CN112222415B - Method for preparing cobalt-based permanent magnet material by using cobalt-based reclaimed material - Google Patents
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Abstract
The application relates to a method for preparing a cobalt-based permanent magnet material by using a cobalt-based reclaimed material, belonging to the field of rare earth permanent magnet materials. Performing sand blasting treatment, melt casting and homogenization treatment on the cobalt-based reclaimed material, and performing air flow grinding to obtain metal powder; preparing alloy raw materials, and carrying out air flow grinding on the alloy powder raw materials to prepare alloy powder; and simultaneously adding an antioxidant and a lubricant to mix the metal powder and the alloy powder, and performing molding, isostatic pressing and sintering to obtain the final cobalt-based permanent magnet material.
Description
Technical Field
The application relates to a method for preparing a cobalt-based permanent magnet material by using a cobalt-based reclaimed material, belonging to the field of rare earth permanent magnet materials.
Background
The rare earth-cobalt-based permanent magnet material has excellent magnetic performance and temperature stability, and has important application in the high technical field. As the waste cobalt-based magnetic waste increases year by year, a process technology for recovering valuable metal resources from the waste cobalt-based magnetic waste is developed, and the method has no doubt important environmental protection significance and considerable economic benefit. The preparation method of the cobalt-based permanent magnet material in the actual production process at present mainly carries out alloying reaction through smelting to generate uniform metalate. The alloy is made into fine powder by powder metallurgy, the powder is oriented under a magnetic field to be made into a material, and then the material is sintered and magnetized in a high magnetic field, so that magnetic domains are ordered, and the permanent magnet material is obtained.
In the prior art, the recovery and regeneration method for cobalt-based magnetic waste generally has two modes: one is to directly smelt cobalt-based waste and alloy raw materials together, for example, chinese patent publication No. CN108560247A discloses a method for preparing finished samarium cobalt permanent magnet products by utilizing waste samarium cobalt permanent magnets, but the proportion of components is required to be known before smelting, and the use amount of powder is greatly limited. The other is to directly crush and grind the cobalt-based waste after cleaning, and the powder prepared by the method has impurity foreign matters, so that the final cobalt-based permanent magnet has a non-magnetic area, and the normal use of the product is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, which reduces impurities in the hard magnet material, avoids a non-magnetic area of a cobalt-based permanent magnet finished product and improves the quality of the cobalt-based permanent magnet.
The aim of the application is realized by the following technical scheme:
the preparation method comprises the steps of performing sand blasting treatment, melt casting, homogenization treatment and air flow grinding on the cobalt-based reclaimed material to obtain metal powder; preparing alloy raw materials, and carrying out air flow grinding on the alloy powder raw materials to prepare alloy powder; and simultaneously adding an antioxidant and a lubricant to mix the metal powder and the alloy powder, and performing molding, isostatic pressing and sintering to obtain the final cobalt-based permanent magnet material.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the sand blasting treatment specifically comprises the following steps: spraying abrasive to remove impurities on the surface of the reclaimed materials under the air pressure of 0.1-0.5 Mpa; the abrasive is one or more of steel sand, alumina, quartz sand and silicon carbide; the grain diameter of the abrasive is 1-3.5mm. The sprayed impurities mainly contain non-magnetic substances such as glue, paint, stains and the like, and the surface of the recycled material after the impurities are removed is bright. After sand blasting treatment, abrasive fine powder remains on the surface of the reclaimed material, and the surface is cleaned by gasoline to remove abrasive residue on the surface. Specifically, putting the cobalt-based reclaimed materials after sand blasting into a roller, adding gasoline for rolling for 5-30min, and then carrying out ventilation drying for 1-3 h.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the homogenization treatment temperature is 200-850 ℃ and the time is 2-10h. The alloy remelted by the reclaimed materials is subjected to high-temperature homogenization treatment, so that each element can be fully diffused in an alloy ingot, and the influence of smelting on magnetic performance is reduced.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the particle size of the metal powder obtained by the air current grinding is 1.0-4.0 mu m; the grain size of the alloy powder is 3.0-5 mu m. Because the cobalt-based reclaimed material is smelted, the intermediate oxygen and impurities of the alloy are removed, and the controllable oxygen content is required to be supplemented during air flow grinding, so that the magnetic performance is ensured; the granularity of the metal powder is controlled to be 1.0-4.0 mu m, the granularity of the alloy powder is controlled to be 3.0-5 mu m, and the granularity of the metal powder is finer than that of the alloy powder, because the thickness of the granularity of the powder can influence sintering temperature and magnetic property, and the configuration of different granularities can lead the metal powder and the alloy powder to be more uniform when being mixed, thereby reducing the use of lubricant.
In the above method for preparing cobalt-based permanent magnetic material by using cobalt-based reclaimed materials, the alloy powder raw material elements include: sm, co, cu, fe, zr.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the mass ratio of the metal powder to the alloy powder raw materials is (1-7) in the process of uniformly stirring the reclaimed metal powder and the alloy powder raw materials: (3-9). Because the cobalt-based recycled material is subjected to a series of procedures of primary smelting, powder preparation, forming, sintering, aging, remelting and the like, the actual components of the cobalt-based recycled material deviate greatly from the components of the original design formula. From ICP data analysis, mainly the content of the samarium is reduced, the content of the cobalt is increased, and the other elements are changed to different degrees, so that the raw materials of the metal powder and the alloy powder are required to be proportioned.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the antioxidant comprises the following components in percentage by mass: 0.5-60% fatty acid salt and 40-99.5% aviation gasoline.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the lubricant comprises the following components in percentage by mass: 60-80% of paraffin, 10-25% of gasoline and 5-15% of acetone.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the isostatic pressing specifically comprises the following steps: vacuum packaging the green body with plastic film, placing into an isostatic pressing machine, and maintaining the pressure for 10-90s under 150-300MPa oil pressure to obtain a blank.
In the method for preparing the cobalt-based permanent magnet material by using the cobalt-based reclaimed material, the final cobalt-based permanent magnet material comprises the following components in percentage by mass: sm:24% -27%, co:49% -52%, cu:5.0% -7.0%, fe:15% -18%, zr:2.0% -3.5% and the balance is unavoidable impurities.
Compared with the prior art, the application has the following advantages: in the process of preparing the cobalt-based permanent magnet by regenerating the cobalt-based waste, the impurities and oxygen in the cobalt-based reclaimed material are better removed by carrying out sand blasting treatment on the cobalt-based reclaimed material, and then the non-magnetic area of the cobalt-based permanent magnet finished product is greatly reduced by carrying out melt casting and homogenization treatment, so that the quality of the cobalt-based permanent magnet is improved; the method can be used for large-scale industrial production by simply adjusting the components of the metal reclaimed materials, and has the advantages of simple preparation process, short flow, low manufacturing cost and certain positive effect on environmental protection.
Detailed Description
The following are specific examples of the present application, and the technical solutions of the present application are further described, but the present application is not limited to these examples.
Example 1:
a method for preparing cobalt-based permanent magnet material by using cobalt-based reclaimed materials, the preparation method comprises the following steps:
(1) Sand blasting, namely pressing an abrasive into a nozzle by using air pressure of 0.5Mpa to spray the abrasive onto the surface of the cobalt-based reclaimed material, removing non-magnetic substances on the surface of the product, putting the cobalt-based reclaimed material into a roller, adding gasoline to roll for 20min, and then carrying out ventilation drying for 2h; the abrasive is a mixture of steel grit, alumina, quartz sand and silicon carbide; wherein the grain size of the steel sand is 2.5mm, the grain size of the alumina is 1.5mm, the grain size of the quartz sand is 2.0mm, and the grain size of the silicon carbide is 3.5mm.
(2) Smelting: and (3) smelting the cobalt-based reclaimed material subjected to sand blasting in a medium-frequency smelting furnace to obtain alloy liquid of the reclaimed material, injecting the alloy liquid into a water-cooling copper mold for cooling to obtain an alloy ingot, and then carrying out homogenization treatment at 500 ℃ for 6 hours.
(3) Pulverizing: coarse crushing, medium crushing and air flow grinding are carried out on the alloy cast ingot to obtain metal powder with the grain diameter of 3-4.5 mu m; preparing alloy raw materials, preparing alloy powder with the particle size of 3.5-5 mu m by air current grinding, and simultaneously adding an antioxidant and a lubricant to mix and stir the alloy powder and the alloy powder raw materials according to a ratio of 3:7, wherein the antioxidant is a mixture of 60% sodium stearate, 40% aviation gasoline, and the lubricant is 60% paraffin, 25% gasoline and 15% acetone; wherein the alloy powder comprises the following raw materials: 26%, co:48%, cu:6.2%, fe:18%, zr:2.9%.
(4) And (3) forming: carrying out orientation molding by a press, wherein the orientation magnetic field is more than or equal to 1.5T, and the density of the first molding is 4.0-5.0g/cm 3 Then placing the green body in an isostatic press for secondary pressing, wherein the oil pressure is 250Mpa, the dwell time is 60S, and the density of the green body is improved by 5.1g/cm 3 Above mentioned
(5) Sintering: and (3) placing the formed green body in a sintering furnace, sintering for 180mins at 1200 ℃, and then performing aging treatment to obtain the cobalt-based permanent magnet.
Example 2:
a method for preparing cobalt-based permanent magnet material by using cobalt-based reclaimed materials, the preparation method comprises the following steps:
(1) Sand blasting, namely pressing an abrasive into a nozzle by using air pressure of 0.3Mpa to spray the abrasive onto the surface of the cobalt-based reclaimed material, removing non-magnetic substances on the surface of the product, putting the cobalt-based reclaimed material into a roller, adding gasoline to roll for 15min, and then carrying out ventilation drying for 1h; the abrasive is a mixture of steel sand, alumina, quartz sand and the like; wherein the grain size of the steel sand is 2.5mm, the grain size of the alumina is 1.5mm, the grain size of the quartz sand is 2.0mm, and then the homogenization treatment is carried out at 600 ℃ for 5 hours.
(2) Smelting: and (3) placing the cobalt-based reclaimed material subjected to sand blasting treatment into a medium-frequency smelting furnace for smelting to obtain alloy liquid of the reclaimed material, and injecting the alloy liquid into a water-cooling copper mold for cooling to obtain an alloy ingot.
(3) Pulverizing: coarse crushing, medium crushing and air flow grinding are carried out on the alloy cast ingot to obtain metal powder with the grain diameter of 3-4.5 mu m; preparing alloy raw materials, preparing alloy powder with the particle size of 3.5-5 mu m by air current grinding, and simultaneously adding an antioxidant and a lubricant to mix and stir the alloy powder and the alloy powder raw materials according to the ratio of 4:6, wherein the antioxidant is a mixture of 55% sodium stearate, 45% aviation gasoline, and the lubricant is 80% paraffin, 10% gasoline and 10% acetone; wherein the alloy powder comprises the following raw materials: 25.5%, co:47%, cu:5.8%, fe:15%, zr:3.0%.
(4) And (3) forming: carrying out orientation molding by a press, wherein the orientation magnetic field is more than or equal to 1.5T, and the density of the first molding is 4.0-5.0g/cm 3 Then placing the green body in an isostatic press for secondary pressing, wherein the oil pressure is 150Mpa, the dwell time is 20S, and the density of the green body is improved by 5.1g/cm 3 Above mentioned
(5) Sintering: and (3) placing the formed green body in a sintering furnace, sintering for 180mins at 1200 ℃, and then performing aging treatment to obtain the cobalt-based permanent magnet.
Example 3:
a method for preparing cobalt-based permanent magnet material by using cobalt-based reclaimed materials, the preparation method comprises the following steps:
(1) Sand blasting, namely pressing an abrasive into a nozzle by using air pressure of 0.1Mpa to spray the abrasive onto the surface of the cobalt-based reclaimed material, removing non-magnetic substances on the surface of the product, putting the cobalt-based reclaimed material into a roller, adding gasoline to roll for 20min, and then carrying out ventilation drying for 2h; the abrasive is steel grit, wherein the grain diameter of the steel grit is 2.5mm, and then the homogenization treatment is carried out at 300 ℃ for 9 hours.
(2) Smelting: and (3) placing the cobalt-based reclaimed material subjected to sand blasting treatment into a medium-frequency smelting furnace for smelting to obtain alloy liquid of the reclaimed material, and injecting the alloy liquid into a water-cooling copper mold for cooling to obtain an alloy ingot.
(3) Pulverizing: coarse crushing, medium crushing and air flow grinding are carried out on the alloy cast ingot to obtain metal powder with the grain diameter of 3-4.5 mu m; preparing alloy raw materials, preparing alloy powder with the particle size of 3.5-5 mu m by air current grinding, and simultaneously adding an antioxidant and a lubricant to mix and stir the alloy powder and the alloy powder raw materials according to a ratio of 3:7, wherein the antioxidant is a mixture of 50% sodium stearate, 50% aviation gasoline, and the lubricant is 75% paraffin, 15% gasoline and 10% acetone; wherein the alloy powder comprises the following raw materials: 27%, co:50%, cu:7.0%, fe:20%, zr:4.0%.
(4) And (3) forming: carrying out orientation molding by a press, wherein the orientation magnetic field is more than or equal to 1.5T, and the density of the first molding is 4.0-5.0g/cm 3 Then placing the green body in an isostatic press for secondary pressing, wherein the oil pressure is 250Mpa, the dwell time is 60S, and the density of the green body is improved by 5.1g/cm 3 Above mentioned
(5) Sintering: and (3) placing the formed green body in a sintering furnace, sintering for 180mins at 1200 ℃, and then performing aging treatment to obtain the cobalt-based permanent magnet.
Comparative example 1:
the difference from example 1 is only that the raw materials are directly mixed as Sm:26%, co:48%, cu:6.2%, fe:18%, zr: and (2) forming, isostatic pressing and sintering 2.9% of alloy powder raw materials to obtain the cobalt-based permanent magnet.
Table 1: performance measurement result of permanent magnet characteristic measuring instrument for cobalt-based permanent magnet
The above results show that, overall, the cobalt-based permanent magnet prepared by regenerating the cobalt-based waste material has good magnetic performance, and the cobalt-based permanent magnet material still accords with the national standard, does not affect the use, and has lower cost because the cobalt-based permanent magnet material is prepared by directly utilizing the reclaimed material, although the magnetic performance is slightly lower than that of the cobalt-based permanent magnet material prepared by directly using the raw material. In general, the preparation method has the advantages of simple preparation process, short flow and low manufacturing cost, and the prepared cobalt-based permanent magnet material has high magnetic force and high stability.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the application. Various modifications or additions to the described embodiments may be made by those skilled in the art to which the application pertains or may be substituted in a similar manner without departing from the spirit of the application or beyond the scope of the appended claims.
While the application has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (1)
1. A method for preparing cobalt-based permanent magnet material by using cobalt-based reclaimed materials is characterized by comprising the steps of carrying out sand blasting treatment, melt casting, homogenization treatment and jet milling on the cobalt-based reclaimed materials to prepare metal powder; preparing alloy raw materials, and carrying out air flow grinding on the alloy powder raw materials to prepare alloy powder; simultaneously adding an antioxidant and a lubricant to mix the metal powder and the alloy powder, and preparing the cobalt-based permanent magnet material through molding, isostatic pressing and sintering;
the sand blasting treatment specifically comprises the following steps: spraying abrasive to remove impurities on the surface of the reclaimed materials under the air pressure of 0.5 Mpa; the abrasive is a mixture of steel grit, aluminum oxide, quartz sand and silicon carbide; wherein the grain size of the steel sand is 2.5mm, the grain size of the alumina is 1.5mm, the grain size of the quartz sand is 2.0mm, and the grain size of the silicon carbide is 3.5mm;
in the process of uniformly stirring the raw materials of the metal powder and the alloy powder, the mass ratio of the raw materials of the metal powder and the alloy powder is 3:7, preparing a base material;
the antioxidant comprises the following components in percentage by mass: 60% of fatty acid salt and 40% of aviation gasoline;
the cobalt-based permanent magnet material comprises the following components: sm:24% -27%, co:49% -52%, cu:5.0% -7.0%, fe:15% -18%, zr:2.0% -3.5%, and the balance is unavoidable impurities;
the homogenization treatment temperature is 500 ℃ and the time is 6 hours;
the grain diameter of the metal powder obtained by the air current grinding is 3-4.5 mu m; air flow grinding to obtain alloy powder with particle size of 3.5-5 μm;
the alloy powder comprises the following raw materials: 26%, co:48%, cu:6.2%, fe:18%, zr:2.9%;
the lubricant comprises the following components in percentage by mass: 60% paraffin, 25% gasoline and 15% acetone;
the isostatic pressing comprises the following specific steps: and (3) vacuum packaging the green body by using a plastic film, putting the green body into an isostatic pressing machine, and maintaining the pressure for 60s under the oil pressure of 250MPa to obtain a blank.
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