CN1414122A - Regeneration method of rare earth permanent magnet material - Google Patents
Regeneration method of rare earth permanent magnet material Download PDFInfo
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- CN1414122A CN1414122A CN01136628A CN01136628A CN1414122A CN 1414122 A CN1414122 A CN 1414122A CN 01136628 A CN01136628 A CN 01136628A CN 01136628 A CN01136628 A CN 01136628A CN 1414122 A CN1414122 A CN 1414122A
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- reworked
- hydrogen treat
- magnetic
- rare earth
- earth permanent
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
A process for regenerating the leftover of permanent-magnet RE alloy includes such steps as removing impurities, washing, drying, treating in H2 gas, breaking, fine grinding, adding R-enriched alloy powder, die pressing in magnetic field ,vacuum sintering in protecting atmosphere, and heat treating. Its advantages are high efficiency and magnetic property, and low cost.
Description
Technical field
The present invention relates to a kind of renovation process of rare earth permanent-magnetic material, belong to technical field of magnetic materials.
Background technology
Rare-Earth Cobalt type permanent magnetism (RCo
5, R
2Co
17And R
2Fe
14Type B) appearance has greatly improved the performance and the range of application of permanent magnet material.Simultaneously, rare earth permanent magnet can produce and is about 10% waste product and offal in processes such as sintering, processing, assembling, has influenced the utilization ratio of rare earth metal, has reduced economic benefit of enterprises.In order to reduce the magnet cost, existing people has invented some with rare earth permanent magnet spent material and tankage regenerating technique, mainly contain hydrometallurgical processes (referring to CN1174104A), dry process technology (referring to CN1127797A), Ca reducing process (referring to CN1272946A).The main drawback of hydrometallurgical processes is that complex process, the rate of recovery are low, cost is high, easy contaminate environment.The main drawback of dry process technology is that energy consumption is big, produce a large amount of slags in the fusion process, and homogeneity of product is poor, and the rare earth element recovery rate is low, and cost reduces limited.And the Ca reducing process is the same with hydrometallurgical processes, and complex process, the rate of recovery is low, cost is high, easy contaminate environment and will consume a large amount of Ca.
Also proposed materials recycling method in a kind of transition rare earth permanent-magnet production among the open CN1269587A of Chinese patent, its method is directly at N after waste material is cleaned
2Use mechanical means powder process in the gas, add a certain proportion of new powder again,, be prepared into transition rare earth permanent-magnet through moulding, sintering.The main drawback of this method is: because these offals and waste material are sintered compact, hardness is very high, be difficult to broken, after the cleaning directly at N
2Use mechanical means powder process in the gas, efficient is low, energy consumption is big, rich R loses many mutually; In addition, waste material is not classified, all must add new powder through overtesting in any offal and the waste material, the test work amount is big, and new powder addition is big, has increased cost.
Summary of the invention
The object of the invention is to propose a kind of renovation process of rare earth permanent-magnetic material, on the basis that guarantees to have than high magnetic characteristics, reduces production costs effectively.
For achieving the above object, the renovation process of the rare earth permanent-magnetic material of the present invention's proposition carries out according to the following steps:
(1) at first the reworked materials such as offal, defective material and waste material of RE permanent magnetic alloy is removed foreign material, clean, deoil, drying;
(2) above-mentioned drying is good reworked material places the hydrogen treat device, is evacuated to below the 10Pa, in logical then hydrogen to 0.1～1.0MPa scope, and keeps 20～40 minutes, and reworked material becomes thick magnetic after hydrogen treat;
(3) with the thick magnetic after the hydrogen treat, fine powder is broken to 2～12 μ m;
(4) in the fine powder after hydrogen treat, add the rich R alloy powder of 0～40% (mass percent);
(5) be 0.5～3 ton/cm with fine powder at pressure
2, carry out moulding under magneticstrength 〉=12.0kOe condition;
(6) with above-mentioned shaped object sintering under protective atmosphere or vacuum, 1080～1125 ℃ of sintering temperatures are incubated 2～4 hours;
(7) magnet behind the sintering after heat treatment is rare earth permanent-magnetic material of the present invention.
For reducing the consumption of rich rare earth alloy, reduce cost, reworked material is divided into non-oxide reworked material and the reworked material that contains the oxidation material, carry out hydrogen treat respectively.In the non-oxide reworked material fine powder after hydrogen treat, add rich R alloy powder, in containing the reworked material fine powder of oxidation material, add the rich R alloy powder of 5～40% (mass percents) less than 5% (mass percent).
With technology of the present invention reworked material directly can be prepared magnetic or magnet, not need to smelt again, technology is simple, and is easy to reworked material is broken into meal and fine powder, efficient height, rich R alloy powder addition is few simultaneously, so greatly reduce production cost.
Embodiment
The used starting material of the present invention are offal, defective material and the waste material etc. of rare earth permanent magnet, are commonly referred to as reworked material.Reworked material is divided into non-oxide reworked material and contains oxidation material reworked material two big classes, and non-oxide reworked material and qualified product have essentially identical chemical ingredients and magnetic property, contain oxidation material reworked material and then contain very high oxygen level, and magnetic energy product is very low.At first two big class reworked materials are removed foreign material, clean, deoil, drying; Adopt the hydrogen treat method, the non-oxide reworked material that drying is good places the hydrogen treat device respectively with the reworked material that contains the oxidation material, is evacuated to below the 10Pa, in logical then hydrogen to 0.1～1.0MPa scope, and keeps 20～40 minutes.Reworked material becomes thick magnetic after hydrogen treat.Because the hydrogen treat method is to utilize the rare earth permanent-magnetic material alloy to cause alloy pulverization inhaling the intercrystalline cracking that hydrogen process interalloy itself produced and the characteristic of transgranular fracture, obtains the alloy coarse meal of certain particle size.By the thick alloy powder of rare earth permanent magnet that the hydrogen treat method makes, its fragility is very big, and it is broken and prepare fine powder to be easy to carry out fine powder, the powdered preparation time is short, the oxidation of alloy in pulverizing process is low, and the oxidation-resistance of hydride is very strong, thereby can prepare the magnet of superior performance; Utilize airflow milling, ball milling etc. that the thick magnetic fine powder after the hydrogen treat is broken into 2～12 μ m fine powders; Before the moulding, the rich R alloy powder that in containing the reworked material fine powder of oxidation material, adds 5～40% (mass percents), to supply the required enough rich R phases of final sintered magnet, in non-oxide reworked material fine powder, add rich R alloy powder, can effectively reduce the consumption of rich rare earth alloy like this less than 5% (mass percent); Is 0.5～3 ton/cm with above fine powder at pressure
2, carry out pressure forming under magneticstrength 〉=12.0kOe condition.In order to obtain the rare earth permanent magnet reworked material base substrate of better quality, can be at 2～4 tons/cm
2Condition is carried out isostatic cool pressing; With shaped object sintering under protective atmosphere or vacuum, 1080～1125 ℃ of sintering temperatures are incubated 2～4 hours; Magnet behind the sintering is cooled to 900～950 ℃, is incubated 1～2 hour, is chilled to room temperature with the speed of 60～100 ℃/min.And then be heated to 500～650 ℃, and be incubated after 3 hours, be chilled to room temperature with the speed of 60～100 ℃/min.Be rare earth permanent-magnetic material of the present invention after the cooling.
Embodiment 1
Get SmCo
5Non-oxide reworked material is removed foreign material, cleans, deoils, drying.The raw material that above-mentioned drying is good places the device of hydrogen treat, is evacuated to below the 1Pa, and logical then hydrogen keeps after 30 minutes to 0.1MPa, obtains mean particle size less than 2 millimeters meal.This meal is worn into about 5 microns fine powder with airflow milling, is 2 tons/cm at pressure again
2, carry out pressure forming under the magneticstrength 15kOe condition, make blank.With blank sintering under argon gas, 1125 ℃ of sintering temperatures are incubated 2 hours, are cooled to 900 ℃ with the speed of 0.7 ℃/min, are incubated 1 hour, are chilled to room temperature with the speed of 60 ℃/min.Measure B
r=9.6kGs, iH
c=26.7kOe, (BH)
Max=21.8MGOe.
Embodiment 2
With Nd
15Fe
76.5Al
0.5B
8Non-oxide offal and waste material remove foreign material, clean, deoil, drying.The raw material that above-mentioned drying is good places the device of hydrogen treat, is evacuated to below the 10Pa, and logical then hydrogen is to 0.1MPa, and keeps 20 minutes, obtains mean particle size less than 2 millimeters meal.This meal is worn into about 5 microns fine powder with airflow milling, is Nd:44wt% with this fine powder and 3% nominal composition again, Fe:55wt%, and the rich Nd alloy powder of B:1wt% mixes.Is 2 tons/cm with this mixing fine powders at pressure
2, carry out pressure forming under the magneticstrength 20kOe condition, again at 2 tons/cm
2Condition is carried out isostatic cool pressing, makes blank.With blank sintering under vacuum state, 1080 ℃ of sintering temperatures are incubated 3 hours, with 900 ℃ of the speed of 10 ℃/min coolings, are incubated 2 hours, are chilled to room temperature with the speed of 60 ℃/min.Be heated to 600 ℃ then, be incubated after 3 hours, be chilled to room temperature with the speed of 60 ℃/min.Measure B
r=12.3kGs,
iH
c=17.8kOe, (BH)
Max=35.5MGOe.
Embodiment 3
With Nd
1.5Fe
76.5Al
0.5B
8Offal that contains the oxidation material and waste material remove foreign material, clean, deoil, drying.The raw material that above-mentioned drying is good places the device of hydrogen treat, is evacuated to below the 1Pa, and logical then hydrogen is to 1.0MPa, and keeps 40 minutes, obtains mean particle size less than 2 millimeters meal.This meal is worn into about 5 microns fine powder with airflow milling.Be Nd:44wt% with this fine powder and 20% nominal composition again, Fe:55wt%, the rich Nd alloy powder of B:1wt% mixes.Is 2 tons/cm with this mixed powder at pressure
2, carry out pressure forming under the magneticstrength 20kOe condition, again at 2 tons/cm
2Carry out isostatic cool pressing under the condition, make blank.With blank sintering under vacuum, 1110 ℃ of sintering temperatures are incubated 3 hours, with 900 ℃ of the speed of 10 ℃/min coolings, are incubated 2 hours, are chilled to room temperature with the speed of 60 ℃/min.Be heated to 600 ℃ then, be incubated after 3 hours, be chilled to room temperature with the speed of 60 ℃/min.Measure B
r=12.0kGs,
iH
c=16.5kOe, (BH)
Max=33.5MGOe.
Embodiment 4
With Nd
15Fe
76.5Nb
0.5B
8The reworked material that contains the oxidation material remove foreign material, clean, deoil, drying.The raw material that above-mentioned drying is good places the device of hydrogen treat, is evacuated to below the 5Pa, and logical then hydrogen is to 0.5MPa, and keeps 40 minutes, obtains mean particle size less than 2 millimeters meal.This meal is worn into about 5 microns fine powder with airflow milling.Be Nd:44wt% with this fine powder and 40% nominal composition again, Fe:55wt%, the rich Nd alloy powder of B:1wt% mixes.Is 2 tons/cm with this mixed powder at pressure
2, carry out under the magneticstrength 20kOe condition just molded, again at 2 tons/cm
2Carry out isostatic cool pressing under the condition, make blank.With blank sintering under vacuum, 1125 ℃ of sintering temperatures are incubated 3 hours, with 900 ℃ of the speed of 10 ℃/min coolings, are incubated 2 hours, are chilled to room temperature with the speed of 60 ℃/min.Be heated to 600 ℃ then, be incubated after 3 hours, be chilled to room temperature with the speed of 60 ℃/min.Measure B
r=10.5kGs,
iH
c=17.5kOe, (BH)
Max=25MGOe.
Claims (4)
1. the renovation process of a rare earth permanent-magnetic material in turn includes the following steps:
(1) at first the reworked materials such as offal, defective material and waste material of RE permanent magnetic alloy is removed foreign material, clean, deoil, drying;
(2) above-mentioned drying is good reworked material places the hydrogen treat device, is evacuated to below the 10Pa, in logical then hydrogen to 0.1～1.0MPa scope, and keeps 20～40 minutes, and reworked material becomes thick magnetic after hydrogen treat;
(3) with the thick magnetic after the hydrogen treat, fine powder is broken to 2～12 μ m;
(4) will carefully confusingly expect to be 0.5～3 ton/cm at pressure
2, carry out moulding under magneticstrength 〉=12.0kOe condition;
(5) with above-mentioned shaped object sintering under protective atmosphere or vacuum, 1080～1125 ℃ of sintering temperatures are incubated 2-4 hour;
(6) magnet behind the sintering after heat treatment is rare earth permanent-magnetic material of the present invention.
2. in accordance with the method for claim 1, its feature is being divided into reworked material non-oxide reworked material and two kinds of the reworked materials that contains the oxidation material, and carries out hydrogen treat respectively.
3. according to claim 1,2 described methods, it is characterized in that adding after the non-oxide reworked material hydrogen treat rich R alloy powder less than 5% (mass percent).
4. according to claim 1,2 described methods, it is characterized in that containing the rich R alloy powder that adds 5%-40% (mass percent) in the fine powder of reworked material after hydrogen treat of oxidation material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011366281A CN1173051C (en) | 2001-10-23 | 2001-10-23 | Regeneration method of rare earth permanent magnet material |
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|---|---|---|---|
| CNB011366281A CN1173051C (en) | 2001-10-23 | 2001-10-23 | Regeneration method of rare earth permanent magnet material |
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|---|---|
| CN1414122A true CN1414122A (en) | 2003-04-30 |
| CN1173051C CN1173051C (en) | 2004-10-27 |
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ID=4673789
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011366281A Expired - Fee Related CN1173051C (en) | 2001-10-23 | 2001-10-23 | Regeneration method of rare earth permanent magnet material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100454449C (en) * | 2006-04-24 | 2009-01-21 | 严高林 | Method for regenerating high-performance permanent magnet by degenerated rare earth permanent magnet material |
| CN102146514A (en) * | 2010-02-05 | 2011-08-10 | 中国科学院宁波材料技术与工程研究所 | Method for regenerating anisotropic rare-earth permanent-magnet material |
| CN102453804A (en) * | 2010-10-20 | 2012-05-16 | 宁波科宁达工业有限公司 | Method for recycling waste and old nickel-plated rare-earth-iron-boron series permanent magnet material |
| CN104668567A (en) * | 2015-02-10 | 2015-06-03 | 北京工业大学 | Method for recycling compression molding waste bonded magnet by use of resin swelling washing method |
| CN108666127A (en) * | 2018-06-04 | 2018-10-16 | 安徽天宇磁业股份有限公司 | Based on energy-saving and environment-friendly permanent magnet processing technology |
| CN109396444A (en) * | 2018-11-05 | 2019-03-01 | 湖南航天磁电有限责任公司 | A kind of processing method of sintered samarium cobalt permanent magnet tailing |
-
2001
- 2001-10-23 CN CNB011366281A patent/CN1173051C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100454449C (en) * | 2006-04-24 | 2009-01-21 | 严高林 | Method for regenerating high-performance permanent magnet by degenerated rare earth permanent magnet material |
| CN102146514A (en) * | 2010-02-05 | 2011-08-10 | 中国科学院宁波材料技术与工程研究所 | Method for regenerating anisotropic rare-earth permanent-magnet material |
| CN102146514B (en) * | 2010-02-05 | 2013-06-19 | 中国科学院宁波材料技术与工程研究所 | Method for regenerating anisotropic rare-earth permanent-magnet material |
| CN102453804A (en) * | 2010-10-20 | 2012-05-16 | 宁波科宁达工业有限公司 | Method for recycling waste and old nickel-plated rare-earth-iron-boron series permanent magnet material |
| CN102453804B (en) * | 2010-10-20 | 2015-11-25 | 宁波科宁达工业有限公司 | A kind of regeneration method of waste and old nickel-plated rare-earth-iron-boron series permanent magnet |
| CN104668567A (en) * | 2015-02-10 | 2015-06-03 | 北京工业大学 | Method for recycling compression molding waste bonded magnet by use of resin swelling washing method |
| CN108666127A (en) * | 2018-06-04 | 2018-10-16 | 安徽天宇磁业股份有限公司 | Based on energy-saving and environment-friendly permanent magnet processing technology |
| CN109396444A (en) * | 2018-11-05 | 2019-03-01 | 湖南航天磁电有限责任公司 | A kind of processing method of sintered samarium cobalt permanent magnet tailing |
| CN109396444B (en) * | 2018-11-05 | 2021-08-31 | 湖南航天磁电有限责任公司 | Method for processing leftover bits and pieces of sintered samarium cobalt permanent magnet |
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| Publication number | Publication date |
|---|---|
| CN1173051C (en) | 2004-10-27 |
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Granted publication date: 20041027 Termination date: 20111023 |