CN104576019A - Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials - Google Patents
Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials Download PDFInfo
- Publication number
- CN104576019A CN104576019A CN201410696475.9A CN201410696475A CN104576019A CN 104576019 A CN104576019 A CN 104576019A CN 201410696475 A CN201410696475 A CN 201410696475A CN 104576019 A CN104576019 A CN 104576019A
- Authority
- CN
- China
- Prior art keywords
- iron boron
- neodymium iron
- magnetic body
- boron magnetic
- waste material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Landscapes
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to an NdFeB (neodymium-iron-boron) magnet, in particular to a method for preparing the NdFeB magnet by waste materials, and belongs to the technical field of magnetic materials. The preparing method of the NdFeB magnet comprises the following steps that firstly, NdFeB magnet waste materials are cleaned and are dried through being blown, the NdFeB magnet waste materials are crushed into particles being 10 to 15mm by a crushing machine, rare earth metal is added into the particles, then, hydrogen crushing treatment is carried out to obtain crushed powder, and next, antioxidants are added for airflow grinding to obtain fine powder with the average particle diameter being 3.0 to 4.0 mu. m; next, lubricating agents are added, orientation is carried out under the protection atmosphere of nitrogen gas, in addition, pressing forming is carried out, and finally, NdFeB magnet finished products are obtained through discharging plasma sintering, secondary tempering heat treatment and surface treatment. The method has the advantages that waste materials are used as major raw materials, the simple and feasible preparing method is adopted, the recovery and utilization rate of the waste materials is effectively improved, in addition, Tb, Dy, Nd and Ce are added and compounded in the preparing process, and the obtained NdFeB magnet has better coercive force, residual magnetism and magnetic energy product.
Description
Technical field
The present invention relates to a kind of neodymium iron boron magnetic body, be specifically related to a kind of method utilizing waste material to prepare neodymium iron boron magnetic body, belong to technical field of magnetic materials.
Background technology
Neodymium iron boron magnetic body is as rare earth permanent-magnetic material of new generation, and having the features such as high remanent magnetism, high-coercive force and high energy product, is the permanent magnetic material that in the world today, comprehensive magnetic can be the strongest.Along with the development of electronic information, automobile and machinery manufacturing industry, neodymium iron boron magnetic body also obtains fast development, particularly now the environmental consciousness of people is more and more stronger, and the demand of Nd-Fe-B permanent magnet for the high combination property that can be used for the energy-conservation field of Environment Protection such as electric automobile, wind-powered electricity generation constantly increases.
Along with automobile, electronic device and other instrument and equipments constantly update and scrap, a large amount of neodymium iron boron magnetic body waste materials can be produced, and the fragility of neodymium iron boron magnetic body itself is larger, in the processes such as production, aft-loaded airfoil, all can produces a lot of waste material.And neodymium iron boron magnetic body itself is somewhat expensive material; the generation of a large amount of waste materials can increase into product cost greatly; waste material itself also can bring pollution simultaneously; and rare earth material is wherein non-renewable resources; from the angle consideration improving economic benefits, protection of the environment and economize on resources, make full use of neodymium iron boron magnetic body waste material imperative.At present, the method utilized for neodymium iron boron magnetic body waste recovery is a lot, such as: 1) by waste material again melting, more again sinters through series of process and obtains new neodymium iron boron magnetic body; 2) by waste material after hydrogen fragmentation, measure its composition, then the neodymium iron boron powder adding identical component mixes, then through airflow milling, suppress, sinter new neodymium iron boron magnetic body into; 3) from waste material, extract rare metal and other precious metals.These three kinds of methods all can reach the object recycling neodymium iron boron magnetic body waste material to a certain extent, but the rate of recovery is all not too high, and the performance of the new neodymium iron boron magnetic body obtained also decreases.
A kind of method utilizing waste material to prepare Nd Fe B alloys is disclosed in Chinese invention patent application file (publication number: CN1687470A), its main technique is the composition first determined in waste material, again after the operation such as it is dry through surface finish, peeling, melting and Homogenization Treatments, add in the ratio of 20-50% after slightly broken and essence breaks the powder making 3 μm-6 μm in new Nd Fe B alloys batching, eventually pass compacting and sintering obtains neodymium iron boron magnetic body.Although the method can play certain recovery effect, course of processing relative complex, and just add a small amount of waste material in new batching, recovery utilization rate is not high, and the magnetic property of neodymium iron boron magnetic body is also good not.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide one to utilize waste material, improve waste recovery utilance high, prepare the method for the good neodymium iron boron magnetic body of comprehensive magnetic energy.
Object of the present invention is achieved through the following technical solutions, and a kind of method utilizing waste material to prepare neodymium iron boron magnetic body, described method comprises the steps:
S1, waste material pre-treatment: cleaned by neodymium iron boron magnetic body waste material and dry up, become the particle of 10mm-15mm under inert gas shielding by crusher in crushing;
S2, powder process: rare earth metal will be added in above-mentioned waste granules and obtain through hydrogen break process the flour that average grain diameter is 10.0 μm-13.0 μm, then add antioxidant, mix laggard promoting the circulation of qi stream and grind average grain diameter is the fine powder of 3.0 μm-4.0 μm;
S3, compacting and sintering: in above-mentioned fine powder, add lubricant, again under the protective atmosphere of nitrogen, carry out orientation with the pulsed magnetic field of 3.5T-5.5T, the pressure of 200-220MPa and compressing, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process;
S4, tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment, finally carry out surface treatment and obtain neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 900-930 DEG C, and temperature retention time is 2.5-3.0h, and the temperature of second level tempering heat treatment is 500-620 DEG C, and temperature retention time is 2.0-3.5h.
The present invention take neodymium iron boron waste material as primary raw material, adopt the preparation method of simple possible, the recovery utilization rate of effective raising waste material, and compositely rare-earth metal Tb, Dy, Nd and Ce is added in the process of preparation, by they synergies in magnet, make the neodymium iron boron magnetic body obtained have good magnetic property, especially there is good coercive force, remanent magnetism and magnetic energy product.
Prepare in the method for neodymium iron boron magnetic body at the above-mentioned waste material that utilizes, the cleaning process described in step S1 is neodymium iron boron magnetic body waste material is placed in the Na that mass fraction is 30%-60%, temperature is 40-60 DEG C
2cO
34-8min is soaked in solution.Alkalescence is adopted not to be very large in the present invention, the Na that fail safe is high
2cO
3solution carries out decontamination process to neodymium iron boron waste material surface, and carries out at 40-60 DEG C, can promote that the indissoluble Substance Transformation of scraped surface is soluble substance, strengthens clean effect.Therefore, by neodymium iron boron waste material mass fraction be 30%-60%, temperature is the Na of 40-60 DEG C
2cO
3soak in solution, can effectively remove the impurity such as the greasy dirt on its surface, to prevent from producing harmful effect to the quality of neodymium iron boron magnetic body finished product in the follow-up course of processing.
Prepare in the method for neodymium iron boron magnetic body at the above-mentioned waste material that utilizes, the total content of the rare earth metal described in step S2 is 3.0%-5.0%.As preferably, described rare earth metal is the Ce of Nd, 0.8%-1.0% of Dy, 1.0%-2.0% of Tb, 0.5%-1.0% of 0.5%-1.0%.In neodymium iron boron magnetic body, improve the magnetic properties such as the coercive force of magnet usually through interpolation rare earth element as Pr, Nd, Dy, Gd, Ho, Tb etc.Rare earth element tb, Dy, Nd and Ce is added in neodymium iron boron magnetic body of the present invention, Tb and Dy is heavy rare earth, the saturated pole intensity of the compound that they are formed in NdFeB magnet is lower, but there is high anisotropy field, and there is temperature compensation function, therefore can improve coercive force and the temperature stability of magnet; And the saturated pole intensity of the compound that light rare earth Nd and Ce is formed in NdFeB magnet is higher, but effectively can improve remanent magnetism and the magnetic energy product of neodymium iron boron magnetic body, therefore heavy rare earth Tb, Dy and the composite of light rare earth Nd, Ce add, effectively can improve the coercive force of neodymium iron boron magnetic body, remanent magnetism and magnetic energy product, make the neodymium iron boron magnetic body obtained have good comprehensive magnetic energy.Although rare earth metal add the magnetic property that can improve neodymium iron boron magnetic body, but on the one hand because the price of rare earth metal is relatively high, particularly heavy rare earth, rare earth metal adds the magnetic property that too much can reduce magnet on the contrary on the other hand, therefore in the present invention, the total content of rare earth metal is controlled at 3.0%-5.0%, heavy rare earth Tb, Dy control at 0.5%-1.0%, and light rare earth Nd, Ce control respectively at 1.0%-2.0% and 0.8%-1.0%.
Prepare in the method for neodymium iron boron magnetic body at the above-mentioned waste material that utilizes, in the hydrogen break process described in step S2, the heating-up temperature of dehydrogenation reaction is 480-600 DEG C, and heating time is 200-240min.Compared with Mechanical Crushing flouring technology, hydrogen decrepitation can keep the integrality of crystal grain by the ratio reducing transgranular fracture in pulverizing process, and can suppress the abnormal growth of crystal grain in sintering process, thus effectively improves the combination property of magnet.For hydrogen decrepitation, its cardinal principle is rich neodymium phase and Nd
2fe
14b phase successively inhales hydrogen, causes volumetric expansion, and due to the difference of both expansion rates, cause producing internal stress at crystal grain intersection, along crystal boundary, alloy is then preferential occurs that crackle is broken for single crystal grain through External Force Acting.Hydrogen break process in the present invention comprises inhales hydrogen and dehydrogenation two processes, namely after first the particle after crusher in crushing being added rare earth metal, proceeding in reaction vessel and passing into hydrogen makes it inhale hydrogen to 0.20-0.22MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 480-600 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 200-240min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 70-90 DEG C, obtains flour after being cooled to room temperature.In the present invention, after hydrogen fragmentation, utilize the powder process of airflow milling technique, not only can by powder and air completely isolated, make the oxygen content of powder lower, and the particle diameter of final obtained powder particle can be made less, be conducive to the quality improving neodymium iron boron magnetic body final finished.And in the process of airflow milling, add a small amount of antioxidant and the neodymium iron boron magnetic body obtained then can be made to have better non-oxidizability.Wherein, antioxidant described in the present invention be triethanolamine borate, N-dodecyl bi-quaternary ammonium salt, tristerin one or more, its consumption is 0.01%-0.03%.
Prepare in the method for neodymium iron boron magnetic body at the above-mentioned waste material that utilizes, in order to reduce the friction between powder particle, preventing powder particle from reuniting thus improving the mobility of powder, after airflow milling, adding lubricant carry out orientation compacting again.But the addition of lubricant can not be too much, otherwise causing being difficult to deviate to reduce on the contrary magnet remanent magnetism and magnetic energy product completely when sintering, therefore in the present invention, the addition of lubricant being controlled at 0.01%-0.02%.Wherein, described lubricant is one or more in fat alcohol polyethylene ether, olein and lauryl sodium sulfate.
Prepare in the method for neodymium iron boron magnetic body at the above-mentioned waste material that utilizes, as preferably, in orientation and after pressing process, the present invention adopts discharge plasma sintering process to obtain neodymium iron boron magnetic body blank, wherein sintering atmosphere is vacuum degree is 0.012Pa-0.018Pa or argon gas atmosphere, and sintering pressure is 38-45MPa, and sintering temperature is 690-830 DEG C, heating rate is 130-180 DEG C/min, and temperature retention time is 4-8min.Discharge plasma sintering process is the pressure sintering method utilizing DC pulse resistance sintering; it can carry out in vacuum or protective atmosphere; have that programming rate is fast, sintering time is short, sintering temperature is low, uniform crystal particles, be conducive to controlling the fine structure of sintered body, and simple to operate, safe and reliable, energy savings, low cost and other advantages.Waste material is utilized to prepare in the method for neodymium iron boron magnetic body in the present invention, sintering temperature, sintering pressure, heating rate and the temperature retention time quality to obtained neodymium iron boron magnetic body has material impact, and the unreasonable of these parameters arranges the quality that all can reduce final neodymium iron boron magnetic body.Programming rate is too fast, sintering temperature is too high, makes grain growth speed fast and causes crystal grain abnormal large, reducing the performance of magnet, otherwise then do not reach the quality requirement of magnet; Sintering pressure increases in right amount effectively can suppress growing up and reducing sintering temperature of crystal grain, but sintering pressure is excessive, can make on the contrary to reduce density and these beneficial effects; Temperature retention time is long, crystal grain can be made during this period of time sharply to grow up, reduce magnetic property, temperature retention time is too short, and the density of magnet can be caused to reduce, and therefore sintering temperature, sintering pressure, heating rate and temperature retention time all control in suitable scope by the present invention.In addition, in the present invention, after sintering second annealing heat treatment and surface treatment are carried out to magnet, make final neodymium iron boron magnetic body have better combination property.Wherein, surface treatment is the common surface treatment process in this area.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention utilizes waste material to prepare neodymium iron boron magnetic body, at waste material on pretreated basis, compositely add heavy rare earth Tb, Dy and light rare earth Nd, Ce, by their reasonable disposition in neodymium iron boron magnetic body and synergy, the comprehensive magnetics such as the coercive force of the neodymium iron boron magnetic body obtained, remanent magnetism and magnetic energy product can be good.
2) the present invention utilizes waste material to prepare the method simple possible of neodymium iron boron magnetic body, and by the reasonable set of each technological parameter, the recovery utilization rate of neodymium iron boron magnetic body waste material is high, the good combination property of the neodymium iron boron magnetic body obtained.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Embodiment 1
Waste material pre-treatment: the waste material produced in N38 neodymium iron boron magnetic body production process is placed in the Na that mass fraction is 35%, temperature is 40 DEG C
2cO
3soak 5min in solution to carry out cleaning and drying up, under inert gas shielding, then become the particle of 10mm by crusher in crushing.
Powder process: account for the rare earth metal of the 3.0%-5.0% of neodymium iron boron magnetic body gross mass by adding content in above-mentioned waste granules and obtain through hydrogen break process the flour that average grain diameter is 10.0 μm, then the triethanolamine borate of 0.01% is added, mixing laggard promoting the circulation of qi stream grinds average grain diameter is the fine powder of 3.0 μm, and stirs 1.5h with mixer; Wherein rare earth metal is specially the Tb of 0.5%, Dy, the Nd of 1.0%, the Ce of 0.8% of 0.5%;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely after first the particle after crusher in crushing being added rare earth metal, proceeding in reaction vessel and passing into high-purity hydrogen (content >=99.99%) makes it inhale hydrogen to 0.20MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 480 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 200min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 70 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in the above-mentioned fine powder be stirred, add the fat alcohol polyethylene ether of 0.01%, again under the protective atmosphere of nitrogen, carry out orientation with the pulsed magnetic field of 3.5T, the pressure of 200MPa and compressing, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; The atmosphere of to be vacuum degree the be 0.012Pa of the sintering atmosphere wherein in discharge plasma sintering process, sintering pressure is 38MPa, and sintering temperature is 690 DEG C, and heating rate is 140 DEG C/min, and temperature retention time is 5min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment, finally carries out surface treatment and obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 900 DEG C, and temperature retention time is 2.5h, and the temperature of second level tempering heat treatment is 500 DEG C, and temperature retention time is 2.0h.
Embodiment 2
Waste material pre-treatment: the leftover pieces produced in the aft-loaded airfoil process of N38 neodymium iron boron magnetic body are placed in the Na that mass fraction is 45%, temperature is 50 DEG C
2cO
3soak 6min in solution to carry out cleaning and drying up, under inert gas shielding, then become the particle of 12mm by crusher in crushing.
Powder process: account for the rare earth metal of the 3.0%-5.0% of neodymium iron boron magnetic body gross mass by adding content in above-mentioned waste granules and obtain through hydrogen break process the flour that average grain diameter is 12.0 μm, then the N-dodecyl bi-quaternary ammonium salt of 0.02% is added, mixing laggard promoting the circulation of qi stream grinds average grain diameter is the fine powder of 4.0 μm, and stirs 2.0h with mixer; Wherein rare earth metal is specially the Tb of 0.8%, Dy, the Nd of 1.5%, the Ce of 0.9% of 0.8%;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely after first the particle after crusher in crushing being added rare earth metal, proceeding in reaction vessel and passing into high-purity hydrogen (content >=99.99%) makes it inhale hydrogen to 0.21MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 500 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 220min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 80 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in the above-mentioned fine powder be stirred, add the fat alcohol polyethylene ether of 0.01% and the olein of 0.01%, again under the protective atmosphere of nitrogen, carry out orientation with the pulsed magnetic field of 4.5T, the pressure of 210MPa and compressing, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; Sintering atmosphere wherein in discharge plasma sintering process is argon gas atmosphere, and sintering pressure is 40MPa, and sintering temperature is 750 DEG C, and heating rate is 160 DEG C/min, and temperature retention time is 6.5min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment, finally carries out surface treatment and obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 910 DEG C, and temperature retention time is 2.8h, and the temperature of second level tempering heat treatment is 550 DEG C, and temperature retention time is 3.0h.
Embodiment 3
Waste material pre-treatment: waste and old for N38 neodymium iron boron magnetic body is placed in the Na that mass fraction is 55%, temperature is 60 DEG C
2cO
3soak 7min in solution to carry out cleaning and drying up, under inert gas shielding, then become the particle of 14mm by crusher in crushing.
Powder process: account for the rare earth metal of the 3.0%-5.0% of neodymium iron boron magnetic body gross mass by adding content in above-mentioned waste granules and obtain through hydrogen break process the flour that average grain diameter is 13.0 μm, then the triethanolamine borate of 0.01% and the tristerin of 0.01% is added, mixing laggard promoting the circulation of qi stream grinds average grain diameter is the fine powder of 4.0 μm, and stirs 2.5h with mixer; Wherein rare earth metal is specially the Tb of 1.0%, Dy, the Nd of 1.5%, the Ce of 1.0% of 1.0%;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely after first the particle after crusher in crushing being added rare earth metal, proceeding in reaction vessel and passing into high-purity hydrogen (content >=99.99%) makes it inhale hydrogen to 0.22MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 600 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 240min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 90 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in the above-mentioned fine powder be stirred, add the lauryl sodium sulfate of 0.02%, again under the protective atmosphere of nitrogen, carry out orientation with the pulsed magnetic field of 5.5T, the pressure of 220MPa and compressing, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; Sintering atmosphere wherein in discharge plasma sintering process is vacuum degree is 0.015Pa atmosphere, and sintering pressure is 45MPa, and sintering temperature is 800 DEG C, and heating rate is 180 DEG C/min, and temperature retention time is 8min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment, finally carries out surface treatment and obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 930 DEG C, and temperature retention time is 3.0h, and the temperature of second level tempering heat treatment is 620 DEG C, and temperature retention time is 3.5h.
The obtained neodymium iron boron magnetic body of the waste material of N38 neodymium iron boron magnetic body will be utilized in embodiment 1-3 to carry out performance test, and the performance of the N38 neodymium iron boron magnetic body prepared with normal process compares, result is as shown in table 2.
The performance comparison result of the neodymium iron boron magnetic body that table 2: embodiment of the present invention 1-3 obtains and neodymium iron boron magnetic body prepared by normal process
Comparative example is N38 neodymium iron boron magnetic body prepared by normal process.
In sum, the present invention utilizes neodymium iron boron magnetic body waste material to prepare new neodymium iron boron magnetic body, and adding and the setting of rational technological parameter by heavy rare earth Tb, Dy and light rare earth Nd, Ce, the remanent magnetism of the neodymium iron boron magnetic body obtained and magnetic energy product exceed the general performance scope that normal process prepares the neodymium iron boron magnetic body of gained, coercive force significantly improves, and final demagnetization curve rectangular degree is high, make the magnetic property of magnet more stable.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (8)
1. utilize waste material to prepare a method for neodymium iron boron magnetic body, it is characterized in that, described method comprises the steps:
S1, waste material pre-treatment: cleaned by neodymium iron boron magnetic body waste material and dry up, become the particle of 10mm-15mm under inert gas shielding by crusher in crushing;
S2, powder process: rare earth metal will be added in above-mentioned waste granules and obtain through hydrogen break process the flour that average grain diameter is 10.0 μm-13.0 μm, then add antioxidant, mix laggard promoting the circulation of qi stream and grind average grain diameter is the fine powder of 3.0 μm-4.0 μm;
S3, compacting and sintering: in above-mentioned fine powder, add lubricant, again under the protective atmosphere of nitrogen, carry out orientation with the pulsed magnetic field of 3.5T-5.5T, the pressure of 200-220MPa and compressing, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process;
S4, tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment, finally carry out surface treatment and obtain neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 900-930 DEG C, and temperature retention time is 2.5-3.0h, and the temperature of second level tempering heat treatment is 500-620 DEG C, and temperature retention time is 2.0-3.5h.
2. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, is characterized in that, the cleaning process described in step S1 is neodymium iron boron magnetic body waste material is placed in the Na that mass fraction is 30%-60%, temperature is 40-60 DEG C
2cO
34-8min is soaked in solution.
3. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, is characterized in that, the total content of the rare earth metal described in step S2 is 3.0%-5.0%.
4. the waste material that utilizes according to claim 1 or 3 prepares the method for neodymium iron boron magnetic body, it is characterized in that, the rare earth metal described in step S2 is the Ce of Nd, 0.8%-1.0% of Dy, 1.0%-2.0% of Tb, 0.5%-1.0% of 0.5%-1.0%.
5. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, is characterized in that, in the hydrogen break process described in step S2, the heating-up temperature of dehydrogenation reaction is 480-600 DEG C, and heating time is 200-240min.
6. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, is characterized in that, the addition of the antioxidant described in step S2 is 0.01%-0.03%.
7. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, is characterized in that, the addition of the lubricant described in step S3 is 0.01%-0.02%.
8. the method utilizing waste material to prepare neodymium iron boron magnetic body according to claim 1, it is characterized in that, in discharge plasma sintering process described in step S3, sintering atmosphere is vacuum degree is 0.012Pa-0.018Pa or argon gas atmosphere, sintering pressure is 38-45MPa, sintering temperature is 690-830 DEG C, heating rate is 130-180 DEG C/min, and temperature retention time is 4-8min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410696475.9A CN104576019B (en) | 2014-11-26 | 2014-11-26 | Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410696475.9A CN104576019B (en) | 2014-11-26 | 2014-11-26 | Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104576019A true CN104576019A (en) | 2015-04-29 |
| CN104576019B CN104576019B (en) | 2017-02-22 |
Family
ID=53091847
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410696475.9A Expired - Fee Related CN104576019B (en) | 2014-11-26 | 2014-11-26 | Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104576019B (en) |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105274417A (en) * | 2015-10-20 | 2016-01-27 | 宁波科田磁业有限公司 | Method for utilizing neodymium iron boron airflow mill tailings for preparing neodymium iron boron magnetic steel |
| CN105957678A (en) * | 2016-06-30 | 2016-09-21 | 中铝广西有色金源稀土有限公司 | Method for recycling sintered NdFeB waste |
| TWI555041B (en) * | 2015-05-08 | 2016-10-21 | 中國鋼鐵股份有限公司 | Method of producing ndfeb magnet using ndfeb magnet waste |
| CN106158339A (en) * | 2016-06-22 | 2016-11-23 | 北京科技大学 | Sintered NdFeB reclaims the method that waste material prepares high-performance permanent magnet through diffusion penetration |
| CN106328364A (en) * | 2015-06-15 | 2017-01-11 | 中国钢铁股份有限公司 | Method for fabricating NdFeB magnet from waste NdFeB magnet |
| CN106373688A (en) * | 2016-08-31 | 2017-02-01 | 浙江东阳东磁稀土有限公司 | Method for preparing rare earth permanent magnet material |
| CN110090964A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of method that the waste recovery of rare-earth Nd-Fe-B coating recycles |
| CN110280770A (en) * | 2019-08-12 | 2019-09-27 | 哈尔滨工业大学 | A kind of method of discharge plasma sintering recycling light-alloy processing bit |
| CN110534331A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of high energy product, high-coercive force Sintered NdFeB magnet |
| CN111145997A (en) * | 2019-12-31 | 2020-05-12 | 慈溪市恒韵照明有限公司 | Preparation method of N30 type sintered mixed rare earth alloy magnetic material for improving coercive force |
| CN111921611A (en) * | 2020-09-08 | 2020-11-13 | 安徽万磁电子有限公司 | Waste treatment process for magnet machining |
| CN112017833A (en) * | 2020-08-20 | 2020-12-01 | 合肥工业大学 | Efficient utilization method of neodymium iron boron jet mill base material |
| CN112071546A (en) * | 2020-09-01 | 2020-12-11 | 安徽省瀚海新材料股份有限公司 | Processing method for producing modified neodymium-iron-boron magnet by using neodymium-iron-boron waste |
| CN112201428A (en) * | 2020-07-28 | 2021-01-08 | 宁波科田磁业有限公司 | Method for preparing high-performance magnetic steel by using neodymium iron boron reclaimed materials |
| CN112331474A (en) * | 2020-11-24 | 2021-02-05 | 北京工业大学 | Recycling method of neodymium iron boron block waste |
| CN112791765A (en) * | 2020-12-04 | 2021-05-14 | 横店集团东磁股份有限公司 | Bonded neodymium iron boron magnet recycling method |
| CN113223800A (en) * | 2021-04-28 | 2021-08-06 | 慈溪市兴发磁业科技有限公司 | Low-cost neodymium iron boron permanent magnet and preparation method thereof |
| CN117012538A (en) * | 2023-10-07 | 2023-11-07 | 江西荧光磁业有限公司 | Preparation process of neodymium-iron-boron magnet based on waste recovery |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1167524A (en) * | 1997-08-22 | 1999-03-09 | Meidensha Corp | Solder anticorrosive film forming method |
| JP2006077264A (en) * | 2004-09-07 | 2006-03-23 | Kenichi Machida | METHOD FOR RECYCLING RARE-EARTH SINTERED MAGNET AND TRANSITION-METAL BASED SCRAP, AND METHOD FOR MANUFACTURING MAGNETIC-MATERIAL POWDER FOR GHz BAND WAVE ABSORBER AND METHOD FOR MANUFACTURING WAVE ABSORBER |
| CN101562068A (en) * | 2009-01-20 | 2009-10-21 | 内蒙古科技大学 | Method for manufacturing neodymium iron boron permanent-magnet material by neodymium iron boron powder scrap |
| CN102723166A (en) * | 2012-06-29 | 2012-10-10 | 温州市南磁科技有限公司 | NdFeB permanent magnet and processing process thereof |
| CN102744406A (en) * | 2012-05-16 | 2012-10-24 | 华南理工大学 | Method for preparing fully dense anisotropic nanocrystalline neodymium-iron-boron (NdFeB) bulk magnet material |
| CN103440948A (en) * | 2013-08-16 | 2013-12-11 | 宁波科田磁业有限公司 | Reusing method for galvanization sintered neodymium iron boron waste |
| CN103646777A (en) * | 2013-12-11 | 2014-03-19 | 江苏大学 | Method for preparing crystal boundary nano-composite intensified neodymium iron boron magnet |
| CN103866127A (en) * | 2014-02-27 | 2014-06-18 | 中铝广西有色金源稀土股份有限公司 | Method for preparing neodymium iron boron through regenerating waste material containing neodymium, iron and boron |
-
2014
- 2014-11-26 CN CN201410696475.9A patent/CN104576019B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1167524A (en) * | 1997-08-22 | 1999-03-09 | Meidensha Corp | Solder anticorrosive film forming method |
| JP2006077264A (en) * | 2004-09-07 | 2006-03-23 | Kenichi Machida | METHOD FOR RECYCLING RARE-EARTH SINTERED MAGNET AND TRANSITION-METAL BASED SCRAP, AND METHOD FOR MANUFACTURING MAGNETIC-MATERIAL POWDER FOR GHz BAND WAVE ABSORBER AND METHOD FOR MANUFACTURING WAVE ABSORBER |
| CN101562068A (en) * | 2009-01-20 | 2009-10-21 | 内蒙古科技大学 | Method for manufacturing neodymium iron boron permanent-magnet material by neodymium iron boron powder scrap |
| CN102744406A (en) * | 2012-05-16 | 2012-10-24 | 华南理工大学 | Method for preparing fully dense anisotropic nanocrystalline neodymium-iron-boron (NdFeB) bulk magnet material |
| CN102723166A (en) * | 2012-06-29 | 2012-10-10 | 温州市南磁科技有限公司 | NdFeB permanent magnet and processing process thereof |
| CN103440948A (en) * | 2013-08-16 | 2013-12-11 | 宁波科田磁业有限公司 | Reusing method for galvanization sintered neodymium iron boron waste |
| CN103646777A (en) * | 2013-12-11 | 2014-03-19 | 江苏大学 | Method for preparing crystal boundary nano-composite intensified neodymium iron boron magnet |
| CN103866127A (en) * | 2014-02-27 | 2014-06-18 | 中铝广西有色金源稀土股份有限公司 | Method for preparing neodymium iron boron through regenerating waste material containing neodymium, iron and boron |
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI555041B (en) * | 2015-05-08 | 2016-10-21 | 中國鋼鐵股份有限公司 | Method of producing ndfeb magnet using ndfeb magnet waste |
| CN106328364A (en) * | 2015-06-15 | 2017-01-11 | 中国钢铁股份有限公司 | Method for fabricating NdFeB magnet from waste NdFeB magnet |
| CN105274417A (en) * | 2015-10-20 | 2016-01-27 | 宁波科田磁业有限公司 | Method for utilizing neodymium iron boron airflow mill tailings for preparing neodymium iron boron magnetic steel |
| CN106158339B (en) * | 2016-06-22 | 2019-01-11 | 北京科技大学 | The method that sintered NdFeB recycling waste material prepares high-performance permanent magnet through diffusion penetration |
| CN106158339A (en) * | 2016-06-22 | 2016-11-23 | 北京科技大学 | Sintered NdFeB reclaims the method that waste material prepares high-performance permanent magnet through diffusion penetration |
| CN105957678B (en) * | 2016-06-30 | 2018-01-02 | 中铝广西有色金源稀土有限公司 | A kind of method of sintered NdFeB materials recycling |
| CN105957678A (en) * | 2016-06-30 | 2016-09-21 | 中铝广西有色金源稀土有限公司 | Method for recycling sintered NdFeB waste |
| CN106373688A (en) * | 2016-08-31 | 2017-02-01 | 浙江东阳东磁稀土有限公司 | Method for preparing rare earth permanent magnet material |
| CN106373688B (en) * | 2016-08-31 | 2019-03-29 | 浙江东阳东磁稀土有限公司 | A method of preparing rare earth permanent-magnetic material |
| CN110090964A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of method that the waste recovery of rare-earth Nd-Fe-B coating recycles |
| CN110280770A (en) * | 2019-08-12 | 2019-09-27 | 哈尔滨工业大学 | A kind of method of discharge plasma sintering recycling light-alloy processing bit |
| CN110534331A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of high energy product, high-coercive force Sintered NdFeB magnet |
| CN111145997A (en) * | 2019-12-31 | 2020-05-12 | 慈溪市恒韵照明有限公司 | Preparation method of N30 type sintered mixed rare earth alloy magnetic material for improving coercive force |
| CN111145997B (en) * | 2019-12-31 | 2021-09-28 | 慈溪市兴发磁业科技有限公司 | Preparation method of N30 type sintered mixed rare earth alloy magnetic material for improving coercive force |
| CN112201428A (en) * | 2020-07-28 | 2021-01-08 | 宁波科田磁业有限公司 | Method for preparing high-performance magnetic steel by using neodymium iron boron reclaimed materials |
| CN112017833A (en) * | 2020-08-20 | 2020-12-01 | 合肥工业大学 | Efficient utilization method of neodymium iron boron jet mill base material |
| CN112017833B (en) * | 2020-08-20 | 2023-03-24 | 合肥工业大学 | Efficient utilization method of neodymium iron boron jet mill base material |
| CN112071546A (en) * | 2020-09-01 | 2020-12-11 | 安徽省瀚海新材料股份有限公司 | Processing method for producing modified neodymium-iron-boron magnet by using neodymium-iron-boron waste |
| CN112071546B (en) * | 2020-09-01 | 2024-04-12 | 安徽省瀚海新材料股份有限公司 | Processing method for producing modified NdFeB magnet by using NdFeB waste |
| CN111921611A (en) * | 2020-09-08 | 2020-11-13 | 安徽万磁电子有限公司 | Waste treatment process for magnet machining |
| CN111921611B (en) * | 2020-09-08 | 2021-11-16 | 安徽万磁电子有限公司 | Waste treatment process for magnet machining |
| CN112331474A (en) * | 2020-11-24 | 2021-02-05 | 北京工业大学 | Recycling method of neodymium iron boron block waste |
| CN112331474B (en) * | 2020-11-24 | 2022-06-07 | 北京工业大学 | Recycling method of neodymium iron boron block waste |
| CN112791765A (en) * | 2020-12-04 | 2021-05-14 | 横店集团东磁股份有限公司 | Bonded neodymium iron boron magnet recycling method |
| CN112791765B (en) * | 2020-12-04 | 2022-05-20 | 横店集团东磁股份有限公司 | Recycling method of bonded neodymium iron boron magnet |
| CN113223800A (en) * | 2021-04-28 | 2021-08-06 | 慈溪市兴发磁业科技有限公司 | Low-cost neodymium iron boron permanent magnet and preparation method thereof |
| CN117012538A (en) * | 2023-10-07 | 2023-11-07 | 江西荧光磁业有限公司 | Preparation process of neodymium-iron-boron magnet based on waste recovery |
| CN117012538B (en) * | 2023-10-07 | 2024-02-02 | 江西荧光磁业有限公司 | Preparation process of neodymium-iron-boron magnet based on waste recovery |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104576019B (en) | 2017-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104576019A (en) | Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials | |
| CN102211192B (en) | Method for preparing high-performance neodymium iron boron by using secondary recycled materials | |
| CN105575577B (en) | Sinter cerium-rich rare earth permanent-magnet material and preparation method thereof | |
| CN107316726A (en) | A kind of preparation method of sintered samarium cobalt magnet | |
| CN104575901A (en) | Neodymium iron boron magnet added with terbium powder and preparation method thereof | |
| CN104599801A (en) | Rare earth permanent magnetic material and preparation method thereof | |
| CN106971802A (en) | A kind of recycled sinter Nd-Fe-B permanent magnetic preparation | |
| CN104575902A (en) | Neodymium iron boron magnet added with cerium and preparation method thereof | |
| CN106158339B (en) | The method that sintered NdFeB recycling waste material prepares high-performance permanent magnet through diffusion penetration | |
| CN103794323A (en) | Commercial rare earth permanent magnet produced from high-abundance rare earth and preparing method thereof | |
| CN104801718A (en) | Recycling process of sintering neodymium iron boron discard black wafer | |
| CN103545079A (en) | Double-principal-phase yttrium-contained permanent magnet and preparing method of double-principal-phase yttrium-contained permanent magnet | |
| CN107689279A (en) | One kind improves the coercitive method of sintered NdFeB built-up magnet | |
| CN107564647A (en) | A kind of method that rare-earth Nd-Fe-B coating waste recovery recycles | |
| CN105355412A (en) | Method for obtaining high-magnetism sintered NdFeB through sulfidizing | |
| CN106847457A (en) | A kind of rare-earth permanent magnet and the method for preparing rare-earth permanent magnet | |
| CN106298134A (en) | A kind of double principal phase agglomeration permanent magnetic material and preparation method and application | |
| CN108447641A (en) | A kind of amorphous nano-crystalline iron-based composite soft magnetic alloy and preparation method thereof | |
| CN107442550A (en) | The recycling method of neodymium iron boron waste material after plating | |
| CN113871120B (en) | Mixed rare earth permanent magnet material and preparation method thereof | |
| CN104064303B (en) | A kind of didymium holmium yttrium multielement rare earth alloy permanent magnetic material and preparation method | |
| CN111210962A (en) | Sintered neodymium iron boron containing SmFeN or SmFeC and preparation method thereof | |
| CN106158214A (en) | A kind of preparation method of Re Fe B magnetic material | |
| CN113096952B (en) | Preparation method of neodymium iron boron magnetic material | |
| CN103045866A (en) | Method for recycling neodymium-iron-boron alloy scraps |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170222 Termination date: 20171126 |