CN103774036B - Nanodiffusion-reduction method prepares the method for neodymium iron boron - Google Patents
Nanodiffusion-reduction method prepares the method for neodymium iron boron Download PDFInfo
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Abstract
A kind of nanodiffusion-reduction method disclosed by the invention prepares the method for neodymium iron boron, specifically comprises the following steps: the 1) preparation of oxide nano rare earth colloidal sol; 2) preparation of neodymium iron boron blank; 3) the oxide nano rare earth diffusion of neodymium iron boron blank; 4) the desolventizing process of neodymium iron boron blank; 5) the neodymium iron boron blank after desolventizing process in step 4) is loaded sintering box sintering, last thermal treatment; Method of the present invention can keep remanent magnetism, the magnetic energy product that neodymium iron boron is very high, effectively can improve again the coercive force of neodymium iron boron magnetic body.
Description
Technical field
The present invention relates to a kind of method that nanodiffusion-reduction method prepares neodymium iron boron.
Background technology
Neodymium iron boron is primarily of Nd
2fe
14b, rich-Nd phase and rich B phase composite, wherein Nd
2fe
14b is Magnetic Phase, determines remanent magnetism and magnetic energy product, and the heterogeneous microstructure of rich-Nd phase and magnet determines the coercive force of magnet.Be difficult to prepare the neodymium iron boron simultaneously possessing high remanent magnetism and high-coercive force by traditional technology, the reduction of remanent magnetism will be caused to reach high-coercive force, coercitive decline will be caused to reach high remanent magnetism, the unacceptable product major part that the neodymium iron boron of prior art occurs in producing simultaneously is because coercive force is too low, has great importance to the product qualified rate that raising neodymium iron boron is produced as unacceptable product low for coercive force is processed into salable product by how lower cost.
Summary of the invention
Technical problem to be solved by this invention is, overcome the shortcoming of above prior art: provide a kind of nanodiffusion-reduction method to prepare the method for neodymium iron boron, the method can keep remanent magnetism, the magnetic energy product that neodymium iron boron is very high, effectively can improve again the coercive force of neodymium iron boron magnetic body.
Technical solution of the present invention is as follows: a kind of nanodiffusion-reduction method prepares the method for neodymium iron boron, specifically comprises the following steps:
1) preparation of oxide nano rare earth colloidal sol: rare earth oxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10-20 ︰ 1 loads abrasive dust in ball mill, and rareearth oxidate powder pellet is milled to the oxide nano rare earth that particle diameter is 20-30 nanometer; Again oxide nano rare earth is carried out Passivation Treatment, finally oxide nano rare earth is added in solvent that to be mixed with oxide nano rare earth colloidal sol for subsequent use, in described oxide nano rare earth colloidal sol, the weight percent of oxide nano rare earth is 38-76%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder prepared by powder metallurgic method compression moulding after orientation in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protection of inert gas, immerses in protection liquid (as sherwood oil) for subsequent use after reaching process requirement;
3) the oxide nano rare earth diffusion of neodymium iron boron blank: by step 2) in the neodymium iron boron blank for preparing after ultrasonic cleaning, activation treatment, immersing in the oxide nano rare earth colloidal sol prepared in step 1), is soak 2-4 hour in the oxide nano rare earth colloidal sol of 40-45 DEG C in temperature; Neodymium iron boron blank in this step can for the magnetic property unacceptable product after sintering, machining in neodymium iron boron production.DIFFUSION TREATMENT in nano-oxide colloidal sol is immersed by after unacceptable product cleaning, activation treatment;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and be evacuated to vacuum tightness: 10
-2-10
-3pa, Heating temperature extremely: 390-410 DEG C, was incubated after 120-150 minute, applying argon gas be cooled to 20-30 DEG C for subsequent use;
5) the neodymium iron boron blank after desolventizing process in step 4) is loaded sintering box, add granules of metal Ca, build lid and proceed in vacuum sintering furnace, be evacuated to 10
-2more than Pa, start heating, heating and temperature control is at 1000-1200 DEG C, be incubated after 2-4 hour, room temperature is cooled to the speed of 50 DEG C/more than s, finally heat-treat to obtain and qualified can keep remanent magnetism, the magnetic energy product that neodymium iron boron is very high, effectively can improve again the coercive-force neodymium-ferrum-boron permanent magnet of neodymium iron boron magnetic body.
As preferably, described rare earth oxide is the one in Praseodymium trioxide, Neodymium trioxide, dysprosium oxide, terbium sesquioxide, gadolinium sesquioxide, Holmium trioxide, praseodymium neodymium oxide.
As preferably, described solvent is the one in gasoline, sherwood oil.
As optimization, in step 2) in neodymium iron boron powder orientation number of times in magnetic field be more than 3 times.
As preferably, described sintering box is the one in graphite, quartzy box.
As optimization, the particle diameter of described granules of metal Ca is 2-4mm.
In step 5), the weight ratio of described neodymium iron boron blank and granules of metal Ca is 5-6 ︰ 1wt%.
Described thermal treatment comprises one-level ageing treatment, secondary time effect process.
The invention has the beneficial effects as follows: both maintained high remanent magnetism, magnetic energy product by the neodymium iron boron magnetic body of the inventive method preparation or process; The ultra-high coercive force that heavy rare earths of having got back produces is that fish and bear's paw get both; Jump out in traditional technology and namely wanted high-coercive force to give up remanent magnetism, high remanent magnetism must give up coercitive vicious circle.Magnetic property unacceptable product in adjustable production process of the present invention.Because the magnetic property unacceptable product in neodymium iron boron production, major part is that coercive force is low, method of the present invention can be adopted heavy rare earths to be seeped into the coercive force improving neodymium iron boron in defective neodymium iron boron, and then reach qualified coercive force, improves product qualified rate.Present invention reduces cost simultaneously, saved raw material, eliminate the operations such as part Rare earth metal metallurgy, melting processing, the broken powder process of hydrogen, shorten the production cycle, not only environmental protection, but also safety.
Embodiment
With specific embodiment, the present invention is described in further details below, but the present invention is not only confined to following specific embodiment.
Embodiment one
1) preparation of Nanometer-sized Neodymium Oxide colloidal sol: Neodymium trioxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10:1 loads in ball mill, and Neodymium trioxide powder is milled to the Nanometer-sized Neodymium Oxide that particle diameter is 20-30 nanometer; Again Nanometer-sized Neodymium Oxide is carried out Passivation Treatment, described Passivation Treatment is common process, finally Nanometer-sized Neodymium Oxide is added in sherwood oil that to be mixed with Nanometer-sized Neodymium Oxide colloidal sol for subsequent use, and in described Nanometer-sized Neodymium Oxide colloidal sol, the weight percent of Nanometer-sized Neodymium Oxide is 38%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder prepared by powder metallurgic method compression moulding after orientation in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protection of inert gas, immerses in sherwood oil for subsequent use after reaching process requirement;
3) the Nanometer-sized Neodymium Oxide diffusion of neodymium iron boron blank: by step 2) in the neodymium iron boron blank for preparing after ultrasonic cleaning, activation treatment, immersing the temperature prepared in step 1) is soak 3 hours in the Nanometer-sized Neodymium Oxide colloidal sol of 45 DEG C;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and vacuumize, be heated to 410 DEG C, be incubated after 120 minutes, applying argon gas be cooled to 25 DEG C for subsequent use;
5) the neodymium iron boron blank after desolventizing process in step 4) is loaded graphite, adding particle diameter is 2-4mm granules of metal Ca, and the weight ratio of described neodymium iron boron blank and granules of metal Ca is 5 ︰ 1, builds lid and proceeds in vacuum sintering furnace, be evacuated to 10
-2more than Pa, start heating, heating and temperature control is at 1200 DEG C, and be incubated after 3 hours, be cooled to room temperature with the speed of 50 DEG C/s, finally carry out normative heat treatment, ageing treatment can obtain neodymium iron boron.
Embodiment two
1) preparation of nano oxidized praseodymium colloidal sol: Praseodymium trioxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10:1 loads in ball mill, Praseodymium trioxide powder is milled to the nano oxidized praseodymium that particle diameter is 20-30 nanometer; Again nano oxidized praseodymium is carried out Passivation Treatment, finally nano oxidized praseodymium is added in gasoline that to be mixed with nano oxidized praseodymium colloidal sol for subsequent use, in described nano oxidized praseodymium colloidal sol, the weight percent of nano oxidized praseodymium is 56%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder powder metallurgic method prepared is compression moulding after orientation 3 times in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protection of inert gas, immerses in sherwood oil for subsequent use after reaching process requirement;
3) the nano oxidized praseodymium diffusion of neodymium iron boron blank: by step 2) in unacceptable product in the neodymium iron boron blank for preparing or neodymium iron boron production process after ultrasonic cleaning, activation treatment, immersing the temperature prepared in step 1) is soak 4 hours in the nano oxidized praseodymium colloidal sol of 40 DEG C;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and vacuumize, be heated to 390 DEG C, be incubated after 150 minutes, applying argon gas be cooled to 20 DEG C for subsequent use;
5) loaded in sintering box by the neodymium iron boron blank after desolventizing process in step 4), adding particle diameter is 2-4mm granules of metal Ca, and the weight ratio of described neodymium iron boron blank and granules of metal Ca is 6 ︰ 1, builds lid and proceeds in vacuum sintering furnace, be evacuated to 10
-2pa, start heating, heating and temperature control, at 1100 DEG C, is incubated after 4 hours, is cooled to room temperature with the speed of 50 DEG C/s, finally carry out one-level timeliness, secondary time effect process can obtain neodymium iron boron.
Embodiment three
1) preparation of nano oxidized dysprosium colloidal sol: dysprosium oxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10:1 loads in ball mill, dysprosium oxide powder is milled to the nano oxidized dysprosium that particle diameter is 20-30 nanometer; Again nano oxidized dysprosium is carried out Passivation Treatment, finally nano oxidized dysprosium is added in sherwood oil that to be mixed with nano oxidized dysprosium colloidal sol for subsequent use, in described nano oxidized dysprosium colloidal sol, the weight percent of nano oxidized dysprosium is 76%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder powder metallurgic method prepared is compression moulding after orientation 3 times in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under argon shield, immerses in sherwood oil for subsequent use after reaching the dimensional requirement of needs;
3) the nano oxidized dysprosium diffusion of neodymium iron boron blank: by step 2) in the neodymium iron boron blank for preparing after ultrasonic cleaning, activation treatment, immersing the temperature prepared in step 1) is soak 4 hours in the nano oxidized dysprosium colloidal sol of 45 DEG C;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and vacuumize, be heated to 400 DEG C, be incubated after 130 minutes, applying argon gas be cooled to 20 DEG C for subsequent use;
5) loaded in sintering box by the neodymium iron boron blank after desolventizing process in step 4), adding particle diameter is 2-4mm granules of metal Ca, and the weight ratio of described neodymium iron boron blank and granules of metal Ca is 5.5 ︰ 1, builds lid and proceeds in vacuum sintering furnace, be evacuated to 10
-2pa, start heating, heating and temperature control is at 1100 DEG C, and be incubated after 4 hours, be cooled to room temperature with the speed of 50 DEG C/s, finally carrying out traditional thermal treatment can obtain neodymium iron boron.
Embodiment four
1) preparation of nano oxidized gadolinium colloidal sol: gadolinium sesquioxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10:1 loads in ball mill, gadolinium sesquioxide powder is milled to the nano oxidized gadolinium that particle diameter is 20-30 nanometer; Again nano oxidized gadolinium is carried out Passivation Treatment, described Passivation Treatment is common process, finally nano oxidized gadolinium is added in sherwood oil that to be mixed with nano oxidized gadolinium colloidal sol for subsequent use, and in described nano oxidized gadolinium colloidal sol, the weight percent of nano oxidized gadolinium is 40%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder prepared by powder metallurgic method compression moulding after orientation in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protection of inert gas, immerses in sherwood oil for subsequent use after reaching process requirement;
3) the nano oxidized gadolinium diffusion of neodymium iron boron blank: by step 2) in the neodymium iron boron blank for preparing after ultrasonic cleaning, activation treatment, immersing the temperature prepared in step 1) is soak 3 hours in the nano oxidized gadolinium colloidal sol of 45 DEG C;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and vacuumize, be heated to 410 DEG C, be incubated after 120 minutes, applying argon gas be cooled to 25 DEG C for subsequent use;
5) the neodymium iron boron blank after desolventizing process in step 4) is loaded graphite, adding particle diameter is 2-4mm granules of metal Ca, and the weight ratio of described neodymium iron boron blank and granules of metal Ca is 5 ︰ 1, builds lid and proceeds in vacuum sintering furnace, be evacuated to 10
-2more than Pa, start heating, heating and temperature control is at 1200 DEG C, and be incubated after 3 hours, be cooled to room temperature with the speed of 50 DEG C/s, finally carry out normative heat treatment, ageing treatment can obtain neodymium iron boron.
Embodiment five
1) preparation of nano oxidized holmium colloidal sol: Holmium trioxide powder is crossed 120 mesh sieves, the ratio of grinding media to material mixing of then pressing 10:1 loads in ball mill, Holmium trioxide powder is milled to the nano oxidized holmium that particle diameter is 20-30 nanometer; Again nano oxidized holmium is carried out Passivation Treatment, finally nano oxidized holmium is added in gasoline that to be mixed with nano oxidized holmium colloidal sol for subsequent use, in described nano oxidized holmium colloidal sol, the weight percent of nano oxidized holmium is 70%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder powder metallurgic method prepared is compression moulding after orientation 3 times in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protection of inert gas, immerses in sherwood oil for subsequent use after reaching process requirement;
3) the nano oxidized holmium diffusion of neodymium iron boron blank: by step 2) in unacceptable product in the neodymium iron boron blank for preparing or neodymium iron boron production process after ultrasonic cleaning, activation treatment, immersing the temperature prepared in step 1) is soak 4 hours in the nano oxidized holmium colloidal sol of 40 DEG C;
4) the desolventizing process of neodymium iron boron blank: neodymium iron boron blank good for DIFFUSION TREATMENT in step 3) is put into heating under vacuum case and heat and vacuumize, be heated to 390 DEG C, be incubated after 150 minutes, applying argon gas be cooled to 20 DEG C for subsequent use;
5) loaded in sintering box by the neodymium iron boron blank after desolventizing process in step 4), adding particle diameter is 2-4mm granules of metal Ca, and the weight ratio of described neodymium iron boron blank and granules of metal Ca is 6 ︰ 1, builds lid and proceeds in vacuum sintering furnace, be evacuated to 10
-2pa, start heating, heating and temperature control, at 1100 DEG C, is incubated after 4 hours, is cooled to room temperature with the speed of 50 DEG C/s, finally carry out one-level timeliness, secondary time effect process can obtain neodymium iron boron.
Claims (6)
1. nanodiffusion-reduction method prepares a method for neodymium iron boron, it is characterized in that: specifically comprise the following steps:
1) preparation of oxide nano rare earth colloidal sol: rareearth oxidate powder pellet is milled to the oxide nano rare earth that particle diameter is 20-30 nanometer, again oxide nano rare earth is carried out Passivation Treatment, finally oxide nano rare earth is added in solvent that to be mixed with oxide nano rare earth colloidal sol for subsequent use, in described oxide nano rare earth colloidal sol, the weight percent of oxide nano rare earth is 38-76%;
2) preparation of neodymium iron boron blank: neodymium iron boron powder prepared by powder metallurgic method compression moulding after orientation in magnetic field, then carry out isostatic pressed process and obtain neodymium iron boron blank, neodymium iron boron blank is carried out mechanical workout under protective atmosphere, immerses in protection liquid for subsequent use after reaching requirement;
3) the oxide nano rare earth diffusion of neodymium iron boron blank: by step 2) in the neodymium iron boron blank for preparing after ultrasonic cleaning, activation treatment, immerse step 1) in the oxide nano rare earth colloidal sol for preparing, be soak 2-4 hour in the oxide nano rare earth colloidal sol of 40-45 DEG C in temperature;
4) the desolventizing process of neodymium iron boron blank: by step 3) in the good neodymium iron boron blank of DIFFUSION TREATMENT put into heating under vacuum case and heat and vacuumize, be heated to 390-410 DEG C, be incubated after 120-150 minute, applying argon gas be cooled to 20-30 DEG C for subsequent use;
5) by step 4) in neodymium iron boron blank after desolventizing process load sintering box, add granules of metal Ca, build lid and proceed in vacuum sintering furnace, be evacuated to 10
-2more than Pa, start heating, heating and temperature control, at 1000-1200 DEG C, is incubated after 2-4 hour, is cooled to room temperature, finally heat-treats and can obtain neodymium iron boron with the speed of 50 DEG C/s;
Described rare earth oxide is the one in Praseodymium trioxide, Neodymium trioxide, dysprosium oxide, terbium sesquioxide, gadolinium sesquioxide, Holmium trioxide, praseodymium neodymium oxide;
Described solvent is the one in gasoline, sherwood oil.
2. nanodiffusion-reduction method according to claim 1 prepares the method for neodymium iron boron, it is characterized in that: in step 2) in neodymium iron boron powder orientation number of times in magnetic field be more than 3 times.
3. nanodiffusion-reduction method according to claim 1 prepares the method for neodymium iron boron, it is characterized in that: described sintering box is the one in graphite, quartzy box.
4. nanodiffusion-reduction method according to claim 1 prepares the method for neodymium iron boron, it is characterized in that: the particle diameter of described granules of metal Ca is 2-4mm.
5. nanodiffusion-reduction method according to claim 1 prepares the method for neodymium iron boron, it is characterized in that: in step 5) in, the weight ratio of described neodymium iron boron blank and granules of metal Ca is 5-6:1.
6. nanodiffusion-reduction method according to claim 1 prepares the method for neodymium iron boron, it is characterized in that: described thermal treatment comprises one-level ageing treatment, secondary time effect process.
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| CN105081338B (en) * | 2014-05-08 | 2017-05-10 | 中国科学院宁波材料技术与工程研究所 | Method for preparing mono-dispersed NdFeB nano particles |
| CN105810425B (en) * | 2014-12-29 | 2020-04-24 | 天津三环乐喜新材料有限公司 | Manufacturing method of intensive sintered neodymium-iron-boron permanent magnet |
| CN105070498B (en) * | 2015-08-28 | 2016-12-07 | 包头天和磁材技术有限责任公司 | Improve the coercitive method of magnet |
| CN106935390B (en) * | 2015-12-31 | 2020-03-27 | 厦门钨业股份有限公司 | Surface treatment method of rare earth sintered magnet |
| CN110379578B (en) * | 2019-05-30 | 2021-03-12 | 宁波金科磁业有限公司 | Low-cost rare earth-free magnetic material and preparation method thereof |
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| CN101615459B (en) * | 2009-04-28 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | Method for improving performance of sintered Nd-Fe-B permanent magnetic material |
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