crystallization process in the preparation process of the magnetic powder plays a vital role, whether the crystallization treatment is fully qualified is a key step for determining the performance of the magnetic powder, and crystal particles can be generated under two conditions in the preparation process of the neodymium iron boron quick quenching permanent magnetic powder, wherein one condition is that a splash spark generated in a vacuum quick quenching procedure is splashed into a storage barrel; the other is that in the initial stage of rapid quenching and arc starting and the final furnace shutdown stage, the molten liquid is discharged in an inertial flowing mode instead of an overflow mode, and non-ideal amorphous and crystalline powder is also easily generated, and the two non-artificially generated microparticles can generate the phenomena of skinning or bubbling during the aging test of the prepared magnetic product, thereby not only affecting the performance of the magnetic powder, but also obviously shortening the service life of the magnetic powder. Further, the neodymium iron boron quick quenching permanent magnet powder oxidation process flow comprises the following steps: loading, spreading, steam humidifying, drying, blanking, detecting and packaging. Further, the steam humidification makes the neodymium iron boron permanent magnet powder wet but not contain liquid water.
Although the scheme can eliminate partial crystals to a great extent, the paving, humidifying and drying modes are adopted, the phenomena of insufficient humidification and uneven temperature are certainly caused, the crystals cannot be completely eliminated, and the internal stress structure of the magnetic powder is influenced, so that the conventional permanent magnetic powder oxidation process has obvious defects.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for preparing permanent magnetic powder by applying double-sided wet-warm oxidation treatment, which can improve the crystallization temperature of alloy by compositely adding a certain content of Nb and Zr in a raw material formula, lead to the increase of nucleation rate, obviously refine crystal grains, obviously improve coercive force, improve the comprehensive performance of magnetic powder preparation by optimizing the process, particularly reflect the accurate control of time, temperature, grain diameter and the like during crystallization treatment, simultaneously pour a magnetic powder sample into a double-sided wet-warm treatment device for high-humidity treatment after crystallization treatment, simultaneously accompany with high-temperature treatment of two gradients, and adopt a special interval humidification and contact drying method, not only can effectively oxidize and eliminate crystals, but also can improve the internal stress structure of the magnetic powder and fully ensure the comprehensiveness and uniformity of the magnetic powder sample oxidation treatment, thoroughly eliminate the crystal in the magnetic powder, completely oxidize the crystal, improve the comprehensive performance of the magnetic powder product and prolong the service life.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation method of permanent magnetic powder applying double-sided wet-warm oxidation treatment comprises the following steps:
s1, raw material formula: 15.5% -19% of praseodymium-neodymium alloy, 3% -7% of lanthanum-cerium alloy, 2% -2.5% of niobium, 2.5% -3% of zirconium, 1.15% -1.25% of boron and the balance of pure iron, cleaning with acetone after removing oxide skin to form ingredients to be smelted;
s2, vacuum melting: putting the ingredients into a vacuum induction furnace, carrying out high-temperature smelting under the protection of argon, wherein the pressure of the argon is 0.04Pa-0.05Pa, raising the temperature to 1650 ℃ in the smelting process, and cooling for 20min-40min after the materials are fully melted and fully boiled for 3-5min to form an alloy liquid, starting casting, and forming a master alloy;
s3, vacuum rapid quenching: vacuumizing in a rapid quenching furnace, adding argon to positive pressure of +0.01MPa, heating and melting mother alloy to form alloy liquid, overflowing from a crucible in the rapid quenching furnace through the edge of a pouring gate, flowing into the edge of a molybdenum wheel rotating at high speed, solidifying and cooling the alloy liquid under the action of the rotating molybdenum wheel to form an alloy strip, wherein the linear speed of the rotation of the molybdenum wheel is 17-23 m/s, and the solidification and cooling speed is 102-106 k/s;
s4, initial pressure: pressing the alloy strip into primary powder of 50 meshes by a press machine, and screening out powder with large particle size;
s5, crystallization heat treatment: filling the primary powder into a charging barrel of a crystallization furnace, setting the temperature at 700 ℃, vacuumizing, and then filling argon, crystallizing the primary powder under positive pressure for 5-10 min to obtain a crystallized sample;
s6, aging treatment: pouring the magnetic powder sample into a double-sided wet-temperature treatment device for high-humidity treatment, and simultaneously carrying out high-temperature treatment along with two gradients to realize oxidation elimination treatment on crystals in the magnetic powder sample;
s7, jet milling: performing jet milling on the aged sample by using a closed-loop running colliding fluidized bed to obtain neodymium iron boron alloy superfine permanent magnet powder with a specified particle size;
s8, magnetic powder performance detection: and screening and classifying the neodymium iron boron alloy superfine permanent magnetic powder, then carrying out multiple magnetic powder performance tests, and separately packaging into identifiers.
Further, in the step S2, the ingredients are firstly vacuumized in a vacuum induction furnace and heated at low power for 2-3min for preheating, argon is filled after moisture and gas are discharged, the mixture is lifted to the maximum power for melting, and the alloy is melted down and then refined at low power for 10min for casting.
Further, after the crystallization heat treatment in the step S5, the raw material is cooled to 40 ℃ in a grading manner, and then is discharged, specifically, a three-stage water cooling manner is adopted, and the cooling speed is gradually increased.
Further, in the step S5, the crystallization furnace is vacuumized to 10-2Pa, argon is filled to 0.03-0.04 Pa, and the rotation frequency of the furnace tube of the crystallization furnace is 22-28 Hz.
Furthermore, the double-sided wet-temperature treatment device comprises an oxidation treatment chamber, a feed inlet and a discharge outlet are respectively arranged at the upper end and the lower end of the oxidation treatment chamber, a pair of fixed upright columns are fixedly connected at the inner bottom end of the oxidation treatment chamber, the fixed upright columns are installed on a stepping motor, an output end of the stepping motor is fixedly connected with a single-layer treatment plate, a falling strip is fixedly connected at the lower end of the single-layer treatment plate, a pair of single-layer treatment plates are provided with a plurality of uniformly distributed self-variable separation columns near one end, the space formed by the self-variable separation columns is matched with a magnetic powder sample, an installation plate is fixedly connected at the upper end of the single-layer treatment plate, a plurality of uniformly distributed atomization nozzles are installed at one end of the installation plate near the single-layer treatment plate, the atomization nozzles are connected with a booster water pump through, and fully exposing the single surface of the magnetic powder sample to realize full contact between steam and the magnetic powder sample, and realizing full-volume high-humidity high-temperature oxidation treatment after turning to surface change.
Furthermore, install the electro-magnet array in the individual layer processing board, it has the trachea to link to alternate in the individual layer processing board, it is connected with the electronic air pump on fixed mounting and the fixed post to link the trachea, individual layer processing board surface is cut and is had a plurality of and from becoming the insulated column assorted inflation hole, and the inflation hole is less than the particle diameter of magnetic sample, from becoming the insulated column and adopting elastic bag to make and with even trachea intercommunication, from becoming the insulated column and adopting inflatable convenient realization from protruding and reseing, can protruding partition magnetic sample on the one hand, keep certain space, prevent to take place the reunion phenomenon each other and influence the treatment effect, will divide the bank apart the face and can not block the contact of steam and magnetic sample after the reposition of bleeding simultaneously
Furthermore, a silica gel heating sheet is installed in the self-changing isolation column, the silica gel heating sheet and the atomizing spray head work synchronously, the initial temperature is 80-100 ℃, after the high-humidity treatment is finished, the temperature is uniformly raised to 120-plus 150 ℃ for drying, the high-humidity and high-temperature oxidation treatment effect can be kept, the steam is kept warm to prevent the steam from being directly liquefied when meeting cold, meanwhile, the mild heat treatment can be carried out on the magnetic powder sample, the internal stress structure is improved, and the treatment time can be saved.
Furthermore, the length of the self-changing isolation column is one half of the particle size of the magnetic powder sample and is consistent with the length of the anti-falling strip, the distance between the single-layer treatment plates is slightly larger than the particle size of the magnetic powder sample, the magnetic powder sample can be prevented from being stacked while being tiled, and the single-layer tiling is always kept.
Furthermore, atomizing nozzle interval blowout atomizing steam to the wet magnetic powder sample surface is the standard but the naked eye can not see the liquid pearl, is unlikely to appear humidity too big and the phenomenon of condensing into the liquid pearl when guaranteeing atomizing steam wet magnetic powder sample.
Further, the magnetic property detection comprises the detection of residual magnetism Br, intrinsic Hcb, intrinsic coercive force Hcj and magnetic energy product BH index, and the performance of the permanent magnetic powder can be comprehensively judged.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme can realize that the crystallization temperature of the alloy is improved by compositely adding a certain content of Nb and Zr in the raw material formula, so that the nucleation rate is increased, crystal grains can be obviously refined, the coercive force is obviously improved, the comprehensive performance of magnetic powder preparation is improved through the optimization in the process, the method is particularly embodied in the precise control of time, temperature, particle size and the like during crystallization treatment, simultaneously, a magnetic powder sample is poured into a double-sided wet-temperature treatment device for high-humidity treatment after the crystallization treatment, simultaneously, high-temperature treatment with two gradients is carried out, and a special interval humidification and contact type drying method is adopted, so that crystals can be effectively eliminated by oxidation, the internal stress structure of the magnetic powder can be improved, the whole surface property and the uniformity of the magnetic powder sample can be fully ensured, the crystals in the magnetic powder can be thoroughly eliminated, the magnetic powder can be completely oxidized, and the comprehensive performance of the magnetic, the service life is prolonged.
(2) The double-sided wet-temperature treatment device can realize that the magnetic powder sample is tiled between a pair of single-layer treatment plates in a single-layer mode, so that the single surface of the magnetic powder sample is fully exposed, the steam and the magnetic powder sample are fully contacted, and the full-volume high-humidity high-temperature oxidation treatment is realized after the surface is changed.
(3) Install the electro-magnet array in the individual layer processing board, it has the gas pipe to cross in the individual layer processing board, it is connected with the electronic air pump on fixed mounting and the fixed post to link the gas pipe, individual layer processing board surface is cut a plurality of and is become the discrete pillar assorted inflation hole certainly, and the inflation hole is less than the particle diameter of magnetic sample, become the discrete pillar certainly and adopt the elastic bag to make and with even trachea intercommunication, it is convenient to realize from protruding and reseing from the inflatable isolated pillar certainly to adopt the variable segregation, can protruding partition magnetic sample on the one hand, keep certain space, prevent to take place the reunion phenomenon each other and influence the treatment effect, simultaneously after reseing of bleeding to expose the parting surface can not block the contact of steam and magnetic sample
(4) The self-changing isolation column is internally provided with a silica gel heating sheet, the silica gel heating sheet and the atomizing spray head work synchronously, the initial temperature is 80-100 ℃, after the high-humidity treatment is finished, the temperature is uniformly raised to 120-plus 150 ℃ for drying, the high-humidity and high-temperature oxidation treatment effect can be kept, the steam is kept warm to prevent the steam from being directly liquefied when meeting cold, meanwhile, the mild heat treatment can be carried out on the magnetic powder sample, the internal stress structure is improved, and the treatment time can be saved.
(5) The length of the self-changing isolation column is one half of the particle size of the magnetic powder sample, and is consistent with the length of the anti-falling strip, the distance between the pair of single-layer processing plates is slightly larger than the particle size of the magnetic powder sample, the magnetic powder sample can be prevented from being stacked while being tiled, and the single-layer tiling is always kept.
(6) Atomizing nozzle interval blowout atomizing steam to wet magnetic powder sample surface but the naked eye can't see the liquid pearl and be the standard, be unlikely to appear humidity too big and the phenomenon of condensing into the liquid pearl when guaranteeing atomizing steam wet magnetic powder sample.
(7) The magnetic property detection comprises the detection of remanence Br, intrinsic Hcb, intrinsic coercive force Hcj and magnetic energy product BH index, and the performance of the permanent magnetic powder can be comprehensively judged.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic structural view of a double-sided wet/warm processing apparatus according to the present invention;
FIG. 3 is a schematic structural view of a single layer processing plate of the present invention;
FIG. 4 is a cross-sectional view of a single layer treated panel of the present invention;
FIG. 5 is a schematic structural view of a magnetic powder sample according to the present invention in a flat state;
FIG. 6 is a schematic view of the magnetic powder sample according to the present invention in a processing state.
The reference numbers in the figures illustrate:
the device comprises an oxidation treatment chamber 1, a feed inlet 2, a fixed upright column 3, a single-layer treatment plate 4, a stepping motor 5, a mounting plate 6, a booster water pump 7, an atomizing spray head 8, a discharge outlet 9, a self-changing isolation column 10, an anti-falling strip 11, an electromagnet array 12, a gas connecting pipe 13, an electric air pump 14 and a silica gel heating plate 15.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise specifically stated or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are used in a broad sense, and for example, "connected" may be a fixed connection, a detachable connection, an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection through an intermediate medium, and a communication between two elements.
Example 1:
referring to fig. 1, a method for preparing permanent magnetic powder by applying a double-sided wet-warm oxidation treatment includes the following steps:
s1, raw material formula: 15.5% of praseodymium-neodymium alloy, 3% of lanthanum-cerium alloy, 2% of niobium, 2.5% of zirconium, 1.15% of boron and the balance of pure iron, and cleaning with acetone after removing oxide skin to form ingredients to be smelted;
s2, vacuum melting: putting the ingredients into a vacuum induction furnace, carrying out high-temperature smelting under the protection of argon, wherein the pressure of the argon is 0.05Pa, raising the temperature to 1650 ℃ in the smelting process, starting casting when the materials are completely molten and fully boiled for 3 to become reddish to form alloy liquid, and cooling for 20min after the casting is finished to form a master alloy;
s3, vacuum rapid quenching: vacuumizing a rapid quenching furnace, adding argon to positive pressure of +0.01MPa, wherein the width of a rapid quenching strip under positive pressure is obviously smaller than that of a negative pressure rapid quenching strip, the size consistency of the strip is better than that under negative pressure, the width of the strip is narrow, and less metal liquid is cooled in unit time, so that the cooling speed is high, the mother alloy is heated and melted to form alloy liquid, the alloy liquid overflows from a crucible in the rapid quenching furnace through the edge of a sprue and flows into the edge of a molybdenum wheel rotating at high speed, the alloy liquid is solidified and cooled under the action of the rotating molybdenum wheel to form an alloy strip, the linear speed of the rotation of the molybdenum wheel is 17m/s, and the solidification and cooling speed is 102 k/s;
s4, initial pressure: pressing the alloy strip into primary powder of 50 meshes by a press machine, and screening out powder with large particle size;
s5, crystallization heat treatment: filling the primary powder into a charging barrel of a crystallization furnace, setting the temperature at 700 ℃, vacuumizing, and then filling argon, crystallizing the primary powder under positive pressure for 5min to obtain a crystallized sample;
s6, aging treatment: pouring the magnetic powder sample into a double-sided wet-temperature treatment device for high-humidity treatment, and simultaneously carrying out high-temperature treatment along with two gradients to realize oxidation elimination treatment on crystals in the magnetic powder sample;
s7, jet milling: performing jet milling on the aged sample by using a closed-loop running colliding fluidized bed to obtain neodymium iron boron alloy superfine permanent magnet powder with a specified particle size;
s8, magnetic powder performance detection: and screening and classifying the neodymium iron boron alloy superfine permanent magnetic powder, then carrying out multiple magnetic powder performance tests, and separately packaging into identifiers.
In the step S2, the ingredients are firstly vacuumized and heated at low power for 2min for preheating in a vacuum induction furnace, argon is filled after moisture and gas are discharged, the mixture is lifted to the maximum power for melting, and casting is carried out after the alloy is melted down and then refined at low power for 10 min.
And step S5, cooling the crystallized heat-treated material to 40 ℃ in a grading manner, and discharging the material, wherein a three-stage water cooling manner is adopted, and the cooling speed is gradually increased.
In step S5, the crystallization furnace is vacuumized to 10-2Pa, argon is filled to 0.04Pa, and the rotation frequency of the furnace tube of the crystallization furnace is 22 Hz.
Referring to fig. 2-3, the double-sided wet-warm processing device comprises an oxidation processing chamber 1, a feed inlet 2 and a discharge outlet 9 are respectively arranged at the upper end and the lower end of the oxidation processing chamber 1, a pair of fixed upright posts 3 are fixedly connected to the inner bottom end of the oxidation processing chamber 1, a stepping motor 5 is mounted on the fixed upright posts 3, a single-layer processing plate 4 is fixedly connected to the output end of the stepping motor 5, a falling-prevention strip 11 is fixedly connected to the lower end of the single-layer processing plate 4, a plurality of uniformly distributed self-changing isolation posts 10 are arranged at one end of the single-layer processing plate 4 close to each other, a space formed between the self-changing isolation posts 10 is matched with a magnetic powder sample, a mounting plate 6 is fixedly connected to the upper end of the single-layer processing plate 4, a plurality of uniformly distributed atomizing nozzles 8 are mounted at one end of the mounting plate 6 close to the single-layer processing, and fully exposing the single surface of the magnetic powder sample to realize full contact between steam and the magnetic powder sample, and realizing full-volume high-humidity high-temperature oxidation treatment after turning to surface change.
Referring to fig. 4-6, an electromagnet array 12 is installed in a single-layer processing plate 4, a gas connecting pipe 13 is inserted into the single-layer processing plate 4, the gas connecting pipe 13 is connected with an electric air pump 14 fixedly installed on a fixed upright post 3, a plurality of expansion holes matched with self-changing isolation columns 10 are cut on the surface of the single-layer processing plate 4, the expansion holes are smaller than the particle size of a magnetic powder sample, the self-changing isolation columns 10 are made of elastic bags and are communicated with the gas connecting pipe 13, the self-changing isolation columns 10 are convenient to self-bulge and reset by adopting an inflatable type, on one hand, the magnetic powder samples can be bulged to separate each other, a certain space is kept, the treatment effect is prevented from being influenced by the agglomeration phenomenon, meanwhile, the separation surface is exposed after air suction and reset, the contact between steam and the magnetic powder samples cannot be blocked, a silica gel heating sheet 15 is installed in the self, the initial temperature is 80-100 ℃ and is maintained to 120-150 ℃ after the high-humidity treatment is finished, the temperature is uniformly increased to 150 ℃ for drying, the high-humidity and high-temperature oxidation treatment effect can be kept, the steam is kept warm to prevent the steam from being directly liquefied when meeting cold, meanwhile, the mild heat treatment can be carried out on the magnetic powder sample, the internal stress structure is improved, and the treatment time can be saved.
The length of the self-changing isolation column 10 is one half of the particle size of the magnetic powder sample, and is consistent with the length of the anti-falling strip 11, the distance between the pair of single-layer processing plates 4 is slightly larger than the particle size of the magnetic powder sample, so that the magnetic powder sample can be prevented from being stacked while being tiled, and the single-layer tiling is always kept.
Atomizing nozzle 8 interval blowout atomizing steam to wet magnetic powder sample surface but the naked eye can not see the liquid pearl as the standard, is unlikely to appear humidity too big and the phenomenon of condensing into the liquid pearl when guaranteeing atomizing steam wet magnetic powder sample.
When the device is used, a magnetic powder sample is put from a feeding hole 2, the magnetic powder sample slides down to be tiled in a single-layer mode in a gap between a pair of single-layer treatment plates 4, an electromagnet array 12 on one single-layer treatment plate 4 on one side is randomly started to adsorb the magnetic powder sample, a stepping motor 5 on the other side is started to drive the corresponding single-layer treatment plate 4 to rotate one hundred eighty degrees downwards, one side of the magnetic powder sample is fully exposed, opposite atomizing nozzles 8 are started to eject atomizing steam at intervals, meanwhile, a silica gel heating plate 15 in the single-layer treatment plate 4 is started and heated to 80-100 ℃ and is maintained to be subjected to high-humidity treatment, the stepping motor 5 is started to reset the single-layer treatment plate 4 on the other side after treatment for a certain time, the same operation is adopted to carry out oxidation treatment on the other side of the magnetic powder sample, after the whole volume high-humidity treatment is finished, the pair of single-layer treatment plates 4 are reset to wrap the, after drying, synchronously rotating a pair of single-layer processing plates 4 downwards, controlling the electromagnet array 12 to be powered off, and slowly dropping the magnetic powder sample losing the magnetic attraction and collecting the magnetic powder sample flowing out along the channel 9.
The magnetic property detection comprises the detection of remanence Br, intrinsic Hcb, intrinsic coercive force Hcj and magnetic energy product BH index, and the performance of the permanent magnetic powder can be comprehensively judged.
Example 2:
referring to fig. 1, a method for preparing permanent magnetic powder by applying a double-sided wet-warm oxidation treatment includes the following steps:
s1, raw material formula: 17% of praseodymium-neodymium alloy, 5% of lanthanum-cerium alloy, 2.2% of niobium, 2.8% of zirconium, 1.2% of boron and the balance of pure iron, cleaning with acetone after removing oxide skin to form ingredients to be smelted;
s2, vacuum melting: putting the ingredients into a vacuum induction furnace, carrying out high-temperature smelting under the protection of argon, wherein the pressure of the argon is 0.045Pa, raising the temperature to 1650 ℃ in the smelting process, forming alloy liquid after the materials are completely molten and fully boiled for 4min to generate reddish color, starting casting, and cooling for 30min after the casting is finished to form a master alloy;
s3, vacuum rapid quenching: vacuumizing in a rapid quenching furnace, adding argon to positive pressure of +0.01MPa, heating and melting mother alloy to form alloy liquid, overflowing from a crucible in the rapid quenching furnace through the edge of a pouring gate, flowing into the edge of a molybdenum wheel rotating at high speed, solidifying and cooling the alloy liquid under the action of the rotating molybdenum wheel to form an alloy strip, wherein the linear speed of the rotation of the molybdenum wheel is 20m/s, and the solidification and cooling speed is 104 k/s;
s4, initial pressure: pressing the alloy strip into primary powder of 50 meshes by a press machine, and screening out powder with large particle size;
s5, crystallization heat treatment: filling the primary powder into a charging barrel of a crystallization furnace, setting the temperature at 700 ℃, vacuumizing, and then filling argon, crystallizing the primary powder under positive pressure for 8min to obtain a crystallized sample;
s6, aging treatment: pouring the magnetic powder sample into a double-sided wet-temperature treatment device for high-humidity treatment, and simultaneously carrying out high-temperature treatment along with two gradients to realize oxidation elimination treatment on crystals in the magnetic powder sample;
s7, jet milling: performing jet milling on the aged sample by using a closed-loop running colliding fluidized bed to obtain neodymium iron boron alloy superfine permanent magnet powder with a specified particle size;
s8, magnetic powder performance detection: and screening and classifying the neodymium iron boron alloy superfine permanent magnetic powder, then carrying out multiple magnetic powder performance tests, and separately packaging into identifiers.
In the step S2, the ingredients are firstly vacuumized and heated at low power for 2.5min for preheating in a vacuum induction furnace, argon is filled after moisture and gas are discharged, the mixture is lifted to the maximum power for melting, and casting is carried out after the alloy is melted down and then refined at low power for 10 min.
And step S5, cooling the crystallized heat-treated material to 40 ℃ in a grading manner, and discharging the material, wherein a three-stage water cooling manner is adopted, and the cooling speed is gradually increased.
In the step S5, the crystallization furnace is vacuumized to 10-2Pa, argon is filled to 0.035Pa, and the rotation frequency of the furnace tube of the crystallization furnace is 25 Hz.
The remainder was in accordance with example 1.
Example 3:
referring to fig. 1, a method for preparing permanent magnetic powder by applying a double-sided wet-warm oxidation treatment includes the following steps:
s1, raw material formula: 19% of praseodymium-neodymium alloy, 7% of lanthanum-cerium alloy, 2.5% of niobium, 3% of zirconium, 1.25% of boron and the balance of pure iron, and cleaning with acetone after removing oxide skin to form ingredients to wait for smelting;
s2, vacuum melting: putting the ingredients into a vacuum induction furnace, carrying out high-temperature smelting under the protection of argon, wherein the pressure of the argon is 0.04Pa, raising the temperature to 1650 ℃ in the smelting process, forming alloy liquid after the materials are completely molten and fully boiled for 5min to generate reddish color, starting casting, and cooling for 40min after the casting is finished to form a master alloy;
s3, vacuum rapid quenching: vacuumizing in a rapid quenching furnace, adding argon to positive pressure of +0.01MPa, heating and melting mother alloy to form alloy liquid, overflowing from a crucible in the rapid quenching furnace through the edge of a pouring gate, flowing into the edge of a molybdenum wheel rotating at high speed, solidifying and cooling the alloy liquid under the action of the rotating molybdenum wheel to form an alloy strip, wherein the linear speed of the rotation of the molybdenum wheel is 23m/s, and the solidification and cooling speed is 106 k/s;
s4, initial pressure: pressing the alloy strip into primary powder of 50 meshes by a press machine, and screening out powder with large particle size;
s5, crystallization heat treatment: filling the primary powder into a charging barrel of a crystallization furnace, setting the temperature at 700 ℃, vacuumizing, and then filling argon, crystallizing the primary powder under positive pressure for 10min to obtain a crystallized sample;
s6, aging treatment: pouring the magnetic powder sample into a double-sided wet-temperature treatment device for high-humidity treatment, and simultaneously carrying out high-temperature treatment along with two gradients to realize oxidation elimination treatment on crystals in the magnetic powder sample;
s7, jet milling: performing jet milling on the aged sample by using a closed-loop running colliding fluidized bed to obtain neodymium iron boron alloy superfine permanent magnet powder with a specified particle size;
s8, magnetic powder performance detection: and screening and classifying the neodymium iron boron alloy superfine permanent magnetic powder, then carrying out multiple magnetic powder performance tests, and separately packaging into identifiers.
In the step S2, the ingredients are firstly vacuumized and heated at low power for 3min for preheating in a vacuum induction furnace, argon is filled after moisture and gas are discharged, the mixture is lifted to the maximum power for melting, and casting is carried out after the alloy is melted down and then refined at low power for 10 min.
And step S5, cooling the crystallized heat-treated material to 40 ℃ in a grading manner, and discharging the material, wherein a three-stage water cooling manner is adopted, and the cooling speed is gradually increased.
In step S5, the crystallization furnace is vacuumized to 10-2Pa, argon is filled to 0.03Pa, and the rotation frequency of the furnace tube of the crystallization furnace is 28 Hz.
The remainder was in accordance with example 1.
The invention can realize that the crystallization temperature of the alloy is improved by compositely adding a certain content of Nb and Zr in the raw material formula, so that the nucleation rate is increased, the crystal grains can be obviously refined, the coercive force is obviously improved, the comprehensive performance of the magnetic powder preparation is improved through the optimization of the working procedure, the method is particularly embodied in the precise control of time, temperature, grain diameter and the like during the crystallization treatment, simultaneously, the magnetic powder sample is poured into a double-sided wet-temperature treatment device for high-humidity treatment after the crystallization treatment, simultaneously, the high-temperature treatment with two gradients is carried out, and the special interval humidification and contact type drying method is adopted, so that the crystal can be effectively eliminated by oxidation, the internal stress structure of the magnetic powder can be improved, the whole surface property and the uniformity of the oxidation treatment of the magnetic powder sample can be fully ensured, the crystal in the magnetic powder can be completely eliminated, the complete oxidation can be realized, the service life is prolonged.
The above are merely preferred embodiments of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims (10)

1. A preparation method of permanent magnetic powder applying double-sided wet-warm oxidation treatment is characterized by comprising the following steps: the method comprises the following steps:
s1, raw material formula: 15.5% -19% of praseodymium-neodymium alloy, 3% -7% of lanthanum-cerium alloy, 2% -2.5% of niobium, 2.5% -3% of zirconium, 1.15% -1.25% of boron and the balance of pure iron, cleaning with acetone after removing oxide skin to form ingredients to be smelted;
s2, vacuum melting: putting the ingredients into a vacuum induction furnace, carrying out high-temperature smelting under the protection of argon, wherein the pressure of the argon is 0.04Pa-0.05Pa, raising the temperature to 1650 ℃ in the smelting process, and cooling for 20min-40min after the materials are fully melted and fully boiled for 3-5min to form an alloy liquid, starting casting, and forming a master alloy;
s3, vacuum rapid quenching: vacuumizing in a rapid quenching furnace, adding argon to positive pressure of +0.01MPa, heating and melting mother alloy to form alloy liquid, overflowing from a crucible in the rapid quenching furnace through the edge of a pouring gate, flowing into the edge of a molybdenum wheel rotating at high speed, solidifying and cooling the alloy liquid under the action of the rotating molybdenum wheel to form an alloy strip, wherein the linear speed of the rotation of the molybdenum wheel is 17-23 m/s, and the solidification and cooling speed is 102-106 k/s;
s4, initial pressure: pressing the alloy strip into primary powder of 60 meshes by a press machine, and screening out powder with large particle size;
s5, crystallization heat treatment: filling the primary powder into a charging barrel of a crystallization furnace, setting the temperature at 700 ℃, vacuumizing, and then filling argon, crystallizing the primary powder under positive pressure for 5-10 min to obtain a crystallized sample;
s6, aging treatment: pouring the magnetic powder sample into a double-sided wet-temperature treatment device for high-humidity treatment, and simultaneously carrying out high-temperature treatment along with two gradients to realize oxidation elimination treatment on crystals in the magnetic powder sample;
s7, jet milling: performing jet milling on the aged sample by using a closed-loop running colliding fluidized bed to obtain neodymium iron boron alloy superfine permanent magnet powder with a specified particle size;
s8, magnetic powder performance detection: and screening and classifying the neodymium iron boron alloy superfine permanent magnetic powder, then carrying out multiple magnetic powder performance tests, and separately packaging into identifiers.
2. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 1, characterized in that: in the step S2, the ingredients are firstly vacuumized and heated at low power for 2-3min to be preheated in a vacuum induction furnace, argon is filled after moisture and gas are discharged, the mixture is lifted to the maximum power to be melted, and casting is carried out after the alloy is melted down and refined at low power for 10 min.
3. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 1, characterized in that: and step S5, cooling the crystallized material to 40 ℃ in a grading manner after the crystallization heat treatment, and discharging the material, wherein a three-stage water cooling manner is adopted, and the cooling speed is gradually increased.
4. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 1, characterized in that: in the step S5, the crystallization furnace is vacuumized to 10-2Pa, argon is filled to 0.03-0.04 Pa, and the rotation frequency of the furnace tube of the crystallization furnace is 22-28 Hz.
5. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 1, characterized in that: the double-sided wet-temperature treatment device comprises an oxidation treatment chamber (1), wherein a feed inlet (2) and a discharge outlet (9) are respectively arranged at the upper end and the lower end of the oxidation treatment chamber (1), a pair of fixed stand columns (3) are fixedly connected to the inner bottom end of the oxidation treatment chamber (1), the fixed stand columns (3) are installed on a stepping motor (5), an output end of the stepping motor (5) is fixedly connected with a single-layer treatment plate (4), a falling-preventing strip (11) is fixedly connected to the lower end of the single-layer treatment plate (4), a plurality of uniformly distributed automorphic separation columns (10) are arranged at one end, close to one end, of the single-layer treatment plate (4), a plurality of uniformly distributed atomization nozzles (8) are installed at one end, close to the single-layer treatment plate (4), of the installation plate (6), the atomizing nozzle (8) is connected with a booster water pump (7) through a pipeline.
6. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 5, characterized in that: the single-layer processing board (4) is internally provided with an electromagnet array (12), the single-layer processing board (4) is internally provided with a gas connecting pipe (13) in an inserting mode, the gas connecting pipe (13) is connected with an electric air pump (14) fixedly installed on a fixed upright post (3), the surface of the single-layer processing board (4) is provided with a plurality of expansion holes matched with the self-changing isolation posts (10), the expansion holes are smaller than the particle size of a magnetic powder sample, and the self-changing isolation posts (10) are made of elastic bag bags and communicated with the gas connecting pipe (13).
7. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 5, characterized in that: and a silica gel heating sheet (15) is arranged in the self-changing isolation column (10), the silica gel heating sheet (15) and the atomizing spray head (8) work synchronously, the initial temperature is 80-100 ℃, and after the high-humidity treatment is finished, the temperature is uniformly increased to 120-150 ℃ for drying.
8. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 5, characterized in that: the length of the self-changing isolation column (10) is one half of the particle size of the magnetic powder sample, the length of the self-changing isolation column is consistent with that of the anti-falling strip (11), and the distance between the pair of single-layer processing plates (4) is slightly larger than the particle size of the magnetic powder sample.
9. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 5, characterized in that: the atomizing spray head (8) sprays atomizing steam at intervals, and the standard that the surface of the magnetic powder sample is wetted but liquid beads cannot be seen by naked eyes is taken as a standard.
10. The preparation method of the permanent magnet powder applying double-sided wet and warm oxidation treatment according to claim 1, characterized in that: the magnetic property detection comprises the detection of remanence Br, intrinsic Hcb, intrinsic coercive force Hcj and magnetic energy product BH index.
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