CN106504838A - A kind of preparation method of neodymium iron boron magnetic body - Google Patents
A kind of preparation method of neodymium iron boron magnetic body Download PDFInfo
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- CN106504838A CN106504838A CN201610962943.1A CN201610962943A CN106504838A CN 106504838 A CN106504838 A CN 106504838A CN 201610962943 A CN201610962943 A CN 201610962943A CN 106504838 A CN106504838 A CN 106504838A
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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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
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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
- 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
- H01F1/0576—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 pressed, e.g. hot working
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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
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
Abstract
The invention provides a kind of preparation method of neodymium iron boron magnetic body, including：Nd Fe B alloys is carried out hydrogen to crush, suction hydrogen time >=60 minute in the hydrogen shattering process, dehydrogenation time is T, and 0 ＜ T≤8 hour obtain powder；The powder is carried out airflow milling, powder is obtained；The powder is carried out magnetic field orientating forming processes, magnet idiosome is obtained；The magnet idiosome is sintered and Ageing Treatment successively, neodymium iron boron magnetic body is obtained；The temperature of the sintering is 1000～1100 DEG C；The temperature of the Ageing Treatment is 500～950 DEG C.The present invention has obtained the higher Nd Fe B alloys powder of hydrogen content using rational hydrogen decrepitation, and the higher Nd Fe B alloys powder of this hydrogen content goes out powder speed with higher during airflow milling；Simultaneously the present invention sintered by control and Ageing Treatment technological parameter, it is ensured that can still obtain the neodymium iron boron magnetic body of better performances under conditions of the preparing raw material higher using hydrogen content.
Description
Technical field
A kind of the present invention relates to magnet technology field, more particularly to preparation method of neodymium iron boron magnetic body.
Background technology
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), and its chemical formula is Nd2Fe14B, is a kind of artificial
Permanent magnet, and there is the permanent magnet of most strong magnetic force so far, its maximum magnetic energy product (BHmax) exceeds ferrite 10
More than times, in the state of naked magnetic, its magnetic force can reach 3500 Gauss.The advantage of neodymium iron boron magnetic body is cost performance height, body
Product is little, lightweight, there is good mechanical property, these advantages to make Nd-Fe-B permanent magnet material in modern industry and electronic technology
Obtain a wide range of applications, magnetic king is described as in magnetics circle.Therefore, the preparation of neodymium iron boron magnetic body and extension always continue in the industry
Focus of attention.
In the last few years, as computer, Communication Equipment and auto-producing are fast-developing, to Nd-Fe-B permanent magnet material
Demand is increased sharply；And in terms of the concrete application to magnet, such as automobile motor etc., in miniaturization, lightweight and energy-conserving and environment-protective etc.
Aspect proposes further requirement, while the requirement more and more higher to magnet performance.The preparation technology flow process of neodymium iron boron magnetic body
Generally comprise the steps such as dispensing, melting ingot, powder processed, die mould, sintering tempering, magnetic detection.The pulverizing process one of prior art
As adopt the preparation technology of broken (the HD)+airflow milling (JM) of hydrogen to meet the technological requirement for preparing high performance magnet, but existing
In technology pulverizing process, airflow milling goes out that powder speed is relatively low, increased the production cost of neodymium iron boron magnetic body.
Content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of neodymium iron boron magnetic body, the side that the present invention is provided
Method during neodymium iron boron magnetic body is prepared airflow milling to go out powder speed higher.
The invention provides a kind of preparation method of neodymium iron boron magnetic body, including：
Nd Fe B alloys is carried out hydrogen to crush, powder is obtained, suction hydrogen time >=60 minute in the hydrogen shattering process take off
The hydrogen time be T, 0 ＜ T≤8 hour；
The powder is carried out airflow milling, powder is obtained；
The powder is carried out magnetic field orientating forming processes, magnet idiosome is obtained；
The magnet idiosome is sintered and Ageing Treatment successively, neodymium iron boron magnetic body is obtained；
The temperature of the sintering is 1000～1100 DEG C；
The temperature of the Ageing Treatment is 500～950 DEG C.
Preferably, the suction hydrogen time is 90～180 minutes.
Preferably, the desorption temperature in the hydrogen shattering process is 550～600 DEG C.
Preferably, the time of the sintering is 5～11 hours.
Preferably, the Ageing Treatment is specially：
Product after by sintering carries out the first Ageing Treatment and the second Ageing Treatment successively, obtains neodymium iron boron magnetic body；
The temperature of first Ageing Treatment is 850～950 DEG C；
The temperature of second Ageing Treatment is 500～600 DEG C.
Preferably, the time of first Ageing Treatment is 1～3 hour；
The time of second Ageing Treatment is 4～6 hours.
Preferably, the composition of the Nd Fe B alloys includes：
The praseodymium neodymium alloy of 30～32wt%；
The boron of 0.8～1.2wt%；
The ferrum of 64～68.4wt%；
The aluminum of 0.1～1.8wt%；
The copper of 0.2～0.6wt%；
The cobalt of 0.5～1wt%.
Preferably, the granularity of the powder is 2～8 microns.
Preferably, magnetic field intensity >=16000 Gauss of the magnetic field orientating forming processes.
Preferably, also include after the powder being carried out magnetic field orientating forming processes：
Product after magnetic field orientating forming processes is carried out isostatic pressed process, the higher magnet embryo evenly of density is obtained
Body；
The pressure that the isostatic pressed is processed is 180～240MPa.
Compared with prior art, the present invention is obtained using rational hydrogen decrepitation during neodymium iron boron magnetic body is prepared
The higher Nd Fe B alloys powder body of hydrogen content is arrived, the higher Nd Fe B alloys powder body of this hydrogen content is during airflow milling
Go out powder speed with higher；Simultaneously the present invention sintered by control and Ageing Treatment technological parameter, it is ensured that adopting
The neodymium iron boron magnetic body of better performances can be still obtained under conditions of the higher powder material of hydrogen content.The present invention is by improving neodymium
Hydrogen content in ferroboron powder body effectively increases the production cost for powder speed, reducing neodymium iron boron magnetic body of airflow milling.
Specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than whole embodiment.Embodiment in based on the present invention, this area are common
Technical staff improved or retouching all other example, belong to the scope of protection of the invention.
The invention provides a kind of preparation method of neodymium iron boron magnetic body, including：
Nd Fe B alloys is carried out hydrogen to crush, powder is obtained, suction hydrogen time >=60 minute in the hydrogen shattering process take off
The hydrogen time be T, 0 ＜ T≤8 hour；
The powder is carried out airflow milling, powder is obtained；
The powder is carried out magnetic field orientating forming processes, magnet idiosome is obtained；
The magnet idiosome is sintered and Ageing Treatment successively, neodymium iron boron magnetic body is obtained；
The temperature of the sintering is 1000～1100 DEG C；
The temperature of the Ageing Treatment is 500～950 DEG C.
The present invention does not have special restriction to the Nd Fe B alloys, prepares neodymium ferrum using well known to those skilled in the art
The alloy raw material of boron magnet.In the present invention, the composition of the Nd Fe B alloys is preferably included：The praseodymium neodymium of 30～32wt%
Alloy；The boron of 0.8～1.2wt%；The ferrum of 64～68.4wt%；The aluminum of 0.1～1.8wt%；The copper of 0.2～0.6wt%；0.5
The cobalt of～1wt%.In the present invention, mass content of the praseodymium neodymium alloy in Nd Fe B alloys be preferably 30.5～
31.4%, more preferably 31%.In the present invention, the praseodymium is preferably 0～30% in the mass content of praseodymium neodymium alloy, more preferably
For 5～25%, more preferably 10～20% most preferably 20%.In the present invention, mass content of the neodymium in praseodymium neodymium alloy
Preferably 70～100%, more preferably 75～95%, more preferably 80～90%, most preferably 80%.In the present invention, institute
State mass content of the boron in Nd Fe B alloys and be preferably 0.9～1.1%, more preferably 1%.In the present invention, the ferrum exists
Mass content in Nd Fe B alloys is preferably 65～68%, more preferably 66～67%.In the present invention, the aluminum is in neodymium ferrum
Mass content in boron alloy is preferably 0.5～1.2%, more preferably 0.8～1%.In the present invention, the copper is in neodymium iron boron
Mass content in alloy is preferably 0.3～0.5%, more preferably 0.4%.In the present invention, the cobalt is in Nd Fe B alloys
In mass content be preferably 0.6～0.9%, more preferably 0.7～0.8%.
In the present invention, the preparation method of the Nd Fe B alloys is preferably：
By praseodymium neodymium alloy, boron, ferrum, aluminum, copper and cobalt, according to target composition carries out proportioning mixing, obtains mixture；
The mixture is carried out melting, liquation is obtained；
Cool down after the liquation is cast, obtain Nd Fe B alloys.
In the present invention, the praseodymium neodymium alloy, boron, ferrum, aluminum, copper and cobalt can be obtained by market purchase.In the present invention, institute
State praseodymium neodymium alloy, boron, ferrum, aluminum, copper consistent i.e. with the mass content of each composition in the Fe-Nd-B alloy for obtaining in advance with the consumption of cobalt
Can.The present invention does not have special restriction to the temperature of the melting, melts can above-mentioned raw materials, can be molten in vacuum induction
Melting is carried out in furnace.In the present invention, the temperature of the casting is preferably 1400～1500 DEG C, and more preferably 1420～1480
DEG C, most preferably 1440～1460 DEG C.In the present invention, the method for the cooling is copper roller cooling.In the present invention, the copper
Rotating speed in roller cooling procedure is preferably 20～60 revs/min, more preferably 30～50 revs/min, most preferably 35～45 revs/min.
In the present invention, the Nd Fe B alloys is preferably prepared to slab.In the present invention, the thickness of slab shape Nd Fe B alloys is excellent
Elect 0.1～0.6mm, most preferably more preferably 0.2～0.5mm, 0.3～0.4mm as.
In the present invention, hydrogen is broken for the preparation method of alloy powder, is being inhaled hydrogen and put during hydrogen itself using alloy
Produced grain boundary fracture and transgranular fracture cause alloy pulverization, obtain alloy powder.In the present invention, the hydrogen shattering process
In suction hydrogen time >=60 minute, preferably 90～180 minutes, more preferably 120～140 minutes.In the present invention, the hydrogen
Dehydrogenation time in shattering process is T, and 0 ＜ T≤8 hour are preferably 0.5～6 hour, more preferably 1.5～5 hours, optimum
Elect 3～4 hours as.In the present invention, the desorption temperature in the hydrogen shattering process is preferably 550～600 DEG C, more preferably
560～590 DEG C, most preferably 570～580 DEG C.In the present invention, preferably the product for obtaining is carried out after the completion of the hydrogen is broken
The water-cooled of 2～4 hours, obtains powder.
The present invention does not have special restriction to the method for the airflow milling, prepares neodymium using well known to those skilled in the art
The technical scheme of the airflow milling adopted during iron boron magnet is carried out in Air Grinder.In the present invention, the gas
The granularity of the powder obtained after stream mill is preferably 2～8 microns, more preferably 3～6 microns, most preferably 4～5 microns.
In the present invention, the magnetic field orientating molding is preferably carried out in the absence of oxygen, more preferably in the glove of sealing
Carry out in case.In the present invention, in the magnetic field orientating forming process magnetic field intensity preferably >=16000 Gausses, preferably
16000～19000 Gausses, more preferably 17000～18000 Gausses.In the present invention, preferably will after the magnetic field orientating molding
The product for obtaining carries out isostatic pressed process, obtains magnet idiosome.In the present invention, the pressure that the isostatic pressed is processed is preferably
180～240MPa, more preferably 200～220MPa.
In the present invention, the temperature of the sintering is preferably 1000～1100 DEG C, more preferably 1030～1070 DEG C, optimum
Elect 1050 DEG C as.In the present invention, the time of the sintering is preferably 5～11 hours, more preferably 6～8 hours.In the present invention
In, the temperature of the Ageing Treatment is preferably 500～950 DEG C, more preferably 600～850 DEG C.In the present invention, the timeliness
Processing preferably is carried out step by step：
Product after by sintering carries out the first Ageing Treatment and the second Ageing Treatment successively, obtains neodymium iron boron magnetic body；Described
The temperature of the first Ageing Treatment is 850～950 DEG C；The temperature of second Ageing Treatment is 500～600 DEG C.
In the present invention, the temperature of first Ageing Treatment is preferably 880～910 DEG C, more preferably 900 DEG C.At this
In invention, the time of first Ageing Treatment is preferably 1～3 hour, more preferably 2～2.5 hours.In the present invention, institute
The temperature for stating the second Ageing Treatment is preferably 520～550 DEG C, more preferably 530 DEG C.In the present invention, at second timeliness
The time of reason is preferably 4～6 hours, more preferably 5 hours.
The present invention goes out powder speed by preparing the higher Nd Fe B alloys powder of hydrogen content and improve during airflow milling,
Production cost is reduced, and the preferable neodymium iron boron of magnetic property has been prepared using the higher Nd Fe B alloys powder of hydrogen content
Magnet.
Raw material used in following examples of the present invention is commercial goods.
Embodiment 1
By praseodymium neodymium alloy (mass content of the praseodymium in praseodymium neodymium alloy is 20%, the mass content of neodymium for 80%), ferrum, aluminum,
Mix after boron, cobalt and copper proportioning, the melting in vacuum induction melting furnace by the mixture for obtaining will obtain liquation and pour at 1465 DEG C
Casting, cools down on the copper roller that rotating speed is 40 revs/min, obtains average thickness for 0.33mm Nd Fe B alloys slabs, and composition is：
The praseodymium neodymium alloy of 31.4wt%, the aluminum of 1.2wt%, the copper of 0.5wt%, the cobalt of 1wt%, the boron of 1wt%, balance of ferrum.
Embodiment 2
The Nd Fe B alloys slab that average thickness is 0.31mm is prepared according to the method described in embodiment 1, composition is：
The praseodymium neodymium alloy of 31wt%, the aluminum of 1.8wt%, the copper of 0.6wt%, the cobalt of 0.5wt%, the boron of 1wt%, balance of ferrum.
Embodiment 3
The Nd Fe B alloys slab that average thickness is 0.35mm is prepared according to the method described in embodiment 1, composition is：
The praseodymium neodymium alloy of 30.5wt%, the aluminum of 0.1wt%, the copper of 0.2wt%, the cobalt of 0.5wt%, the boron of 1wt%, balance of ferrum.
Embodiment 4
The Fe-Nd-B alloy casting piece that embodiment 1 is prepared carries out hydrogen and crushes, during suction hydrogen in the hydrogen shattering process
Between be 1 hour, dehydrogenation time 8 hours, desorption temperature be 600 DEG C, cool down 2 hours, obtain powder；
The powder is carried out airflow milling, the powder that granularity is 3.8 microns is obtained；
The powder is being carried out magnetic field orientating forming processes under 18210 gauss magnetic fields in the glove box of sealing anaerobic, so
Isostatic pressed process is carried out under 200MPa afterwards, magnet idiosome is obtained；
The magnet idiosome is sintered at 1050 DEG C 6 hours, at 910 DEG C, then carry out the Ageing Treatment of 2 hours, most
Carry out the Ageing Treatment of 5 hours afterwards at 530 DEG C, obtain neodymium iron boron magnetic body.
Embodiment 5～10
Using the method for embodiment 4, neodymium iron boron magnetic body (the technique bar not provided is prepared according to the process conditions of table 1
Part is same as Example 4).
1 embodiment 5～10 of table prepares the process conditions of neodymium iron boron magnetic body
Embodiment 11
The hydrogen content obtained during Fe-Nd-B magnet is prepared to the embodiment of the present invention 4～10 in powder detects have
Body method is：
Hydrogen content in neodymium iron boron powder is determined using inert gas fusion-thermal conductivity method：The sample for preparing is placed in adding mouth
Interior, put in degassed graphite crucible, melt in slumpability gas high temperature, separate out hydrogen and separate with other gases, lead to
Cross thermal conductivity detection cell to be detected, changed according to thermal conductivity, calculate hydrogen content.
The powder speed that goes out for preparing airflow milling during neodymium iron boron magnetic body to the embodiment of the present invention 4～10 is detected：
Powder speed=the air-flow that goes out of airflow milling grinds grain weight amount/abrasive material duration.
The magnetic property of the neodymium iron boron magnetic body that the embodiment of the present invention 4～10 is prepared is detected, concrete grammar is：
The rare earth permanent magnet measuring system that is designed and developed using Chinese quantitative study institute is detected to magnet.Test process is
The process of demagnetization is filled to sample, J-H coil gathered datas is adopted during filling demagnetization, and J-H/B- is drawn by software data analysis
H demagnetizing curves, and measure and draw Br, the magnetic parameter such as Hcb, Hcj, (BH) max.
The embodiment of the present invention 4～10 prepares powder hydrogen content during neodymium iron boron magnetic body, go out powder speed and magnetic property
Testing result as shown in table 2, table 2 prepares powder hydrogen content during neodymium iron boron for the embodiment of the present invention 4～10, go out powder speed and
Neodymium iron boron magnetic body magnetic property testing result.
2 embodiment of the present invention 4～10 of table prepares powder hydrogen content during neodymium iron boron, goes out powder speed and neodymium iron boron magnetic body
Magnetic property testing result
Embodiment 12
The Fe-Nd-B alloy casting piece that embodiment 2 is prepared carries out hydrogen and crushes, during suction hydrogen in the hydrogen shattering process
Between be 1 hour, dehydrogenation time 8 hours, desorption temperature be 600 DEG C, cool down 2.5 hours, obtain powder；
The powder is carried out airflow milling, the powder that granularity is 4.2 microns is obtained；
The powder is being carried out magnetic field orientating forming processes under 17260 gauss magnetic fields in the glove box of sealing anaerobic, so
Isostatic pressed process is carried out under 220MPa afterwards, magnet idiosome is obtained；
The magnet idiosome is sintered at 1030 DEG C 8 hours, at 900 DEG C, then carries out the Ageing Treatment of 2.5 hours,
The last Ageing Treatment for carrying out 5 hours at 520 DEG C, obtains neodymium iron boron magnetic body.
Embodiment 13～18
Using the method for embodiment 12, neodymium iron boron magnetic body (the technique bar not provided is prepared according to the process conditions of table 3
Part is identical with embodiment 12).
3 embodiment 13～18 of table prepares the process conditions of neodymium iron boron magnetic body
Embodiment 19
The powder during neodymium iron boron magnetic body is prepared to the embodiment of the present invention 12～18 according to the method described in embodiment 11
Hydrogen content, air-flow grind powder speed and the magnetic property of neodymium iron boron magnetic body is detected, as shown in table 4, table 4 is this to testing result
Bright embodiment 12～18 prepares powder hydrogen content during neodymium iron boron, goes out powder speed and neodymium iron boron magnetic body magnetic property testing result.
4 embodiment of the present invention 12～18 of table prepares powder hydrogen content during neodymium iron boron, goes out powder speed and neodymium iron boron magnetic body
Magnetic property testing result
Embodiment 20
The Fe-Nd-B alloy casting piece that embodiment 3 is prepared carries out hydrogen and crushes, during suction hydrogen in the hydrogen shattering process
Between be 1 hour, dehydrogenation time 8 hours, desorption temperature be 600 DEG C, cool down 3 hours, obtain powder；
The powder is carried out airflow milling, the powder that granularity is 4.4 microns is obtained；
The powder is being carried out magnetic field orientating forming processes under 16990 gauss magnetic fields in the glove box of sealing anaerobic, so
Isostatic pressed process is carried out under 220MPa afterwards, magnet idiosome is obtained；
The magnet idiosome is sintered at 1070 DEG C 5 hours, at 880 DEG C, then carries out the Ageing Treatment of 2.5 hours,
The last Ageing Treatment for carrying out 5 hours at 550 DEG C, obtains neodymium iron boron magnetic body.
Embodiment 21～26
Using the method for embodiment 20, neodymium iron boron magnetic body (the technique bar not provided is prepared according to the process conditions of table 5
Part is identical with embodiment 20).
5 embodiment 21～26 of table prepares the process conditions of neodymium iron boron magnetic body
Embodiment 27
The powder during neodymium iron boron magnetic body is prepared to the embodiment of the present invention 20～26 according to the method described in embodiment 11
Hydrogen content, air-flow grind powder speed and the magnetic property of neodymium iron boron magnetic body is detected, as shown in table 6, table 6 is this to testing result
Bright embodiment 20～26 prepares powder hydrogen content during neodymium iron boron, goes out powder speed and neodymium iron boron magnetic body magnetic property testing result.
6 embodiment of the present invention 20～26 of table prepares powder hydrogen content during neodymium iron boron, goes out powder speed and neodymium iron boron magnetic body
Magnetic property testing result
As seen from the above embodiment, the invention provides a kind of preparation method of neodymium iron boron magnetic body, including：Neodymium iron boron is closed
Gold carries out hydrogen and crushes, and suction hydrogen time >=60 minute in the hydrogen shattering process, dehydrogenation time are T, and 0 ＜ T≤8 hour obtain
Powder；The powder is carried out airflow milling, powder is obtained；The powder is carried out magnetic field orientating forming processes, magnet embryo is obtained
Body；The magnet idiosome is sintered and Ageing Treatment successively, neodymium iron boron magnetic body is obtained；The temperature of the sintering be 1000～
1100℃；The temperature of the Ageing Treatment is 500～950 DEG C.The present invention has obtained hydrogen content using rational hydrogen decrepitation
Higher Nd Fe B alloys powder, the higher Nd Fe B alloys powder of this hydrogen content go out with higher during airflow milling
Powder speed；Simultaneously the present invention sintered by control and Ageing Treatment technological parameter, it is ensured that higher using hydrogen content
The neodymium iron boron magnetic body of better performances can be still obtained under conditions of preparing raw material.
Above-described is only the preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of neodymium iron boron magnetic body, including：
Nd Fe B alloys is carried out hydrogen to crush, powder is obtained, suction hydrogen time >=60 minute in the hydrogen shattering process, during dehydrogenation
Between be T, 0 ＜ T≤8 hour；
The powder is carried out airflow milling, powder is obtained；
The powder is carried out magnetic field orientating forming processes, magnet idiosome is obtained；
The magnet idiosome is sintered and Ageing Treatment successively, neodymium iron boron magnetic body is obtained；
The temperature of the sintering is 1000～1100 DEG C；
The temperature of the Ageing Treatment is 500～950 DEG C.
2. method according to claim 1, it is characterised in that the suction hydrogen time is 90～180 minutes.
3. method according to claim 1, it is characterised in that the desorption temperature in the hydrogen shattering process is 550～600
℃.
4. method according to claim 1, it is characterised in that the time of the sintering is 5～11 hours.
5. method according to claim 1, it is characterised in that the Ageing Treatment is specially：
Product after by sintering carries out the first Ageing Treatment and the second Ageing Treatment successively, obtains neodymium iron boron magnetic body；
The temperature of first Ageing Treatment is 850～950 DEG C；
The temperature of second Ageing Treatment is 500～600 DEG C.
6. method according to claim 5, it is characterised in that the time of first Ageing Treatment is 1～3 hour；
The time of second Ageing Treatment is 4～6 hours.
7. method according to claim 1, it is characterised in that the composition of the Nd Fe B alloys includes：
The praseodymium neodymium alloy of 30～32wt%；
The boron of 0.8～1.2wt%；
The ferrum of 64～68.4wt%；
The aluminum of 0.1～1.8wt%；
The copper of 0.2～0.6wt%；
The cobalt of 0.5～1wt%.
8. method according to claim 1, it is characterised in that the granularity of the powder is 2～8 microns.
9. method according to claim 1, it is characterised in that the magnetic field intensity of the magnetic field orientating forming processes >=
16000 Gausses.
10. method according to claim 1, it is characterised in that the powder is carried out after magnetic field orientating forming processes also
Including：
Product after magnetic field orientating forming processes is carried out isostatic pressed process, magnet idiosome is obtained；
The pressure that the isostatic pressed is processed is 180～240MPa.
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