CN106128676A - A kind of sintering method of neodymium iron boron magnetic body - Google Patents
A kind of sintering method of neodymium iron boron magnetic body Download PDFInfo
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- CN106128676A CN106128676A CN201610635404.7A CN201610635404A CN106128676A CN 106128676 A CN106128676 A CN 106128676A CN 201610635404 A CN201610635404 A CN 201610635404A CN 106128676 A CN106128676 A CN 106128676A
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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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- 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
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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
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention provides the sintering method of a kind of neodymium iron boron magnetic body, comprise the following steps, first under lasting vacuumized conditions, by neodymium iron boron magnetic body pressed compact after through the first stage, ladder-elevating temperature is fired, constant temperature under degassing temperature；Then stop continuing evacuation, proceed after second stage intensification constant temperature fires, to obtain neodymium iron boron magnetic body blank.The present invention is in numerous steps prepared by neodymium iron boron magnetic body, start with from sintering method, lasting evacuation is stopped during sintering, magnet is allowed to carry out follow-up sintering step under free vacuum state, rare earth element volatilization at high temperature can be effectively reduced, thus improve the magnetic property of magnet, especially reduce the temperature coefficient of neodymium iron boron, and then improve the stability of neodymium iron boron use at high temperature, moreover it is possible to reduce production cost.
Description
Technical field
The invention belongs to magnet preparing technical field, particularly relate to the sintering method of a kind of neodymium iron boron magnetic body.
Background technology
Either in commercial production the most in daily life, hard magnetic body i.e. permanent magnet, it is possible to long-term its magnetic of holding
Magnet, is difficult to loss of excitation, is difficult to be magnetized, and is all one of the most frequently used muscle material.Hard magnetic body can be divided into natural magnet and people
Making magnet, artificial magnet refers to can be reached the effect identical with natural magnet (magnet) by the alloy of synthesis different materials
Really, but also magnetic force can be improved.The sixties in 20th century, the appearance of rare earth permanent magnet, then the application for magnet opens one newly
Epoch, first generation samarium cobalt permanent magnet SmCo5, second filial generation precipitation hardenable samarium cobalt permanent magnet Sm2Co17, up to now, develop into the third generation
Nd-Fe-B permanent magnet material (NdFeB).Although at present ferrimagnet remains the permanent magnet material that consumption is maximum, but neodymium iron boron magnetic body
The output value substantially exceeded ferrite permanent-magnet materials, have evolved into a big industry.
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, be also the permanent magnet so far with the strongest magnetic force, its maximum magnetic energy product (BHmax) exceeds ferrite 10
More than Bei, when naked magnetic, its magnetic force can reach 3500 Gauss.The advantage of neodymium iron boron magnetic body is that cost performance is high, body
Long-pending little, lightweight, good mechanical property and the feature such as magnetic is strong, the advantage of such high-energy-density makes Nd-Fe-B permanent magnet material
Modern industry and electronic technology obtain a wide range of applications, is described as magnetic king in magnetics circle.Thus, the system of neodymium iron boron magnetic body
The focus that standby and extension always gives more sustained attention in the industry.
At present, industry makes Nd-Fe-B permanent magnet material frequently with sintering process, as Wang Wei waits at " key process parameter and alloy
The element impact on Sintered NdFeB magnetic property Yu mechanical property " in disclose and use sintering process to manufacture Nd-Fe-B permanent magnet material
Technological process, generally comprises that dispensing, melting, steel ingot be broken, powder process, vacuum preserves micropowder, powder is orientated compressing, vacuum
The steps such as sintering, inspection point and plating.Among these, sintering is it is critical that a link, the magnetic property pair of Nd-Fe-B permanent magnet
Sintering process is the most sensitive, the alloy of identical component, due to the difference of sintering process, its magnetic property can several times, Ji Shibei, even
The change of hundreds of times ground.Sintering purpose be below matrix phase fusing point a certain temperature through time process, make pressed compact shrink and densification,
And optimize crystal boundary by follow-up timeliness, it is achieved be separated the drag to increase farmland displacement, makes magnet have high permanent magnetism performance
Microscopic structure.The sintering method the most generally used is liquid-phase sintering and solid-phase sintering.
Along with the development of the association area such as air-conditioning, electric automobile, the demand of the multi-field application of neodymium iron boron magnetic body is more come
The most, its performance requirement be it is also proposed more requirement.Such as some fields such as motors, neodymium iron boron magnetic body needs 150～200
It is on active service between DEG C, and the Curie temperature of neodymium iron boron magnetic body is only 300 DEG C, thus, when magnet temperature under some use state surpasses
When crossing certain temperature, will subtract magnetic because of heat so that Magnet in use lost efficacy, this also becomes recent research in the industry
One of hot issue.
Therefore, the magnetic property of magnet, especially resistance to elevated temperatures, the most forward-looking neodymium ferrum can how be improved
Boron magnet generation manufacturer and the focus of research worker extensive concern.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide the sintering method of a kind of neodymium iron boron magnetic body, this
Bright by the improvement of sintering process in magnet preparation section, it is possible to the effective magnetic property improving neodymium iron boron magnetic body, thus improve
Its temperature tolerance.
The invention provides the sintering method of a kind of neodymium iron boron magnetic body, comprise the following steps:
A) under lasting vacuumized conditions, by neodymium iron boron magnetic body pressed compact after through the first stage, ladder-elevating temperature is fired, de-
Constant temperature under temperature；
B) stop continuing evacuation, proceed after second stage intensification constant temperature fires, to obtain neodymium iron boron magnetic body blank.
Preferably, the described vacuum pressure continuing evacuation is less than or equal to 0.5Pa；
The heating rate that described first stage ladder-elevating temperature is fired is 4～8 DEG C/min；
Described degassing temperature is 800～900 DEG C.
Preferably, the heating rate that described second stage intensification constant temperature is fired is 2～5 DEG C/min；
The temperature that described second stage intensification constant temperature is fired is 900～1080 DEG C；Described second stage intensification constant temperature is fired
Time be 1～15h.
Preferably, described degassing includes that first stage degassing and second stage deaerate；
The temperature of degassing of described first stage is 500～650 DEG C；The temperature of described second stage degassing is 800～900
℃。
Preferably, described step A) particularly as follows:
A1) under lasting vacuumized conditions, neodymium iron boron magnetic body pressed compact is carried out rises gentle constant temperature for the first time for the first time and fires；
A2) under lasting vacuumized conditions, then carry out second time heat up fire and second time constant temperature fire；
A3) under lasting vacuumized conditions, proceeding third time heat up fire and third time constant temperature fire.
Preferably, the heating rate that the intensification of described first time is fired is 4～8 DEG C/min；Described first time constant temperature is fired
Temperature is 200～300 DEG C；
The heating rate that the intensification of described second time is fired is 4～8 DEG C/min；The temperature that described second time constant temperature is fired is
500～650 DEG C；
The heating rate that the intensification of described third time is fired is 4～8 DEG C/min；The temperature that described third time constant temperature is fired is
800～900 DEG C.
Preferably, that described first time constant temperature is fired and that described second time constant temperature is fired cut-off condition is that vacuum pressure is little
In equal to 0.3Pa；
The cut-off condition that described third time constant temperature is fired is that vacuum pressure is constant or vacuum pressure is less than or equal to 0.2Pa.
Preferably, described step B) particularly as follows:
B1) stop continuing evacuation, proceed to rise gentle 4th constant temperature the 4th time and fire；
B2) carry out the 5th time rising after gentle 5th constant temperature fires again, obtain neodymium iron boron magnetic body blank.
Preferably, the described 4th time heating rate fired that heats up is 2～5 DEG C/min；Described 4th constant temperature is fired
Temperature is 1000～1060 DEG C；The time that described 4th time constant temperature is fired is 0.5～6h；
Described 5th time the heating rate fired that heats up is 2～4 DEG C/min；The temperature that described 5th time constant temperature is fired is
1020～1080 DEG C；The time that described 5th time constant temperature is fired is 0.5～6h.
Preferably, described step B) in, described second stage intensification constant temperature also includes cooling after firing；
Described cooling is specially air-cooled under conditions of nitrogen or noble gas.
The invention provides the sintering method of a kind of neodymium iron boron magnetic body, comprise the following steps, first at lasting evacuation bar
Under part, by neodymium iron boron magnetic body pressed compact after through the first stage, ladder-elevating temperature is fired, constant temperature under degassing temperature；Then stop continuing
Evacuation, proceeds after second stage intensification constant temperature fires, to obtain neodymium iron boron magnetic body blank.Compared with prior art, this
Bright serious for there is rare earth element volatilization loss in existing magnet preparation process, magnet composition is big with formula components difference, shadow
The problem ringing blank performance, in numerous steps prepared by neodymium iron boron magnetic body, starts with from sintering method, stops during sintering
The most lasting evacuation, allows magnet carry out follow-up sintering step under free vacuum state, can effectively reduce rare earth unit
Element volatilization at high temperature, thus improve the magnetic property of magnet, especially reduce the temperature coefficient of neodymium iron boron, and then improve neodymium ferrum
The stability of boron use at high temperature, moreover it is possible to reduce production cost.Test result indicate that, neodymium iron boron magnetic body prepared by the present invention
Comparing existing technique, HCJ (Hcj) improves 300～500Oe, and squareness (HK/Hcj) improves 0.01～0.02；
High temperature HCJ (Hcj) improves 300～500Oe, the high-temperature temperature system of the neodymium iron boron magnetic body Hcj that in addition prepared by the present invention
Number β can improve 0.01%～0.02% than existing technique, and residual magnetism temperature coefficient α is basically unchanged.
Accompanying drawing explanation
Fig. 1 is neodymium iron boron magnetic body pressed compact sintering process temperature curve schematic diagram in the present invention.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but
Should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention rather than to invention claim
Limit.
The all raw materials of the present invention, are not particularly limited its source, that commercially buy or according to people in the art
Prepared by the conventional method known to Yuan.
The all raw materials of the present invention, are not particularly limited its purity, present invention preferably employs analytical pure or sintered NdFeB
The conventional purity that field of magnets uses.
The invention provides the sintering method of a kind of neodymium iron boron magnetic body, comprise the following steps:
A) under lasting vacuumized conditions, by neodymium iron boron magnetic body pressed compact after through the first stage, ladder-elevating temperature is fired, de-
Constant temperature under temperature；
B) stop continuing evacuation, proceed after second stage intensification constant temperature fires, to obtain neodymium iron boron magnetic body blank.
Neodymium iron boron magnetic body pressed compact, first under lasting vacuumized conditions, is fired by the present invention through first stage ladder-elevating temperature
After, constant temperature under degassing temperature.
The sintering of described neodymium iron boron magnetic body is not particularly limited by the present invention, with neodymium iron boron well known to those skilled in the art
The sintering concept of magnet, the present invention is preferably liquid-phase sintering or solid-phase sintering, more preferably liquid-phase sintering, more preferably will
Loose being placed in material boat of the most compressing magnet pressed compact is fired in agglomerating plant.Described sintering is set by the present invention
For being not particularly limited, with the equipment of Sintered NdFeB magnet well known to those skilled in the art, the present invention is preferably true
Empty sintering furnace.Temperature homogeneity in the equipment of described sintering is not particularly limited by the present invention, ripe with those skilled in the art
The temperature known all with property, the temperature uniformity of vacuum sintering furnace of the present invention is preferably ± 5 DEG C, more preferably ± 4 DEG C,
Most preferably ± 3 DEG C.The source of described neodymium iron boron magnetic body pressed compact is not particularly limited by the present invention, ripe with those skilled in the art
The conventional production practices known, those skilled in the art can be according to practical condition, prescription and properties of product
Select and adjust, present invention preferably comprises that dispensing, melting, hydrogen explosion be broken, powder process and the main process such as orientation is compressing,
Obtain neodymium iron boron magnetic body pressed compact.
The described definition continuing evacuation is not particularly limited by the present invention, with well known to those skilled in the art conventional raw
The practical operation step of product process, it will be appreciated by those skilled in the art that the described evacuation that continues refers to produce in vacuum
Under the effect of device, sintering process persistently keeps the state that certain vacuum pressure is fired.The present invention to described very
Being not particularly limited of empty generator, with the pressure of conventional vacuum extractor well known to those skilled in the art, ability
Field technique personnel can select according to practical condition, prescription and properties of product and adjust, and the present invention is preferred
Can be 5.5kw～15kw for mechanical pumping power, or 7.5kw～13kw, or 10kw～11kw；Pumping speed can be 70
～150L/s, can be 80～140L/s, can be 100～120L/s；Lobe pump power can be 7.5～22kw, or
10kw～20kw, or 14kw～16kw；Pumping speed can be 600～1200L/s, can be 700～1100L/s, Ke Yiwei
800～1000L/s.The described initial pressure continuing evacuation is not particularly limited by the present invention, ripe with those skilled in the art
The vacuum pressure of the Sintered NdFeB magnet known, the vacuum pressure continuing evacuation of the present invention, i.e. initial vacuum pressure
Power is preferably less than equal to 0.5Pa, more preferably 0.01～0.5Pa, more preferably 0.05～0.4Pa, most preferably 0.1～
0.3Pa。
Curve of firing in described sintering process is not particularly limited by the present invention, and those skilled in the art can be according to reality
The border condition of production, prescription and properties of product select and adjust, and the present invention is to improve the performance of magnet further, institute
State the heating rate that first stage ladder-elevating temperature fires and be preferably 4～8 DEG C/min, more preferably 5～7 DEG C/min, most preferably
5.5～6.5 DEG C/min；Described degassing temperature is preferably 800～900 DEG C, more preferably 820～880 DEG C, most preferably 840～
860℃.The time of constant temperature under described degassing temperature is not particularly limited by the present invention, and those skilled in the art can be according to reality
The condition of production, prescription and properties of product select and adjust, and the present invention is preferably according to the vacuum pressure in sintering furnace
As reference frame, under conditions of lasting evacuation, i.e. under the Stabilization of vacuum extractor, constant temperature under described degassing temperature
Cut-off condition be preferably vacuum pressure less than or equal to 0.3Pa, i.e. when the vacuum pressure in sintering furnace is less than or equal to 0.3Pa,
Can stop third time constant temperature fire, more preferably 0.01～0.3Pa, more preferably 0.05～0.25Pa, most preferably 0.1～
0.2Pa.The definition of described degassing is not particularly limited by the present invention, with in magnet sintering process well known to those skilled in the art
Degassing defines, and it will be appreciated by those skilled in the art that in the sintering process of described magnet, is divided into skimming processes and degassing
Process, wherein degasification process preferably includes first stage degassing and second stage deaerates.First stage ladder liter of the present invention
Temperature is fired, and preferably refers to skimming processes, first stage degasification process and second stage degasification process.
The actual conditions of described skimming processes is not particularly limited by the present invention, with magnet well known to those skilled in the art
The actual conditions of skimming processes in sintering process, those skilled in the art can be according to practical condition, prescription
And properties of product select and adjust, defat platform temperature of the present invention, i.e. skimming temp are preferably 200～300 DEG C,
More preferably 220～280 DEG C, most preferably 240～260 DEG C；The heating rate of described skimming processes is preferably 4～8 DEG C/min,
More preferably 5～7 DEG C/min, most preferably 5.5～6.5 DEG C/min.
The actual conditions of described first stage degasification process is not particularly limited by the present invention, ripe with those skilled in the art
The actual conditions of degasification process in the magnet sintering process known, those skilled in the art can according to practical condition,
Prescription and properties of product select and adjust, the first degassing platform temperature of the present invention, i.e. first stage degassing
Temperature is preferably 500～650 DEG C, more preferably 525～625 DEG C, most preferably 550～600 DEG C；The degassing of described first stage
Heating rate is preferably 4～8 DEG C/min, more preferably 5～7 DEG C/min, most preferably 5.5～6.5 DEG C/min.
The actual conditions of described second stage degasification process is not particularly limited by the present invention, ripe with those skilled in the art
The actual conditions of degasification process in the magnet sintering process known, those skilled in the art can according to practical condition,
Prescription and properties of product select and adjust, the second degassing platform temperature, i.e. degassing temperature or the of the present invention
Two-stage degassing temperature, preferably 800～900 DEG C, more preferably 820～880 DEG C, most preferably 840～860 DEG C；Described
The two-stage heating rate of degassing is preferably 4～8 DEG C/min, more preferably 5～7 DEG C/min, most preferably 5.5～6.5 DEG C/
min。
The present invention is to improve the magnetic property of magnet, and thinning process controls, above-mentioned steps A) it is particularly preferred as:
A1) under lasting vacuumized conditions, neodymium iron boron magnetic body pressed compact is carried out rises gentle constant temperature for the first time for the first time and fires；
A2) under lasting vacuumized conditions, then carry out second time heat up fire and second time constant temperature fire；
A3) under lasting vacuumized conditions, proceeding third time heat up fire and third time constant temperature fire.
The parameter that described first time is heated up by the present invention is not particularly limited, and those skilled in the art can be raw according to reality
Product situation, prescription and properties of product select and adjust, and the heating rate that described first time heats up is preferably 4～8
DEG C/min, more preferably 4.5～7.5 DEG C/min, most preferably 5.5～6.5 DEG C/min.Described first time constant temperature is burnt by the present invention
The temperature of system is not particularly limited, and those skilled in the art can be according to practical condition, prescription and properties of product
Selecting and adjust, first time constant temperature of the present invention is fired, i.e. defat is fired, and the temperature that described first time constant temperature is fired is excellent
Elect 200～300 DEG C as, more preferably 210～270 DEG C, most preferably 230～250 DEG C.Described first time constant temperature is burnt by the present invention
The time of system is not particularly limited, and those skilled in the art can be according to practical condition, prescription and properties of product
Selecting and adjust, the vacuum pressure in the present invention preferably foundation sintering furnace is as reference frame, at the bar of lasting evacuation
Under part, i.e. under the Stabilization of vacuum extractor, the cut-off condition that described first time constant temperature is fired is preferably vacuum pressure and is less than
Equal to 0.3Pa, i.e. when the vacuum pressure in sintering furnace is less than or equal to 0.3Pa, constant temperature for the first time can be stopped and firing, more preferably
It is 0.01～0.3Pa, more preferably 0.05～0.25Pa, most preferably 0.1～0.2Pa.
The parameter that described second time is heated up by the present invention is not particularly limited, and those skilled in the art can be raw according to reality
Product situation, prescription and properties of product select and adjust, and the heating rate that described second time heats up is preferably 4～8
DEG C/min, more preferably 4.5～7.5 DEG C/min, most preferably 5.5～6.5 DEG C/min.Described second time constant temperature is burnt by the present invention
The temperature of system is not particularly limited, and those skilled in the art can be according to practical condition, prescription and properties of product
Selecting and adjust, second time constant temperature of the present invention is fired, i.e. first stage degassing is fired, and described second time constant temperature is fired
Temperature be preferably 500～650 DEG C, more preferably 530～620 DEG C, most preferably 560～590 DEG C.The present invention is to described second
The time that secondary constant temperature is fired is not particularly limited, those skilled in the art can according to practical condition, prescription and
Properties of product select and adjust, and the vacuum pressure in the present invention preferably foundation sintering furnace, as reference frame, is persistently being taken out
Under conditions of vacuum, i.e. under the Stabilization of vacuum extractor, the cut-off condition that described second time constant temperature is fired is preferably vacuum
Pressure is less than or equal to 0.3Pa, i.e. when the vacuum pressure in sintering furnace is less than or equal to 0.3Pa, can stop second time constant temperature and burn
System, more preferably 0.01～0.3Pa, more preferably 0.05～0.25Pa, most preferably 0.1～0.2Pa.
The parameter that described third time is heated up by the present invention is not particularly limited, and those skilled in the art can be raw according to reality
Product situation, prescription and properties of product select and adjust, and the heating rate that described third time heats up is preferably 4～8
DEG C/min, more preferably 4.5～7.5 DEG C/min, most preferably 5.5～6.5 DEG C/min.Described third time constant temperature is burnt by the present invention
The temperature of system is not particularly limited, and those skilled in the art can be according to practical condition, prescription and properties of product
Selecting and adjust, third time constant temperature of the present invention is fired, i.e. second stage degassing is fired, and described third time constant temperature is fired
Temperature be preferably 800～900 DEG C, more preferably 810～890 DEG C, most preferably 830～870 DEG C.The present invention is to the described 3rd
The time that secondary constant temperature is fired is not particularly limited, those skilled in the art can according to practical condition, prescription and
Properties of product select and adjust, and the vacuum pressure in the present invention preferably foundation sintering furnace, as reference frame, is persistently being taken out
Under conditions of vacuum, i.e. under the Stabilization of vacuum extractor, the cut-off condition that described third time constant temperature is fired is preferably vacuum
Pressure is less than or equal to 0.2Pa, i.e. when the vacuum pressure in sintering furnace is less than or equal to 0.2Pa, can stop third time constant temperature and burn
System, more preferably 0.01～0.2Pa, more preferably 0.05～0.15Pa, most preferably 0.08～0.12Pa.
Then the present invention stops lasting evacuation, proceeds after second stage intensification constant temperature fires, to obtain neodymium-iron-boron
Chaeta base.
The definition that the present invention continues evacuation to described stopping is not particularly limited, and those skilled in the art are based on general knowledge energy
Enough understand its correct connotation, i.e. stop vacuum extractor so that sintering furnace is fired under the effect without extraneous continuous vacuum pressure,
I.e. fire when free vacuum.
Curve of firing in described sintering process is not particularly limited by the present invention, and those skilled in the art can be according to reality
The border condition of production, prescription and properties of product select and adjust, and the present invention is to improve the performance of magnet further, institute
State the heating rate that second stage ladder-elevating temperature constant temperature fires and be preferably 2～5 DEG C/min, more preferably 2.5～4.5 DEG C/min,
Most preferably 3～4 DEG C/min；The temperature that described second stage ladder-elevating temperature constant temperature is fired is preferably 900～1080 DEG C, more preferably
It is 930～1050 DEG C, most preferably 960～1020 DEG C；The time that described second stage intensification constant temperature is fired is preferably 1～15h,
More preferably 4～12h, most preferably 7～9h.
The present invention is to improve the magnetic property of magnet, and thinning process controls, above-mentioned steps B) it is particularly preferred as:
B1) stop continuing evacuation, proceed to rise gentle 4th constant temperature the 4th time and fire；
B2) carry out the 5th time rising after gentle 5th constant temperature fires again, obtain neodymium iron boron magnetic body blank.
The described 4th time parameter fired that heats up is not particularly limited by the present invention, and those skilled in the art can be according to reality
The border condition of production, prescription and properties of product select and adjust, and described 4th time the heating rate fired that heats up is excellent
Elect 2～5 DEG C/min, more preferably 2.4～4.6 DEG C/min, most preferably 3.2～3.8 DEG C/min as.The present invention is to the described 4th
The temperature that secondary constant temperature is fired is not particularly limited, those skilled in the art can according to practical condition, prescription and
Properties of product select and adjust, and the temperature that 4th time of the present invention constant temperature is fired is preferably 1000～1060 DEG C, more excellent
Elect 1010～1050 DEG C as, most preferably 1020～1040 DEG C.The present invention does not has spy to the time that described 4th time constant temperature is fired
Not limiting, those skilled in the art can select according to practical condition, prescription and properties of product and adjust,
The time that 4th time of the present invention constant temperature is fired is preferably 0.5～6h, more preferably 1～5h, most preferably 2～4h.
The described 5th time parameter fired that heats up is not particularly limited by the present invention, and those skilled in the art can be according to reality
The border condition of production, prescription and properties of product select and adjust, and described 5th time the heating rate fired that heats up is excellent
Elect 2～4 DEG C/min, more preferably 2.3～3.7 DEG C/min, most preferably 2.7～3.3 DEG C/min as.The present invention is to the described 5th
The temperature that secondary constant temperature is fired is not particularly limited, those skilled in the art can according to practical condition, prescription and
Properties of product select and adjust, and the temperature that 5th time of the present invention constant temperature is fired is preferably 1020～1080 DEG C, more excellent
Elect 1030～1070 DEG C as, most preferably 1040～1060 DEG C.The present invention does not has spy to the time that described 5th time constant temperature is fired
Not limiting, those skilled in the art can select according to practical condition, prescription and properties of product and adjust,
The time that 5th time of the present invention constant temperature is fired is preferably 0.5～6h, more preferably 1～5h, most preferably 2～4h.
Technique after described intensification constant temperature is fired by the present invention is not particularly limited, with well known to those skilled in the art often
Rule step, the present invention is preferably cooling step and Ageing Treatment；The concrete technology of described cooling step is not had by the present invention
Limiting especially, those skilled in the art can be according to actual production process, batch, the concrete size of product and properties of product
Carrying out selective control, the present invention is to improve the magnetic property firing effect and neodymium iron boron magnetic body of neodymium iron boron magnetic body pressed compact, this
Bright preferably cool down under conditions of nitrogen or noble gas, the most air-cooled under conditions of nitrogen or noble gas,
The most air-cooled to less than 100 DEG C under conditions of argon；The speed of described cooling is not particularly limited by the present invention, with this
The cooldown rate of correlation step in neodymium iron boron magnetic body sintering process known to skilled person, those skilled in the art can
Regulate accordingly with the actual production process according to sintering furnace, batch and product size.The present invention to described timeliness at
The concrete steps of reason are not particularly limited, and with the concrete steps of neodymium iron boron magnetic body Ageing Treatment well known to those skilled in the art are
Can, those skilled in the art can regulate accordingly according to the actual production process of sintering furnace, batch and product size.
Although the present invention have employed the method for substep narration in above narration, but those skilled in the art can be correct
Understanding, above-mentioned steps of the present invention is a whole set of continuous firing i.e. sintering process, has continuous print sintering curre.Company of the present invention
It is neodymium iron boron magnetic body pressed compact sintering process temperature curve schematic diagram in the present invention that continuous sintering curre sees Fig. 1, Fig. 1.Such as Fig. 1 institute
Showing, 1 is intensification for the first time, and 2 fire (defat is fired) for constant temperature for the first time, and 3 fire for second time intensification, and 4 is second time constant temperature
Firing (first stage degassing is fired), 5 fire for third time intensification, and 6 fire (second stage degassing is fired) for third time constant temperature,
7 is that the 4th intensification is fired, and 8 is that the 4th constant temperature is fired, and 9 is that the 5th intensification is fired, and 10 is that the 5th constant temperature is fired, and 11 are
Cooling.
The present invention has obtained neodymium iron boron magnetic body blank through above-mentioned steps, then processes through Post isothermal treatment and post processing
After, obtain finished product neodymium iron boron magnetic body.Selection, concrete steps and the technique that above-mentioned Post isothermal treatment and post processing are processed by the present invention
Etc. being not particularly limited, with the post-processing steps in neodymium iron boron magnetic body well known to those skilled in the art, this area skill
Art personnel can be in optimized selection according to practical condition and prescription.
The content of neodymium iron boron magnetic body blank is not particularly limited by the present invention, forms the most by mass percentage, including Pr-
Nd:28%～33%；Dy:0～10%；Tb:0～10%；Nb:0～5%；Al:0～1%；B:0.5%～2.0%；Cu:0～
1%；Co:0～3%；Ga:0～2%；Gd:0～2%；Ho:0～2%；Zr:0～2%；Surplus is Fe.Wherein said Pr-Nd
Mass percentage content be preferably 29%～33%, more preferably 29%～32%, most preferably 29.5%～31%；Described
The mass percentage content of Dy is preferably 1.0%～9.0%, more preferably 2.0%～8.0%, most preferably 3.0%～
7.0%；The mass percentage content of described Tb is preferably 1.0%～9.0%, more preferably 2.0%～8.0%, most preferably
3.0%～7.0%；The mass percentage content of described Nb is preferably 1.0%～4.0%, more preferably 1.5%～3.5%,
It is preferably 1.8%～3.2%；The mass percentage content of described Al be preferably 0.2%～0.8%, more preferably 0.3%～
0.6%, most preferably 0.3%～0.5%；The mass percentage content of described B is preferably 0.8%～1%, more preferably
0.85%～1.3%, more preferably 0.9%～1.2%, most preferably 0.9%～1.1%；The mass percent of described Cu contains
Amount preferably 0.01%～0.8%, more preferably 0.02%～0.7%, most preferably 0.03%～0.6%；The matter of described Co
Amount degree is preferably 0.2%～2.0%, more preferably 0.3%～1.5%, most preferably 0.4%～1.2%；Described
The mass percentage content of Ga is preferably 0%～1.5%, more preferably 0.1%～1.2%, more preferably 0.15%～
1.0%, most preferably 0.2%～0.9%；The mass percentage content of described Gd is preferably 0.3%～1.5%, more preferably
0.5%～1.2%, more preferably 0.7%～1.0%, most preferably 0.8%～0.9%；The mass percentage content of described Ho
Be preferably 0.3%～1.5%, more preferably 0.5%～1.2%, more preferably 0.7%～1.0%, most preferably 0.8%～
0.9%；The mass percentage content of described Zr is preferably 0%～1.5%, more preferably 0.1%～1.2%, more preferably
0.15%～1.0%, most preferably 0.2%～0.9%.
The present invention, in numerous steps prepared by neodymium iron boron magnetic body, starts with from sintering method, stops during sintering
Lasting evacuation, allows magnet carry out follow-up sintering step under free vacuum state, and step refining sintering process of going forward side by side has
Imitate reduces rare earth element volatilization at high temperature, thus improves the magnetic property of magnet, especially reduces the temperature of neodymium iron boron
Coefficient, and then improve the stability of neodymium iron boron use at high temperature, moreover it is possible to reduce production cost.Test result indicate that, this
The neodymium iron boron magnetic body of bright preparation compares existing technique, and HCJ (Hcj) improves 300～500Oe, squareness (HK/Hcj)
Improve 0.01～0.02；High temperature HCJ (Hcj) improves 300～500Oe, the neodymium-iron-boron that in addition prepared by the present invention
The high-temperature temperature factor beta of body Hcj can improve 0.01%～0.02% than existing technique, and residual magnetism temperature coefficient α is basically unchanged.
In order to further illustrate the present invention, below in conjunction with the sintering of a kind of neodymium iron boron magnetic body that the present invention is provided by embodiment
Method is described in detail, but it is to be understood that these embodiments are to implement under premised on technical solution of the present invention,
Give detailed embodiment and concrete operating process, simply for further illustrating the features and advantages of the present invention, and not
Being limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following embodiment.
Embodiment 1
Preparation 35UH sintered NdFeB
The checking done with 35UH sintered neodymium iron boron material, composition of raw material is as shown in table 1 below:
| Element | PrNd | Dy | Ho | Al | B | Cu | Co | Zr | Ga | Fe |
| Wt% | 28.3 | 4.5 | 0 | 0.5 | 1.02 | 0.08 | 0.5 | 0 | 0 | Remaining |
First, by above-mentioned formula, allot 300Kg raw material, wherein iron staff rust cleaning, rare earth material carry out oil-free, amphidromic and
Rustless process, melts metal by vacuum melting (SC) under conditions of Frequency Induction Heating by the raw material prepared, finally obtains
Obtain Nd Fe B alloys.
Then inhaling hydrogen dehydrogenation in hydrogen broken furnace to crush, intermediate crusher crushes further, then by airflow milling nitrogen protection mill
Powder, powder mean particle sizes is 3.3 μm.
Again the neodymium iron boron material powder through airflow milling is mixed in V-type mixes powder machine, then carries out being orientated compressing,
Carry out isostatic cool pressing at isostatic pressing machine and obtain pressed compact, the most again under nitrogen protection, send into sintering furnace, enter according to following sintering procedure
Row sintering,
Then pressed compact is loaded vacuum sintering furnace, be evacuated to vacuum pressure to 0.3Pa, carry out first with 6.3 DEG C/min
Secondary intensification, carries out constant temperature for the first time by neodymium iron boron magnetic body pressed compact at 250 DEG C and fires, when in sintering furnace, vacuum pressure is down to 0.2Pa
After, carry out second time with 6.3 DEG C/min and heat up, neodymium iron boron magnetic body pressed compact is carried out second time constant temperature at 650 DEG C and fires, work as sintering
After in stove, vacuum pressure is down to 0.2Pa, with the speed of 6.3 DEG C/min rise to 850 DEG C carry out third time constant temperature fire, stove to be sintered
After interior pressure is down to 0.2Pa, when being warming up to 900 DEG C with the speed of 3.5 DEG C/min, close vacuum pump set, vacuum shape in holding furnace
State is continuously heating to 1020 DEG C, is incubated 0.5h, then with the ramp of 2 DEG C/min to 1040 DEG C, is incubated 7h, etc. EP (end of program)
After, argon is air-cooled, comes out of the stove when temp controlled meter temperature is less than 100 DEG C.
Use suitable aging technique to process, obtain neodymium iron boron magnetic body.
The neodymium iron boron magnetic body preparing above-mentioned steps carries out magnetism testing, and result sees table 2, and table 2 is implemented for the present invention
The neodymium iron boron magnetic body magnetic property of example 1 preparation and temperature coefficient correction data.
The neodymium iron boron magnetic body magnetic property of table 2 embodiment of the present invention 1 preparation and temperature coefficient correction data
As can be seen from Table 2, the magnetic property of neodymium iron boron magnetic body prepared by this sintering method significantly carries
Height, and coercive force temperature coefficient has significantly reduction, thus improve magnet stability at high temperature.
Embodiment 2
Preparation 45H sintered NdFeB
The checking done with 45H sintered neodymium iron boron material, composition of raw material is as shown in table 3 below:
| Element | PrNd | Dy | Tb | Al | B | Cu | Co | Zr | Ga | Fe |
| Wt% | 27.8 | 0.9 | 0 | 0.2 | 0.95 | 0.15 | 1 | 0.05 | 0.2 | Remaining |
First, by above-mentioned formula, allot 300Kg raw material, wherein iron staff rust cleaning, rare earth material carry out oil-free, amphidromic and
Rustless process, melts metal by vacuum melting (SC) under conditions of Frequency Induction Heating by the raw material prepared, finally obtains
Obtain Nd Fe B alloys.
Then inhaling hydrogen dehydrogenation in hydrogen broken furnace to crush, intermediate crusher crushes further, then by airflow milling nitrogen protection mill
Powder, powder mean particle sizes is 3.0～3.2 μm.
Again the neodymium iron boron material powder through airflow milling is mixed in V-type mixes powder machine, then carries out being orientated compressing,
Carry out isostatic cool pressing at isostatic pressing machine, the most again under nitrogen protection, send into sintering furnace, be sintered according to this sintering method:
Then pressed compact is loaded vacuum sintering furnace, be evacuated to vacuum pressure to 0.3Pa, carry out first with 6.3 DEG C/min
Secondary intensification, carries out constant temperature for the first time by neodymium iron boron magnetic body pressed compact at 250 DEG C and fires, when in sintering furnace, vacuum pressure is down to 0.2Pa
After, carry out second time with 6.3 DEG C/min and heat up, neodymium iron boron magnetic body pressed compact is carried out second time constant temperature at 650 DEG C and fires, work as sintering
After in stove, vacuum pressure is down to 0.2Pa, with the speed of 6.3 DEG C/min rise to 850 DEG C carry out third time constant temperature fire, stove to be sintered
After interior pressure is down to 0.2Pa, when being warming up to 900 DEG C with the speed of 3.5 DEG C/min, close vacuum pump set, vacuum shape in holding furnace
State is continuously heating to 1015 DEG C, is incubated 0.5h, is continuously heating to 1035 DEG C with 2 DEG C/min speed, is incubated 7h, etc. EP (end of program)
After, argon is air-cooled, comes out of the stove when temp controlled meter temperature is less than 100 DEG C.
Use suitable aging technique to process, obtain neodymium iron boron magnetic body.
The neodymium iron boron magnetic body preparing above-mentioned steps carries out magnetism testing, and result sees table 4, and table 4 is implemented for the present invention
The neodymium iron boron magnetic body magnetic property of example 2 preparation and temperature coefficient correction data.
The neodymium iron boron magnetic body magnetic property of table 4 embodiment of the present invention 2 preparation and temperature coefficient correction data
As shown in Table 4, using the sintering method that the present invention provides, the magnetic property of magnet increases substantially, coercivity temperature
Coefficient significantly reduces, and can improve magnet stability at high temperature.
Embodiment 3
Preparation 35SH sintered NdFeB
The checking done with 35SH sintered neodymium iron boron material, composition of raw material is as shown in table 3 below:
| Element | PrNd | Dy | Tb | Al | B | Cu | Co | Zr | Ga | Fe |
| Wt% | 29.3 | 3.5 | 0 | 0.5 | 1.02 | 0.15 | 0.6 | 0.05 | 0 | Remaining |
First, by above-mentioned formula, allot 300Kg raw material, wherein iron staff rust cleaning, rare earth material carry out oil-free, amphidromic and
Rustless process, melts metal by vacuum melting (SC) under conditions of Frequency Induction Heating by the raw material prepared, finally obtains
Obtain Nd Fe B alloys.
Then inhaling hydrogen dehydrogenation in hydrogen broken furnace to crush, intermediate crusher crushes further, then by airflow milling nitrogen protection mill
Powder, powder mean particle sizes is 3.25～3.45 μm.
Again the neodymium iron boron material powder through airflow milling is mixed in V-type mixes powder machine, then carries out being orientated compressing,
Carry out isostatic cool pressing at isostatic pressing machine, the most again under nitrogen protection, send into sintering furnace, be sintered according to this sintering method:
Then pressed compact is loaded vacuum sintering furnace, be evacuated to vacuum pressure to 0.3Pa, carry out first with 6.3 DEG C/min
Secondary intensification, carries out constant temperature for the first time by neodymium iron boron magnetic body pressed compact at 250 DEG C and fires, when in sintering furnace, vacuum pressure is down to 0.2Pa
After, carry out second time with 6.3 DEG C/min and heat up, neodymium iron boron magnetic body pressed compact is carried out second time constant temperature at 650 DEG C and fires, work as sintering
After in stove, vacuum pressure is down to 0.2Pa, with the speed of 6.3 DEG C/min rise to 850 DEG C carry out third time constant temperature fire, stove to be sintered
After interior pressure is down to 0.2Pa, when being warming up to 900 DEG C with the speed of 3.5 DEG C/min, close vacuum pump set, vacuum shape in holding furnace
State is continuously heating to 1017 DEG C, is incubated 0.5h, then with the ramp of 2 DEG C/min to 1037 DEG C, is incubated 7h, etc. EP (end of program)
After, argon is air-cooled, comes out of the stove when temp controlled meter temperature is less than 100 DEG C.
Use suitable aging technique to process, obtain neodymium iron boron magnetic body.
The neodymium iron boron magnetic body preparing above-mentioned steps carries out magnetism testing, and result sees table 5, and table 5 is implemented for the present invention
The neodymium iron boron magnetic body magnetic property of example 3 preparation and temperature coefficient correction data.
The neodymium iron boron magnetic body magnetic property of table 5 embodiment of the present invention 3 preparation and temperature coefficient correction data
As shown in Table 5, using the sintering method that the present invention provides, the magnetic property of magnet increases substantially, coercivity temperature
Coefficient significantly reduces, and can improve magnet stability at high temperature
Above the sintering method of a kind of neodymium iron boron magnetic body that the present invention provides is described in detail, used herein
Principle and the embodiment of the present invention are set forth by specific case, and the explanation of above example is only intended to help to understand
The method of the present invention and core concept thereof, including best mode, and also make any person skilled in the art can be real
Trample the present invention, including manufacturing and using any device or system, and the method implementing any combination.It should be pointed out that, for this skill
For the those of ordinary skill in art field, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out some changing
Entering and modify, these improve and modify in the protection domain also falling into the claims in the present invention.The scope of patent protection of the present invention
Be defined by the claims, and those skilled in the art can be included it is conceivable that other embodiments.If these other real
Execute example and there is the structural element being not different from claim character express, if or they include the word with claim
State the equivalent structural elements without essence difference, then these other embodiments also should comprise within the scope of the claims.
Claims (10)
1. the sintering method of a neodymium iron boron magnetic body, it is characterised in that comprise the following steps:
A) under lasting vacuumized conditions, by neodymium iron boron magnetic body pressed compact after through the first stage, ladder-elevating temperature is fired, in degassing temperature
The lower constant temperature of degree；
B) stop continuing evacuation, proceed after second stage intensification constant temperature fires, to obtain neodymium iron boron magnetic body blank.
Sintering method the most according to claim 1, it is characterised in that the described vacuum pressure of evacuation that continues is for being less than
In 0.5Pa；
The heating rate that described first stage ladder-elevating temperature is fired is 4～8 DEG C/min；
Described degassing temperature is 800～900 DEG C.
Sintering method the most according to claim 1, it is characterised in that the intensification speed that described second stage intensification constant temperature is fired
Rate is 2～5 DEG C/min；
The temperature that described second stage intensification constant temperature is fired is 900～1080 DEG C；Described second stage intensification constant temperature fire time
Between be 1～15h.
Sintering method the most according to claim 1, it is characterised in that described degassing includes first stage degassing and second-order
Section degassing；
The temperature of degassing of described first stage is 500～650 DEG C；The temperature of described second stage degassing is 800～900 DEG C.
Sintering method the most according to claim 1, it is characterised in that described step A) particularly as follows:
A1) under lasting vacuumized conditions, neodymium iron boron magnetic body pressed compact is carried out rises gentle constant temperature for the first time for the first time and fires；
A2) under lasting vacuumized conditions, then carry out second time heat up fire and second time constant temperature fire；
A3) under lasting vacuumized conditions, proceeding third time heat up fire and third time constant temperature fire.
Sintering method the most according to claim 5, it is characterised in that the heating rate that the intensification of described first time is fired is 4
～8 DEG C/min；The temperature that described first time constant temperature is fired is 200～300 DEG C；
The heating rate that the intensification of described second time is fired is 4～8 DEG C/min；The temperature that described second time constant temperature is fired be 500～
650℃；
The heating rate that the intensification of described third time is fired is 4～8 DEG C/min；The temperature that described third time constant temperature is fired be 800～
900℃。
Sintering method the most according to claim 6, it is characterised in that described first time constant temperature is that fire and described second time
The cut-off condition that constant temperature is fired is that vacuum pressure is less than or equal to 0.3Pa；
The cut-off condition that described third time constant temperature is fired is that vacuum pressure is constant or vacuum pressure is less than or equal to 0.2Pa.
8. according to the sintering method described in claim 1～7 any one, it is characterised in that described step B) particularly as follows:
B1) stop continuing evacuation, proceed to rise gentle 4th constant temperature the 4th time and fire；
B2) carry out the 5th time rising after gentle 5th constant temperature fires again, obtain neodymium iron boron magnetic body blank.
Sintering method the most according to claim 8, it is characterised in that described 4th time the heating rate fired that heats up is 2
～5 DEG C/min；The temperature that described 4th time constant temperature is fired is 1000～1060 DEG C；The time that described 4th time constant temperature is fired is
0.5～6h；
Described 5th time the heating rate fired that heats up is 2～4 DEG C/min；The temperature that described 5th time constant temperature is fired be 1020～
1080℃；The time that described 5th time constant temperature is fired is 0.5～6h.
Sintering method the most according to claim 1, it is characterised in that described step B) in, described second stage heats up permanent
Temperature also includes cooling after firing；
Described cooling is specially air-cooled under conditions of nitrogen or noble gas.
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| CN114068121A (en) * | 2021-12-24 | 2022-02-18 | 余姚市宏伟磁材科技有限公司 | Sintered neodymium-iron-boron magnet with low boundary phase potential difference and preparation method thereof |
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