CN105957677A - 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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- CN105957677A CN105957677A CN201610521181.1A CN201610521181A CN105957677A CN 105957677 A CN105957677 A CN 105957677A CN 201610521181 A CN201610521181 A CN 201610521181A CN 105957677 A CN105957677 A CN 105957677A
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- micropowder
- sintering furnace
- vacuum
- recovery method
- container
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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
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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
- 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
-
- 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 and produce sintering technology field, more specifically, it relates to a kind of sintering neodymium ferrum
The recovery method of boron micropowder.
Background technology
Using powder metallurgical technique to prepare the technique that sintered NdFeB is a kind of maturation, its preparation process includes closing
The flow processs such as gold melting, pulverizing, pressing under magnetic field, isostatic pressed and sintering timeliness.Airflow milling powder technology is current
One of Technology that sintered NdFeB is the most key and advanced, at airflow milling powder process, Nd Fe B alloys
It is ground into the powder body that particle mean size is 3～5 microns, creates the powder that part is superfine, grain in the process
Degree is general below 2 microns, owing to the specific surface area of this superfines is big, and extremely easy oxygen in atmosphere
Change, spontaneous combustion, in therefore producing need this part powder body to separate, we term it neodymium iron boron micropowder.
In traditional handicraft, due to the extremely easily spontaneous combustion of neodymium iron boron micropowder, its removal process is extremely hard to control
System, the most often burns process, causes the wasting of resources.Some scholars is by strengthening protection, reducing process oxygen
The method of content is sintered, reclaims, but still there is technological process length, process complexity, and neodymium iron boron is ultra-fine
Powder still has more being exposed in oxygen, the careless slightly situation i.e. causing oxidation, spontaneous combustion, causes the response rate
Cannot ensure.
Summary of the invention
The technical problem to be solved in the present invention is the above-mentioned deficiency for prior art, it is provided that a kind of sintering neodymium ferrum
The recovery method of boron micropowder, solve micropowder aoxidize in removal process, the problem of spontaneous combustion.
The technical solution used in the present invention is such that the recovery method of a kind of sintered NdFeB micropowder, bag
Include following steps:
1) powder delivery: use airtight, the container of deformation can connect airflow milling micropowder discharging opening, with nitrogen or
Noble gas replaces the air in container repeatedly, to forward the micropowder in airflow milling equipment to nitrogen or inertia
In the container of gas shield；Concrete replacement process is: be full of nitrogen in container or noble gas makes it heave,
Extruding container makes gas in container all discharge, and repeats said process 2-3 time；Or can also be continuously toward holding
Nitrogen or noble gas it is filled with by Dilution air in container in device；Purpose is to get rid of the oxygen in container.
2) shove charge: by rapid 1) in be placed in sintering alms bowl head equipped with the container of micropowder, put the most again to vacuum
In sintering furnace；
3) deoxygenation: close the fire door of vacuum sintering furnace, be filled with nitrogen or lazy by vacuum sintering furnace spare interface
Property gas, discharged by atmospheric valve, make in sintering furnace oxygen content less than 100ppm by gas displacement；
4) pre-burning: close the respective valves of vacuum sintering furnace, make vacuum sintering furnace be in normal pressure whole sealing status,
Heating makes the container fusing in sintering furnace；
5) evacuation: start vacuum system and vacuum sintering furnace is carried out evacuation；
6) high temperature sintering: under vacuum, heating, insulation, make micropowder densification, then in inertia
Under gas shield, come out of the stove below quenching to 60 DEG C, obtain micropowder alloy.
Further, step 1) in container be closed plastic bag.
Further, step 2) in sintering alms bowl head material be mullite material, it is to avoid if ferrous material,
Sintering process can be bonded together, it is impossible to pours out.
Further, step 4) in heating-up temperature when being 150～300 DEG C, be incubated 15-30 minute, make burning
Container fusing in freezing of a furnace is burnt.
Further, step 5) in vacuum-sintering stove evacuation, the vacuum to stove is higher than 0.1pa.
Further, step 1), step 3) and step 6) in noble gas be argon.
Further, step 6) in heating-up temperature be 900～1170 DEG C.
Further, step 6) in temperature retention time be 1～5 hour.
The present invention compared with prior art, has following technical effect that
1, in the present invention, micropowder completes to sintering from airflow milling equipment discharging, is in controlled, hypoxia all the time
Under the conditions of, it is to avoid micropowder oxidation, spontaneous combustion problems, can realize entirely reclaiming.
2, the micropowder that this law is bright is after airflow milling produces plastic bag, it is not necessary to open plastic bag operation, it is only necessary to
Being placed in vacuum sintering furnace, plastic bag melts at a certain temperature so that it is be exposed to the sintered ring close to anaerobic
Under border, without micropowder itself being carried out other operation any in the most whole process technical process, its behaviour
Make simple, stopped because of numerous and diverse operation or controlled improper to cause micropowder oxidation, spontaneous combustion, therefore the present invention
Method production efficiency is high, and technique is simple, and product yield is high, purity is good.
3, the bright technique by preheating of this law, makes plastic bag fusing break, which ensure that under vacuumized conditions,
Be placed in vacuum sintering furnace the plastic bag equipped with micropowder will not because of pressure reduction explosion cause micropowder fly upward pollution whole
Individual vacuum system, thus do not damage the vacuum system of vacuum sintering furnace, the response rate have also been obtained raising.
4, plastic bag carbonization under vacuum, high temperature of the bright use of this law, therefore avoids micropowder because sticking to
The problem that cannot realize on plastic bag wall reclaiming, improves the response rate.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
Use airtight plastic bag to connect airflow milling micropowder discharging opening, repeatedly replace in plastic bag with nitrogen
Air, to forward to the micropowder in airflow milling equipment in the plastic bag that nitrogen is protected；Will be equipped with micropowder
Plastic bag is placed in sintering alms bowl head, covers cover plate, then puts to vacuum sintering furnace；Close vacuum sintering furnace
Fire door, be filled with nitrogen by vacuum sintering furnace spare interface, discharged by atmospheric valve, pass through gas displacement
In making sintering furnace, oxygen content is less than 100ppm；Close the respective valves of vacuum sintering furnace, make vacuum sintering furnace
It is in normal pressure whole sealing status, is heated to 150 DEG C, be incubated 30 minutes so that the plastic bag in sintering furnace melts
Change；The vacuum that vacuum sintering furnace is evacuated in stove by startup vacuum system is higher than 0.1pa；In vacuum
Under the conditions of, it is heated to 900 DEG C, is incubated 5 hours, makes micropowder densification, then under inert gas shielding,
Quenching is come out of the stove to less than 60 DEG C, obtains micropowder alloy.Micropowder alloy is carried out performance evaluation, its density
For 7.45g/cm3, oxygen content is 418ppm, and content is relatively low, illustrates not oxidized.
Embodiment 2
Use airtight plastic bag to connect airflow milling micropowder discharging opening, repeatedly replace in plastic bag with argon
Air, to forward to the micropowder in airflow milling equipment in the plastic bag of argon shield；Will be equipped with micropowder
Plastic bag is placed in sintering alms bowl head, covers cover plate, then puts to vacuum sintering furnace；Close vacuum sintering furnace
Fire door, be filled with argon by vacuum sintering furnace spare interface, discharged by atmospheric valve, pass through gas displacement
In making sintering furnace, oxygen content is less than 100ppm；Close the respective valves of vacuum sintering furnace, make vacuum sintering furnace
It is in normal pressure whole sealing status, is heated to 300 DEG C, be incubated 15 minutes so that the plastic bag in sintering furnace
Fusing；The vacuum that vacuum sintering furnace is evacuated in stove by startup vacuum system is higher than 0.1pa；Very
Under empty condition, it is heated to 1170 DEG C, is incubated 1 hour, make micropowder densification, then protect at noble gas
Protect down, come out of the stove below quenching to 60 DEG C, obtain micropowder alloy.Micropowder alloy is carried out performance evaluation,
Its density is 7.48g/cm3, and oxygen content is 397ppm, and 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
For, on the premise of without departing from present configuration, it is also possible to make some deformation and improvement, these are the most not
Effect and practical applicability that the present invention implements can be affected.
Claims (8)
1. the recovery method of a sintered NdFeB micropowder, it is characterised in that comprise the following steps:
1) powder delivery: use airtight, the container of deformation can connect airflow milling micropowder discharging opening, with nitrogen or
Noble gas replaces the air in container repeatedly；
2) shove charge: by rapid 1) in be placed in sintering alms bowl head equipped with the hermetic container of micropowder, cover cover plate,
Put the most again to vacuum sintering furnace；
3) deoxygenation: close the fire door of vacuum sintering furnace, be filled with nitrogen or lazy by vacuum sintering furnace spare interface
Property gas, discharged by atmospheric valve, make in sintering furnace oxygen content less than 100ppm by gas displacement；
4) pre-burning: close the respective valves of vacuum sintering furnace, make vacuum sintering furnace be in normal pressure whole sealing status,
Heating makes the container fusing in sintering furnace；
5) evacuation: start vacuum system and vacuum sintering furnace is carried out evacuation；
6) high temperature sintering: under vacuum, heating, insulation, make micropowder densification, then in inertia
Under gas shield, come out of the stove below quenching to 60 DEG C, obtain micropowder alloy.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 1) container in is closed plastic bag.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 2) the sintering alms bowl head material in is mullite material.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 4) when heating-up temperature is 150～300 DEG C in, it is incubated 15-30 minute, makes the container in sintering furnace melt
Burn.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 5) the vacuum-sintering stove evacuation in, the vacuum to stove is higher than 0.1pa.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 1), step 3) and step 6) in noble gas be argon.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 6) in, heating-up temperature is 900～1170 DEG C.
The recovery method of sintered NdFeB micropowder the most according to claim 1, it is characterised in that step
Rapid 6) in, temperature retention time is 1～5 hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910176A (en) * | 2017-10-10 | 2018-04-13 | 浙江东阳东磁稀土有限公司 | A kind of rare-earth Nd-Fe-B superfine powder recoverying and utilizing method |
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 |
-
2016
- 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910176A (en) * | 2017-10-10 | 2018-04-13 | 浙江东阳东磁稀土有限公司 | A kind of rare-earth Nd-Fe-B superfine powder recoverying and utilizing method |
| 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 |
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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. |
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