CN108115144B - Recycling method of rare earth alloy powder reclaimed material - Google Patents
Recycling method of rare earth alloy powder reclaimed material Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 255
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 173
- 239000000956 alloy Substances 0.000 title claims abstract description 173
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 161
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 151
- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004064 recycling Methods 0.000 title claims abstract description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000001301 oxygen Substances 0.000 claims abstract description 38
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 38
- 238000003801 milling Methods 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- 239000000654 additive Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 44
- 229910000583 Nd alloy Inorganic materials 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 14
- 239000000314 lubricant Substances 0.000 claims description 9
- 238000010902 jet-milling Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 239000006259 organic additive Substances 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 229910000636 Ce alloy Inorganic materials 0.000 claims description 4
- MAMCHKZYNGWYAS-UHFFFAOYSA-N [Sm].[Ce] Chemical compound [Sm].[Ce] MAMCHKZYNGWYAS-UHFFFAOYSA-N 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- -1 peroxide rare earth Chemical class 0.000 claims description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 4
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical group [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 238000005502 peroxidation Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 33
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 238000000465 moulding Methods 0.000 description 9
- 239000002699 waste material Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000012854 evaluation process Methods 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
Abstract
A recycling method of a rare earth alloy powder reclaimed material, wherein the rare earth alloy powder reclaimed material is first rare earth alloy powder with the average oxygen content of 0.2 wt% -1 wt%, and comprises the following steps: 1) adding the first rare earth alloy powder into an airflow milling device, wherein the airflow milling device is only provided with a gas nozzle at the bottom of a milling chamber, and performing impact treatment on the first rare earth alloy powder by using inert gas high-speed airflow with the oxygen content of less than 5ppm to obtain first rare earth alloy treated powder; mixing an additive powder having an average oxygen content of 0.15 wt% or less into the first rare earth alloy powder or the first rare earth alloy-treated powder; 2) obtaining mixed powder after the treatment of the step 1); 3) and sieving the mixed powder to obtain the required powder. The rare earth alloy powder or rare earth powder supplemented by the method of the invention has greatly reduced dosage and low production cost.
Description
Technical Field
The invention relates to a recycling method of an alloy powder reclaimed material, in particular to a recycling method of a rare earth alloy powder reclaimed material.
Background
The existing rare earth alloy powder has high component activity, micron-sized granularity and large specific surface area, and takes the neodymium iron boron alloy powder as an example, the neodymium iron boron alloy powder is very easy to oxidize and burn, so that the oxidized alloy powder and other abnormal materials are easy to generate in the neodymium iron boron production process, and the materials are scrapped.
The Chinese patent application CN104376943A discloses a method for recycling sintered neodymium iron boron formed waste, which comprises the steps of crushing the formed waste under the protection of nitrogen, adding the crushed waste into a conventional jet mill for dispersion to obtain dispersed waste fine powder, and mixing the dispersed waste fine powder with the same series of normal neodymium iron boron fine powder, an antioxidant and gasoline to obtain mixed magnetic powder, wherein the mixing ratio of the waste fine powder to the same series of normal neodymium iron boron fine powder is 1: 2-9.
The existing rare earth alloy waste recovery methods mainly aim at the formed rare earth alloy waste, but record how to recover oxidized rare earth alloy powder waste in the production process, how to efficiently recycle abnormal rare earth alloy powder recovered materials, and reduce the consumption of supplemented rare earth alloy powder, so that the problem to be solved urgently is to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling a rare earth alloy powder reclaimed material.
The technical scheme adopted by the invention for solving the technical problems is as follows: a recycling method of a rare earth alloy powder reclaimed material, wherein the rare earth alloy powder reclaimed material is first rare earth alloy powder with the average oxygen content of 0.2 wt% -1 wt%, and comprises the following steps:
1) adding the first rare earth alloy powder into an airflow milling device, wherein the airflow milling device is only provided with a gas nozzle at the bottom of a milling chamber, and performing impact treatment on the first rare earth alloy powder by using inert gas high-speed airflow with the oxygen content of less than 5ppm to obtain first rare earth alloy treated powder; mixing an additive powder having an average oxygen content of 0.15 wt% or less into the first rare earth alloy powder or the first rare earth alloy-treated powder;
wherein the added powder is micron-sized powder or nano-sized powder and is selected from at least one of second rare earth alloy powder or rare earth metal powder, and the adding amount of the added powder is 0 wt% -3 wt% of the mass of the first rare earth alloy powder;
2) obtaining mixed powder after the treatment of the step 1);
3) and sieving the mixed powder to obtain the required powder.
In the method for recycling the rare earth alloy powder reclaimed material, the air flow mill device is only provided with the air nozzle at the bottom of the milling chamber, namely the side nozzle of the milling chamber does not work or is not provided with the side nozzle, so that the over-crushing of the rare earth alloy powder is reduced, the generation of superfine powder is reduced, the loss of the rare earth material is reduced, the rare earth alloy powder added into the reclaimed material is less, even the rare earth alloy powder does not need to be added, and the recycling cost is greatly reduced. And the squareness and intrinsic coercive force of the magnet prepared from the powder obtained by the method for recycling the rare earth alloy powder reclaimed material are better.
Further, the first rare earth alloy treated powder has a particle size distribution ratio of D90 to D10 of 5.0 or less.
Thereby optimizing the consistency of the particle size distribution and improving the performance of the subsequent magnet product made from the powder.
Further, the first rare earth alloy powder with the average oxygen content of 0.2 wt% -1 wt% is partially peroxide rare earth alloy powder or wholly peroxide rare earth alloy powder.
The treatment effect of the method of the present invention is better when the average oxygen content of the first rare earth alloy powder is 1 wt% or less, and the method of the present invention is also effective but not optimal when the average oxygen content of the first rare earth alloy powder exceeds 1 wt%.
Further, the rotating speed of a sorting wheel of the airflow mill device is 2300rpm-3500 rpm.
When the rotating speed of the sorting wheel is more than 3500rpm, the powder treated by the jet mill is too fine and is easier to generate ultrafine powder, so that the loss of the rare earth material is aggravated; when the rotating speed of the sorting wheel is less than 2300rpm, the powder treated by the jet mill is too coarse, and the magnetic performance of the product is influenced.
Further, the first rare earth alloy powder is subjected to jet milling for 60 seconds or less.
The processing time of the rare earth alloy powder reclaimed material in the grinding chamber is shortened, the generation of ultrafine powder is reduced, and the loss of rare earth materials is reduced. Preferably, the first rare earth alloy powder is subjected to jet milling for 40 seconds or less.
Further, the second rare earth alloy powder is the same as the first rare earth alloy powder in terms of rare earth elements and metal elements, and the rare earth metal powder is the same as the first rare earth alloy powder in terms of rare earth elements.
By adding the additive powder of the same rare earth element and metal element, the performance of the magnet made of the mixed powder is better controlled.
Further, the first rare earth alloy powder and the second rare earth alloy powder are obtained by the following steps: a step of preparing an alloy for a rare earth magnet from a molten rare earth magnet component, and a step of coarsely pulverizing the alloy for a rare earth magnet and then finely pulverizing the coarsely pulverized alloy into fine powder; the first rare earth alloy powder is subjected to peroxidation in the preparation process or the storage process.
Further, the particle size D [3,2] of the first rare earth alloy powder, the second rare earth alloy powder, or the rare earth metal powder is 2.0 to 3.5 micrometers.
The granularity is measured by a Malvern laser granularity meter. The surface area volume average diameter of the first rare earth alloy powder and the second rare earth alloy powder or the rare earth metal powder is 2.0-3.5 microns, so that the first rare earth alloy powder and the second rare earth alloy powder or the rare earth metal powder can be mixed more uniformly.
Further, the pressure of a gas nozzle arranged at the bottom of the jet mill device is 0.5MPa-0.7 MPa.
By controlling the pressure of the gas nozzle to be 0.5MPa-0.7MPa, agglomerated powder can be scattered, and ultrafine powder is not easy to generate.
Further, the first rare earth alloy powder is Nd-Fe-B alloy powder, the second rare earth alloy powder is Pr-Nd alloy powder, or Nd-Fe-B alloy powder or Nd-M alloy powder or Nd-Pr-M alloy powder with the total rare earth content exceeding 30 wt%, M is a metal element except a rare earth metal element, and the rare earth metal powder is Nd powder.
Further, the first rare earth alloy powder is a samarium cobalt alloy powder reclaimed material, and the additive powder is at least one of samarium cerium alloy powder or samarium powder.
The technical scheme adopted by the invention for solving the technical problem is to provide a recycling method of rare earth alloy powder reclaimed materials, which comprises the following steps:
a) adding first rare earth alloy powder with the average oxygen content of 0.2-1 wt% into an airflow milling device, wherein the airflow milling device is only provided with a gas nozzle at the bottom of a milling chamber, and performing impact treatment on the first rare earth alloy powder by using inert gas high-speed airflow with the oxygen content of less than 5ppm to obtain treated powder;
b) adding an organic additive and an additive powder with the oxygen content of below 0.15 wt% into the treated powder, wherein the additive powder is at least one of micron-sized rare earth alloy powder or micron-sized rare earth metal powder, the additive amount of the additive powder is 0 wt% -3 wt% of the treated powder, uniformly mixing, and sieving to obtain mixed powder;
c) and carrying out orientation forming and sintering on the mixed powder to obtain the sintered rare earth magnet.
In the method for recycling the rare earth alloy powder reclaimed material, the air flow mill device is only provided with the air nozzle at the bottom of the milling chamber, namely the side nozzle of the milling chamber does not work or is not provided with the side nozzle, so that the over-crushing of the rare earth alloy powder is reduced, the generation of superfine powder is reduced, the loss of the rare earth material is reduced, the rare earth alloy powder added into the reclaimed material is less, even the rare earth alloy powder does not need to be added, and the recycling cost is greatly reduced. And the squareness and intrinsic coercive force of the magnet prepared by the method for recycling the rare earth alloy powder reclaimed material are better.
Furthermore, the organic additive is a lubricant, the addition amount of the lubricant is 0.03-0.2 wt%, and the mesh number of the sieving screen is 50-300 meshes.
Detailed Description
The present invention will be described in further detail with reference to examples.
The rare earth alloy powder reclaimed material is first rare earth alloy powder with the average oxygen content of 0.2 wt% -1 wt%.
The jet mill adopts a modified jet mill device, the jet mill device is only provided with a gas nozzle at the bottom of the milling chamber, namely the side nozzle of the milling chamber does not work or is not provided with the side nozzle, and the pressure of the gas nozzle arranged at the bottom is 0.5MPa-0.7 MPa. The conventional jet mill of the present invention is treated with a jet mill apparatus commonly used in the art.
The preparation method of the praseodymium-neodymium alloy powder added in the invention comprises the following steps: and preparing the praseodymium-neodymium molten liquid into praseodymium-neodymium alloy, and coarsely crushing the praseodymium-neodymium alloy in a hydrogen crushing mode and finely crushing the praseodymium-neodymium alloy in a conventional jet milling mode to obtain micron-grade praseodymium-neodymium alloy powder. Of course, the method for producing the added neodymium powder, samarium cerium alloy powder, samarium powder, Nd-Fe-B alloy powder, Nd-M alloy powder or Nd-Pr-M alloy powder can be referred to the above-mentioned method.
For the rare earth alloy powder reclaimed materials of different batches, sampling 3 parts of the rare earth alloy powder reclaimed materials every time, carrying out the steps of jet milling, sieving, forming, sintering and the like on 3 parts of samples to prepare the rare earth magnet, and deducing the quantity range of the rare earth alloy powder or the rare earth powder required to be supplemented by testing the performance of the magnet.
Example one
300Kg of neodymium iron boron alloy powder reclaimed material is taken, and the mass percentage of the components of the neodymium iron boron alloy is as follows:
adopt respectively table 1 different jet mill device or processing conditions handle the neodymium iron boron alloy powder reclaimed materials of different average oxygen content, neodymium iron boron alloy powder reclaimed materials local peroxide uses the inert gas high-speed air current that oxygen content is 5ppm below right neodymium iron boron alloy powder reclaimed materials carries out the impact treatment, obtains neodymium iron boron alloy and handles the powder, and the pressure of control mill room bottom gas nozzle is 0.6MPa, and the time that the jet mill handled the powder is 30 seconds, and the rotational speed of jet mill sorting wheel is 3500 rpm. Table 1 the axial extension of the 3 side nozzles in each comparative example has an intersection with the axial extension of the 1 bottom nozzle. The ratio of the particle size distribution D90 to D10 of the neodymium iron boron alloy treated powder treated by the jet milling in each test example is 2.1-4.5. The Nd-Fe-B alloy powder is mixed with Pr-Nd alloy powder with average oxygen content of 0.15 wt%, the addition of Pr-Nd alloy powder after airflow milling treatment in each test example and comparative example is shown in Table 1, the granularity D3, 2 of Pr-Nd alloy powder is 3.5 microns, and the granularity is tested by Malvern laser particle sizer. In table 1, the number of the grinding chamber side nozzles being 0 indicates that the grinding chamber side nozzles of the jet mill device do not operate or the side nozzles are not provided.
Table 1 process conditions for the respective test examples and comparative examples are as follows:
adding a lubricant into the mixed powder added with the praseodymium-neodymium alloy powder, wherein the addition amount of the lubricant is 0.2 wt% of the weight of the mixed powder, fully mixing the mixed powder by using a three-dimensional mixer, and sieving the mixed powder, wherein the mesh number of the sieve is 300 meshes.
The lubricant-added powder was once formed into a cube having a side length of 25mm in an orientation magnetic field of 1.8T at a forming pressure of 0.2ton/cm2 using a perpendicular orientation type magnetic field forming machine, and demagnetized in a magnetic field of 0.2T after the primary forming.
The molded article after the primary molding was sealed so as not to contact air, and then secondary molding was performed using a secondary molding machine (isostatic press) under a pressure of 1.4ton/cm 2.
The molded bodies were transferred to a sintering furnace and sintered at 10-3Pa at 200 deg.C and 850 deg.C for 1.5 hr, sintering at 1080 deg.C for 2 hr, introducing Ar gas to make pressure reach 0.1MPa, and cooling to room temperature.
The sintered body was subjected to heat treatment at 900 ℃ for 1.5 hours in high-purity Ar gas, cooled to room temperature, taken out, further subjected to heat treatment at 490 ℃ for 4 hours, cooled to room temperature, and taken out.
Magnetic property evaluation process: the sintered magnet is subjected to magnetic property detection by using an NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China measurement institute.
The evaluation results of the magnets of the test examples and comparative examples are shown in table 2:
TABLE 2 evaluation of magnetic Properties of test examples and comparative examples
As can be seen from Table 2, under the same oxygen content condition of the recovered Nd-Fe-B powder, the recovered Nd-Fe-B alloy powder treated by the jet mill of the present invention has obviously better Hcj and Hk/Hcj than the recovered Nd-Fe-B alloy powder treated by the conventional jet mill, and no obvious change in Br is observed. The neodymium-iron-boron alloy powder reclaimed material is treated by only arranging the bottom nozzle jet mill device, the addition amount of the praseodymium-neodymium alloy powder can also be reduced along with the reduction of the average oxygen content of the neodymium-iron-boron alloy powder reclaimed material, and the magnet Hcj has an ascending trend.
In the preferred embodiment, the difference from the first embodiment is that Nd-Fe-B alloy powder or Nd-M alloy powder or Nd-Pr-M alloy powder, in which the average oxygen content is 0.15 wt% or less and the total rare earth content exceeds 30 wt%, is mixed into the Nd-Fe-B alloy powder, and M is a metal element other than rare earth metal elements.
Example two
Taking 600Kg of recycled neodymium iron boron alloy powder, wherein the mass percentage of the components of the neodymium iron boron alloy is as follows:
adopt table 3 the jet mill processing conditions handle the neodymium iron boron alloy powder reclaimed materials of different average oxygen content, neodymium iron boron alloy powder reclaimed materials is local peroxide, and it is right to use the inert gas high-speed air current that oxygen content is 5ppm below to carry out the impact treatment with neodymium iron boron alloy powder reclaimed materials, obtain neodymium iron boron alloy and handle the powder, the mill room of jet mill device only bottom sets up gas nozzle, and the pressure of control mill room bottom gas nozzle is 0.7MPa, and the jet mill time and the sorting wheel rotational speed of each embodiment and comparative example are as table 3. The ratio of the particle size distribution D90 to D10 of the neodymium iron boron alloy treated powder treated by the jet milling in each test example is 3.2-5. The neodymium-iron-boron alloy powder is mixed with the praseodymium-neodymium alloy powder with the average oxygen content of 0.1 wt% and an organic additive, the addition amount of the praseodymium-neodymium alloy powder in each test example and each comparative example is shown in table 3, the particle size D [3,2] of the praseodymium-neodymium alloy powder is 2.0 microns, the particle size is tested by a Malvern laser particle sizer, the organic additive is a lubricant, and the addition amount of the lubricant is 0.1 wt% of the weight of the mixed powder.
Table 3 process conditions for the respective test examples and comparative examples are as follows:
and fully mixing the materials by using a three-dimensional mixer, and sieving the materials, wherein the mesh number of the sieve is 200 meshes.
The lubricant-added powder was once formed into a cube having a side length of 25mm in an orientation magnetic field of 1.8T at a forming pressure of 0.2ton/cm2 using a perpendicular orientation type magnetic field forming machine, and demagnetized in a magnetic field of 0.2T after the primary forming.
The molded article after the primary molding was sealed so as not to contact air, and then secondary molding was performed using a secondary molding machine (isostatic press) under a pressure of 1.4ton/cm 2.
The molded bodies were transferred to a sintering furnace and sintered at 10-3Pa at 200 deg.C and 850 deg.C for 1.5 hr, sintering at 1050 deg.C for 2 hr, introducing Ar gas to make pressure reach 0.1MPa, and cooling to room temperature.
The sintered body was heat-treated in high-purity Ar gas at 890 ℃ for 2 hours, cooled to room temperature, taken out, heat-treated at 480 ℃ for 3 hours, cooled to room temperature, and taken out.
Magnetic property evaluation process: the sintered magnet is subjected to magnetic property detection by using an NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China measurement institute.
The evaluation results of the magnets of the test examples and comparative examples are shown in table 4:
TABLE 4 evaluation of magnetic Properties of test examples and comparative examples
As can be seen from table 4, when the oxygen content ratio of the recycled neodymium-iron-boron powder is 0.9 wt%, the Hcj of the magnet tends to increase with the increase of the addition amount of the praseodymium-neodymium alloy powder, and when the addition amount of the praseodymium-neodymium alloy powder exceeds 3 wt%, the Br of the magnet is lower, and the production cost is too high. When the oxygen content of the recycled neodymium iron boron powder is 0.5 wt%, the Hcj of the magnet also tends to rise along with the increase of the addition of the praseodymium-neodymium alloy powder, and when the addition of the praseodymium-neodymium alloy powder exceeds 3 wt%, the Br of the magnet is lower, and the production cost is too high.
In a preferred embodiment, the praseodymium-neodymium alloy powder added to the neodymium-iron-boron alloy treated powder is in the nanometer scale.
EXAMPLE III
Taking 800Kg of neodymium iron boron alloy powder reclaimed material, wherein the neodymium iron boron alloy comprises the following components in percentage by mass:
adopt table 5 jet mill processing conditions handle average oxygen content is 0.6 wt%'s neodymium iron boron alloy powder reclaimed materials, the whole peroxide of neodymium iron boron alloy powder reclaimed materials mix into the additive amount and be 1.5 wt% and average oxygen content is 0.8 wt% neodymium powder in the neodymium iron boron alloy powder reclaimed materials, the granularity D [3,2] that adds the neodymium powder is 2.5 microns, the granularity adopts malvern laser particle sizer test. The neodymium-iron-boron alloy powder reclaimed material added with neodymium powder is subjected to impact treatment by using inert gas high-speed airflow with the oxygen content of less than 5ppm, only a gas nozzle is arranged at the bottom of a grinding chamber of the airflow grinding device, the pressure of the gas nozzle at the bottom of the grinding chamber is controlled to be 0.5MPa, and the airflow grinding time and the rotating speed of a sorting wheel of each embodiment and comparative example are shown in the table 5. The ratio of the particle size distribution D90 to D10 of the neodymium iron boron alloy treated powder treated by the jet milling in each test example is 3.0-4.7. And (4) obtaining mixed powder after the airflow milling treatment.
Table 5 process conditions for each test example and comparative example are as follows:
adding a lubricant into the mixed powder, wherein the adding amount of the lubricant is 0.03 wt% of the weight of the mixed powder, fully mixing the mixed powder by using a three-dimensional mixer, and sieving the mixed powder, wherein the mesh number of the sieve is 50 meshes.
The lubricant-added powder was once formed into a cube having a side length of 25mm in an orientation magnetic field of 1.8T at a forming pressure of 0.2ton/cm2 using a perpendicular orientation type magnetic field forming machine, and demagnetized in a magnetic field of 0.2T after the primary forming.
The molded article after the primary molding was sealed so as not to contact air, and then secondary molding was performed using a secondary molding machine (isostatic press) under a pressure of 1.4ton/cm 2.
The molded bodies were transferred to a sintering furnace and sintered at 10-3Pa at 200 ℃ and 850 ℃ for 1.5 hours, then 1060 ℃ for 4 hours, Ar gas was introduced to make the pressure 0.1MPa, and then the mixture was cooled to room temperature.
The sintered body was heat-treated in high-purity Ar gas at 910 ℃ for 1.5 hours, cooled to room temperature, taken out, heat-treated at 470 ℃ for 4 hours, cooled to room temperature, and taken out.
Magnetic property evaluation process: the sintered magnet is subjected to magnetic property detection by using an NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China measurement institute.
The evaluation results of the magnets of the test examples and comparative examples are shown in table 6:
TABLE 6 evaluation of magnetic Properties of test examples and comparative examples
As can be seen from Table 6, the average oxygen content of the recovered material was 0.6 wt%, the amount of neodymium powder added was 1.5 wt%, the final magnets Hcj and Hk/Hcj were lower at 1000rpm or 1500rpm of the classifying wheel, the final magnets Hcj and Hk/Hcj were lower at 4000rpm, 5000rpm or 6000rpm of the classifying wheel, and the final magnets Br, Hcj and Hk/Hcj exhibited better overall performance when the classifying wheel was rotated at 2300 ion 3500 rpm.
In a modified embodiment, the rare earth alloy powder reclaimed material is samarium cobalt alloy powder reclaimed material with the average oxygen content of 0.2 wt% to 1 wt%, and the added powder is at least one selected from samarium cerium alloy powder or samarium powder. The performance of the finally prepared magnet can meet the requirement of industrial production.
The object to be treated in the method for recycling rare earth alloy powder of the present invention is rare earth alloy powder for partial oxidation or total oxidation having an average oxygen content of 0.2 wt% to 1 wt%, and the method for recycling rare earth alloy powder reclaimed material of the present invention is applicable as long as the average oxygen content of the rare earth alloy powder reclaimed material is 0.2 wt% to 1 wt%.
The above embodiments are only intended to further illustrate some specific embodiments of the present invention, but the present invention is not limited to the embodiments, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention fall within the protection scope of the technical solution of the present invention.
Claims (11)
1. A recycling method of a rare earth alloy powder reclaimed material is characterized in that the rare earth alloy powder reclaimed material is first rare earth alloy powder with the average oxygen content of 0.2 wt% -1 wt%, and the recycling method comprises the following steps:
1) adding the first rare earth alloy powder into an airflow milling device, wherein the airflow milling device is only provided with a gas nozzle at the bottom of a milling chamber, and performing impact treatment on the first rare earth alloy powder by using inert gas high-speed airflow with oxygen content of less than 5ppm to obtain first rare earth alloy treated powder, wherein the pressure of the gas nozzle is 0.5-0.7 MPa; mixing an additive powder having an average oxygen content of 0.15 wt% or less into the first rare earth alloy powder or the first rare earth alloy-treated powder;
wherein the added powder is micron-sized powder or nano-sized powder and is selected from at least one of second rare earth alloy powder or rare earth metal powder, the adding amount of the added powder is 0 wt% -3 wt% of the mass of the first rare earth alloy powder, and the particle size D [3,2] of the first rare earth alloy powder, the second rare earth alloy powder or the rare earth metal powder is 2.0 microns-3.5 microns;
2) obtaining mixed powder after the treatment of the step 1);
3) and sieving the mixed powder to obtain the required powder.
2. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy-treated powder has a particle size distribution ratio of D90 to D10 of 5.0 or less.
3. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy powder with the average oxygen content of 0.2-1 wt% is partially peroxide rare earth alloy powder or wholly peroxide rare earth alloy powder.
4. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the rotating speed of a sorting wheel of the jet mill device is 2300rpm-3500 rpm.
5. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy powder has a jet milling treatment time of 60 seconds or less.
6. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the second rare earth alloy powder is the same as the first rare earth alloy powder in terms of rare earth elements and metal elements, and the rare earth metal powder is the same as the first rare earth alloy powder in terms of rare earth elements.
7. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy powder and the second rare earth alloy powder are obtained by the following steps: a step of preparing an alloy for a rare earth magnet from a melt of a rare earth magnet component and a step of pulverizing the alloy for a rare earth magnet into fine powder by coarse pulverization and then fine pulverization; the first rare earth alloy powder is subjected to peroxidation in the preparation process or the storage process.
8. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy powder is Nd-Fe-B alloy powder, the second rare earth alloy powder is Pr-Nd alloy powder, or Nd-Fe-B alloy powder or Nd-M alloy powder or Nd-Pr-M alloy powder with the total rare earth content exceeding 30 wt%, M is a metal element except a rare earth metal element, and the rare earth metal powder is Nd powder.
9. The method for recycling a reclaimed rare earth alloy powder according to claim 1, wherein: the first rare earth alloy powder is a samarium cobalt alloy powder reclaimed material, and the added powder is selected from at least one of samarium cerium alloy powder or samarium powder.
10. A recycling method of rare earth alloy powder reclaimed materials is characterized by comprising the following steps: the method comprises the following steps:
a) adding first rare earth alloy powder with the average oxygen content of 0.2-1 wt% into an airflow milling device, wherein the airflow milling device is only provided with a gas nozzle at the bottom of a milling chamber, and performing impact treatment on the first rare earth alloy powder by using inert gas high-speed airflow with the oxygen content of less than 5ppm to obtain treated powder, wherein the pressure of the gas nozzle is 0.5-0.7 MPa;
b) adding an organic additive and an additive powder with the average oxygen content of below 0.15 wt% into the treated powder, wherein the additive powder is at least one of micron-sized rare earth alloy powder or micron-sized rare earth metal powder, the additive amount of the additive powder is 0 wt% -3 wt% of the treated powder, and the particle size D [3,2] of the first rare earth alloy powder, the micron-sized rare earth alloy powder or the micron-sized rare earth metal powder is 2.0-3.5 microns, uniformly mixing, and sieving to obtain mixed powder;
c) and forming and sintering the mixed powder to obtain the sintered rare earth magnet.
11. The method of recycling a rare earth alloy powder reclaimed material according to claim 10, characterized in that: the organic additive is lubricant, the addition amount of the organic additive is 0.03-0.2 wt%, and the mesh number of the sieving screen is 50-300 meshes.
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Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee after: Fujian Jinlong Rare Earth Co.,Ltd. Country or region after: China Address before: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. Country or region before: China |