CN105957677B - Recovery method of sintered neodymium iron boron ultrafine powder - Google Patents
Recovery method of sintered neodymium iron boron ultrafine powder Download PDFInfo
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- CN105957677B CN105957677B CN201610521181.1A CN201610521181A CN105957677B CN 105957677 B CN105957677 B CN 105957677B CN 201610521181 A CN201610521181 A CN 201610521181A CN 105957677 B CN105957677 B CN 105957677B
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- superfine powder
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- 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
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a method for recovering sintered NdFeB (neodymium iron boron) ultrafine powder, which comprises the following steps of: 1) powder discharging: transferring the superfine powder in the jet mill equipment to a closed container protected by nitrogen or inert gas; 2) charging: placing the closed container filled with the ultrafine powder in a vacuum sintering furnace, and then placing the closed container in the vacuum sintering furnace; 3) oxygen discharge: the oxygen content in the sintering furnace is less than 100ppm through gas replacement; 4) pre-burning: heating to melt the container in the sintering furnace; 5) vacuumizing: starting a vacuum system to vacuumize the vacuum sintering furnace; 6) and (3) high-temperature sintering: heating to 900-1170 ℃, preserving heat for 1-5 hours, quenching to below 60 ℃, and discharging to obtain the ultrafine powder alloy. The ultrafine powder is discharged from the jet mill equipment to be sintered and is always in a controllable and low-oxygen condition, so that the problems of oxidization and spontaneous combustion of the ultrafine powder are avoided, and the full recovery can be realized.
Description
Technical field
The present invention relates to neodymium iron boron production sintering technology field, more specifically, it relates to which a kind of sintered NdFeB is ultra-fine
The recovery method of powder.
Background technology
It is a kind of ripe technique to prepare sintered NdFeB using powder metallurgical technique, and its preparation process melts including alloy
The flows such as refining, crushing, pressing under magnetic field, isostatic pressed and sintering timeliness.Airflow milling powder technology is that current sintered NdFeB closes the most
One of key and advanced technology, in airflow milling powder process, Nd Fe B alloys is ground into particle mean size as 3~5 microns
Powder, generate the superfine powder in part in the process, granularity is probably below 2 microns, due to this superfines
Specific surface area is big, extremely easily oxidation, spontaneous combustion in atmosphere, therefore in producing need the part powder to separate, we
Referred to as neodymium iron boron superfine powder.
In traditional handicraft, due to the extremely easy spontaneous combustion of neodymium iron boron superfine powder, its removal process is extremely hard to control, therefore
Often burn-up is handled, and causes the wasting of resources.Some scholars are by strengthening protection, the method for reduction process oxygen content is sintered,
Recovery, but still have that technological process is long, process is complicated, neodymium iron boron superfine powder still have it is more be exposed in oxygen, slightly not
It is careful to cause oxidation, the situation of spontaneous combustion, cause the rate of recovery not ensure.
The content of the invention
The technical problem to be solved in the present invention is the above-mentioned deficiency for prior art, there is provided a kind of sintered NdFeB is ultra-fine
The recovery method of powder, solve the problems, such as superfine powder aoxidized in removal process, spontaneous combustion.
The technical solution adopted by the present invention is such：A kind of recovery method of sintered NdFeB superfine powder, including it is following
Step：
1) powder is gone out：Using it is closed, can deformation container connect airflow milling superfine powder discharging opening, with nitrogen or inert gas
The air in container is replaced repeatedly, and the superfine powder in airflow milling equipment is gone in nitrogen or the container of inert gas shielding；
Specifically replacement process is：It is heaved in toward container full of nitrogen or inert gas, extruding container makes gas in container all arrange
Go out, repeat said process 2-3 times；Or can also be continuously dilute by air in container toward nitrogen or inert gas is filled with container
Release；Purpose is to exclude the oxygen in container.
2) shove charge：By it is rapid 1) in equipped with superfine powder container be placed in sintering alms bowl head in, then put again into vacuum sintering furnace；
3) deoxygenation：The fire door of vacuum sintering furnace is closed, nitrogen or inert gas are filled with by vacuum sintering furnace spare interface,
Discharged by atmospheric valve, 100ppm is less than by oxygen content in gas displacement sintering furnace；
4) pre-burning：The respective valves of vacuum sintering furnace are closed, vacuum sintering furnace is in normal pressure whole sealing status, heating makes
Obtain the container fusing in sintering furnace；
5) vacuumize：Start vacuum system to vacuumize vacuum sintering furnace；
6) high temperature sintering：Under vacuum, heat, insulation, be densified superfine powder, then in inert gas shielding
Under, quenching is come out of the stove to less than 60 DEG C, obtains superfine powder alloy.
Further, the container in step 1) is closed polybag.
Further, the sintering alms bowl head material in step 2) is mullite material, is avoided if ferrous material, sintered
Journey can be bonded together, and can not be poured out.
Further, when heating-up temperature is 150~300 DEG C in step 4), 15-30 minutes is incubated, make the appearance in sintering furnace
Device fusing is burnt.
Further, the vacuum-sintering stove evacuation in step 5), to stove in vacuum be higher than 0.1pa.
Further, the inert gas in step 1), step 3) and step 6) is argon gas.
Further, heating-up temperature is 900~1170 DEG C in step 6).
Further, soaking time is 1~5 hour in step 6).
The present invention compared with prior art, has following technique effect：
1st, superfine powder is completed from the discharging of airflow milling equipment to sintering in the present invention, all the time under controllable, hypoxia condition,
Superfine powder oxidation, spontaneous combustion problems are avoided, full recovery can be achieved.
2nd, the bright superfine powder of this law is produced to after polybag from airflow milling, without opening polybag operation, it is only necessary to is placed in true
In empty sintering furnace, polybag melts at a certain temperature, it is exposed to close under the sintering environment of anaerobic, therefore whole processing
Without carrying out any other operation in itself to superfine powder in technical process, its is simple to operate, has prevented because of numerous and diverse operation or control
The improper method production efficiency height for causing superfine powder oxidation, spontaneous combustion, therefore the present invention is made, technique is simple, and product yield is high, purity
It is good.
3rd, the bright technique by preheating of this law, polybag fusing is broken, which ensure that under vacuumized conditions, be placed on true
The polybag equipped with superfine powder will not burst because of pressure difference in empty sintering furnace causes superfine powder to fly upward the whole vacuum system of pollution, so as to
The vacuum system of vacuum sintering furnace is not damaged, and the rate of recovery is also improved.
4th, the bright polybag used of this law is carbonized under vacuum, high temperature, therefore avoids superfine powder because being adhered to polybag
The problem of can not realizing recovery on wall, improve the rate of recovery.
Embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
Airflow milling superfine powder discharging opening is connected using closed polybag, replaces the air in polybag repeatedly with nitrogen,
So that the superfine powder in airflow milling equipment is gone in the polybag of nitrogen protection；Polybag equipped with superfine powder is placed in sintering alms bowl
In head, cover plate is covered, is then put into vacuum sintering furnace；The fire door of vacuum sintering furnace is closed, is connect by the way that vacuum sintering furnace is standby
Mouth is filled with nitrogen, is discharged by atmospheric valve, is less than 100ppm by oxygen content in gas displacement sintering furnace；Vacuum is closed to burn
The respective valves of freezing of a furnace, vacuum sintering furnace is in normal pressure whole sealing status, be heated to 150 DEG C, be incubated 30 minutes so that sintering
Polybag fusing in stove；Start the vacuum that vacuum system to vacuum sintering furnace be evacuated in stove and be higher than 0.1pa；
Under vacuum condition, 900 DEG C are heated to, 5 hours is incubated, is densified superfine powder, then under inert gas shielding, quenching to 60
Come out of the stove below DEG C, obtain superfine powder alloy.Performance evaluation is carried out to superfine powder alloy, its density is 7.45g/cm3, and oxygen content is
418ppm, content is relatively low, illustrates not oxidized.
Embodiment 2
Airflow milling superfine powder discharging opening is connected using closed polybag, replaces the air in polybag repeatedly with argon gas,
So that the superfine powder in airflow milling equipment is gone in the polybag of argon gas protection；Polybag equipped with superfine powder is placed in sintering alms bowl
In head, cover plate is covered, is then put into vacuum sintering furnace；The fire door of vacuum sintering furnace is closed, is connect by the way that vacuum sintering furnace is standby
Mouth is filled with argon gas, is discharged by atmospheric valve, is less than 100ppm by oxygen content in gas displacement sintering furnace；Vacuum is closed to burn
The respective valves of freezing of a furnace, vacuum sintering furnace is in normal pressure whole sealing status, be heated to 300 DEG C, be incubated 15 minutes so that sintering
Polybag fusing in stove；Start the vacuum that vacuum system to vacuum sintering furnace be evacuated in stove and be higher than 0.1pa；
Under vacuum condition, 1170 DEG C are heated to, 1 hour is incubated, is densified superfine powder, then under inert gas shielding, quenching is extremely
Less than 60 DEG C are come out of the stove, and obtain superfine powder alloy.Performance evaluation is carried out to superfine powder alloy, its density is 7.48g/cm3, oxygen content
For 397ppm, content is relatively low, illustrates not oxidized.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art,
Without departing from the structure of the invention, several modifications and improvements can also be made, these are implemented all without the present invention is influenceed
Effect and practical applicability.
Claims (6)
1. a kind of recovery method of sintered NdFeB superfine powder, it is characterised in that comprise the following steps：
1) powder is gone out：Airflow milling superfine powder discharging opening is connected using closed polybag, is replaced repeatedly with nitrogen or inert gas
Air in container；
2) shove charge：By it is rapid 1) in be placed in the sintering alms bowl head of mullite material equipped with the closed container of superfine powder, cover cover plate, so
Put again into vacuum sintering furnace afterwards；
3) deoxygenation：The fire door of vacuum sintering furnace is closed, nitrogen or inert gas are filled with by vacuum sintering furnace spare interface, passed through
Atmospheric valve discharges, and is less than 100ppm by oxygen content in gas displacement sintering furnace；
4) pre-burning：The respective valves of vacuum sintering furnace are closed, vacuum sintering furnace is in normal pressure whole sealing status, heating to burn
Container fusing in freezing of a furnace；
5) vacuumize：Start vacuum system to vacuumize vacuum sintering furnace；
6) high temperature sintering：Under vacuum, heat, insulation, be densified superfine powder, then under inert gas shielding, quench
It is cooled to less than 60 DEG C to come out of the stove, obtains superfine powder alloy.
2. the recovery method of sintered NdFeB superfine powder according to claim 1, it is characterised in that heating temperature in step 4)
Spend for 150~300 DEG C when, be incubated 15-30 minutes, melt container in sintering furnace and burn.
3. the recovery method of sintered NdFeB superfine powder according to claim 1, it is characterised in that the vacuum in step 5)
Sinter stove evacuation, to stove in vacuum be higher than 0.1pa.
4. the recovery method of sintered NdFeB superfine powder according to claim 1, it is characterised in that step 1), step 3)
And the inert gas in step 6) is argon gas.
5. the recovery method of sintered NdFeB superfine powder according to claim 1, it is characterised in that heating temperature in step 6)
Spend for 900~1170 DEG C.
6. the recovery method of sintered NdFeB superfine powder according to claim 1, it is characterised in that when being incubated in step 6)
Between be 1~5 hour.
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| CN107910176B (en) * | 2017-10-10 | 2020-01-10 | 浙江东阳东磁稀土有限公司 | Recycling method of rare earth neodymium iron boron ultrafine powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164723A (en) * | 2007-10-11 | 2008-04-23 | 宝鸡富士特钛业有限公司 | Method for preparing high-purification ultrafine titanium powder for aviation |
| US8609189B2 (en) * | 2011-09-28 | 2013-12-17 | King Abdulaziz University | Method of forming carbon nanotubes from carbon-rich fly ash |
| CN103866126A (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 by using jet mill waste powder |
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- 2016-06-30 CN CN201610521181.1A patent/CN105957677B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164723A (en) * | 2007-10-11 | 2008-04-23 | 宝鸡富士特钛业有限公司 | Method for preparing high-purification ultrafine titanium powder for aviation |
| US8609189B2 (en) * | 2011-09-28 | 2013-12-17 | King Abdulaziz University | Method of forming carbon nanotubes from carbon-rich fly ash |
| CN103866126A (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 by using jet mill waste powder |
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Address after: 542603 Wanggao Industrial Development Zone, Hezhou, the Guangxi Zhuang Autonomous Region Patentee after: China Rare Earth (Guangxi) Jinyuan rare earth new material Co., Ltd Address before: 542829 Wanggao Industrial Development Zone, Hezhou, the Guangxi Zhuang Autonomous Region Patentee before: CHINALCO GUANGXI COLORED JINYUAN RARE EARTH Co.,Ltd. |
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Effective date of registration: 20220523 Address after: 629201 floor 1, building 6, Hedong Avenue, Shehong Economic Development Zone, Suining City, Sichuan Province Patentee after: Sichuan yuanlaishun rare earth new material Co.,Ltd. Address before: 542603 Wanggao Industrial Development Zone, Hezhou, the Guangxi Zhuang Autonomous Region Patentee before: China Rare Earth (Guangxi) Jinyuan rare earth new material Co.,Ltd. |