CN105551790B - 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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- CN105551790B CN105551790B CN201610090762.4A CN201610090762A CN105551790B CN 105551790 B CN105551790 B CN 105551790B CN 201610090762 A CN201610090762 A CN 201610090762A CN 105551790 B CN105551790 B CN 105551790B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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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
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention provides a kind of sintering methods of neodymium iron boron magnetic body, include the following steps, first under conditions of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, reach sintering temperature, obtain neodymium iron boron magnetic body intermediate；Then under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, neodymium iron boron magnetic body blank is obtained.The present invention is in numerous steps prepared by neodymium iron boron magnetic body, start with from sintering method, by the specific high temperature sintering stage in sintering process, it is filled with hydrogen into system, keeps blank material richness neodymium distributed mutually uniform, rare-earth phase is prevented to be consumed, it avoids and generates rare earth phase oxide, be not only not necessarily to add rare earth in component design, saved cost, and the coercivity of product is also improved, have very important significance to the development tool of sintered NdFeB product.
Description
Technical field
The invention belongs to magnet preparing technical field more particularly to a kind of sintering methods of neodymium iron boron magnetic body.
Background technology
Either industrial production still in daily life, hard magnetic body, that is, permanent magnet can keep it magnetic for a long time
Magnet is not easy loss of excitation, is not easy to be magnetized and one of most common muscle material.Hard magnetic body can be divided into natural magnet and people
Magnet is made, artificial magnet refers to that can reach and the identical effect of natural magnet (magnet) by synthesizing the alloy of different materials
Fruit, but also magnetic force can be improved.Early in 18th century, there have been artificial magnets, but manufacture the process ten of more strong magnetic material
It is point slow, alnico magnet (AlNiCo) is produced until the 1930s, just makes it possible the large-scale application of magnet.
Then, it is manufactured that ferrite (Ferrite), the sixties, the appearance of rare earth permanent magnet are then the application of magnet the 1950s
Open a new era, first generation samarium cobalt permanent magnet SmCo5, second generation precipitation hardenable samarium cobalt permanent magnet Sm2Co17, so far,
Develop to third generation Nd-Fe-B permanent magnet material (NdFeB).Although current ferrimagnet is still the maximum permanent-magnet material of dosage,
But the output value of neodymium iron boron magnetic body has substantially exceeded ferrite permanent-magnet materials, has evolved into a big industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), chemical formula Nd2Fe14B is a kind of artificial
Permanent magnet, and the permanent magnet with most strong magnetic force so far, maximum magnetic energy product (BHmax) exceeds ferrite 10
Times or more, in the state of naked magnetic, magnetic force can reach 3500 Gauss.The advantages of neodymium iron boron magnetic body is cost-effective, body
The advantages of the features such as small, light-weight, good mechanical property of product and strong magnetism, such high-energy density, makes Nd-Fe-B permanent magnet material
It is had been widely used in modern industry and electronic technology, magnetic king is known as 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.
Currently, industry makes Nd-Fe-B permanent magnet material frequently with sintering process, such as Wang Wei exists《Key process parameter and alloy
Influence of the element to Sintered NdFeB magnetic property and mechanical property》In disclose Nd-Fe-B permanent magnet material manufactured using sintering process
Technological process generally comprises dispensing, melting, steel ingot are crushed, powder processed, vacuum preserve superfine powder, powder is orientated compression moulding, vacuum
Sintering, inspection point and plating and etc..Among these, sintering is a vital link, the magnetic property pair of Nd-Fe-B permanent magnet
Sintering process is very sensitive, the alloy of identical component, due to the difference of sintering process, magnetic property can several times, Ji Shibei, even
Change to hundreds of times.The purpose of sintering be below matrix phase fusing point a certain temperature through when handle, so that green compact is shunk and is densified,
And crystal boundary is optimized by follow-up timeliness, realize that phase separation to increase the drag of farmland displacement, makes magnet have high permanent magnetism performance
Microscopic structure.The sintering method of generally use is liquid-phase sintering and solid-phase sintering at present.
But in recent years, with neodymium iron boron magnetic body extensive use, promote and require more high stability and more inexpensive
Neodymium iron boron magnetic body production, however sintered Nd-Fe-B permanent magnet rare earth during sintering is easily aoxidized, and design is caused to match
Must add a little rare earths when square, or magnetic property the problems such as especially coercivity is undesirable after sintering, be increasingly becoming its into
The obstacle of one step development.
Thus, how by the improvement in magnet preparation process, reduce extra dilute in neodymium iron boron magnetic body production process
The consumption of soil improves magnet performance, is always the focus of neodymium iron boron magnetic body production firm extensive concern.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of sintering method of neodymium iron boron magnetic body, this hair
The sintering method of bright offer, in component design without increasing dilute additional rare earth, additionally it is possible to effectively improve neodymium iron boron magnetic body
Magnetic property.
The present invention provides a kind of sintering methods of neodymium iron boron magnetic body, include the following steps：
A) under conditions of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature,
Sintering temperature is reached, neodymium iron boron magnetic body intermediate is obtained；
B it) under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, obtains
Neodymium iron boron magnetic body blank.
Preferably, the sintering temperature is 1000~1100 DEG C.
Preferably, the heating rate of the continuous warming is 0.5~3 DEG C/min；The time of the continuous warming be 15~
120min。
Preferably, the ladder-elevating temperature the specific steps are：
A1 it) under conditions of vacuum or protective gas, after neodymium iron boron magnetic body green compact are carried out first time constant temperature firing, obtains
First intermediate；
A2 after the first intermediate) and then by above-mentioned steps obtained carries out second of constant temperature firing, the second intermediate is obtained；
A3 it after) the second intermediate for again obtaining above-mentioned steps carries out third time constant temperature firing, obtains in neodymium iron boron magnetic body
Mesosome.
Preferably, the temperature that the first time constant temperature is fired is 200~250 DEG C；The time that the first time constant temperature is fired
For 90~150min；
The temperature that second of the constant temperature is fired is 450~550 DEG C；The time that second of the constant temperature is fired is 60~
120min；
The temperature that the third time constant temperature is fired is 750~850 DEG C；The time that second of the constant temperature is fired is 90~
120min。
Preferably, described to be specially under conditions of hydrogen：
It is directly filled with hydrogen into equipment, or the protective gas in agglomerating plant is first evacuated to vacuum, then is set to sintering
It is filled with hydrogen in standby.
Preferably, the pressure of the vacuum is less than or equal to 10Pa；The pressure of the hydrogen is 0.030~0.098MPa.
Preferably, the step B) further include,
Neodymium iron boron magnetic body intermediate after constant temperature is fired, is cooled down under conditions of hydrogen, obtains neodymium iron boron magnetic body
Blank.
Preferably, the rate of the cooling is 6.0~8.5 DEG C/min.
The present invention provides a kind of neodymium iron boron magnetic body, the neodymium iron boron magnetic body be by neodymium iron boron magnetic body green compact hydrogen item
Under part, obtained after liquid-phase sintering or solid-phase sintering.
The present invention provides a kind of sintering methods of neodymium iron boron magnetic body, include the following steps, first in vacuum or protection gas
Under conditions of body, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, sintering temperature is reached, neodymium-iron-boron is obtained
Body intermediate；Then it under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, obtains
To neodymium iron boron magnetic body blank.Compared with prior art, the present invention is in numerous steps prepared by neodymium iron boron magnetic body, from sintering method
Start with, by the specific high temperature sintering stage in sintering process, hydrogen is filled with into system, keeps blank material richness neodymium distributed mutually equal
It is even, it prevents rare-earth phase from being consumed, avoids and generate rare earth phase oxide, be not only not necessarily to add a little rare earths in component design, save
About cost, and the magnetic property of product is also improved, have very important significance to the development tool of sintered NdFeB product.Experiment
The result shows that using the sintering method of neodymium iron boron magnetic body provided by the invention, it is practical raw compared to original when composition of raw materials calculates
The rare earth of additionally addition 0.5%~2%, the method that the present invention passes through hydrogenation protecting and logical hydrogen reduction aoxidizes phase, section are needed in production
0.5%~3% rare earth is saved.And neodymium iron boron magnetic body prepared by the present invention compares prior art, room temperature (20 DEG C) magnet
Neodymium iron boron magnetic body remanent magnetism (Br) improves about 1.63% in energy, and intrinsic coercivity (Hcj) improves about 9.17%, squareness (HK/
Hcj about 1.04%) is improved；Neodymium iron boron magnetic body remanent magnetism (Br) improves about 10.5% in high temperature (150 DEG C) magnet performance, intrinsic
Coercivity (Hcj) improves about 21%, and squareness (HK/Hcj) improves about 1.04%, the neodymium-iron-boron that in addition prepared by the present invention
The high-temperature temperature coefficient (α) of body Hcj can reach -0.420~-0.527%/DEG C.
Description of the drawings
Fig. 1 is neodymium iron boron magnetic body green sintering technological temperature curve synoptic diagram in the present invention；
Fig. 2 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1；
Fig. 3 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by common process；
Fig. 4 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1；
Fig. 5 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2；
Fig. 6 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2；
Fig. 7 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3；
Fig. 8 is the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Specific implementation mode
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are intended merely to the feature and advantage further illustrated the present invention, rather than to invention claim
Limitation.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to people in the art
It is prepared by conventional method known to member.
All raw materials of the present invention, are not particularly limited its purity, pure present invention preferably employs analyzing.
The present invention provides a kind of sintering methods of neodymium iron boron magnetic body, include the following steps：
A) under conditions of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature,
Sintering temperature is reached, neodymium iron boron magnetic body intermediate is obtained；
B it) under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, obtains
Neodymium iron boron magnetic body blank.
Neodymium iron boron magnetic body green compact under conditions of vacuum or protective gas, are passed through continuous warming or ladder by the present invention first
After heating, sintering temperature is reached, neodymium iron boron magnetic body intermediate is obtained.
The sintering is not particularly limited in the present invention, with the sintering side of neodymium iron boron magnetic body well known to those skilled in the art
Method, the present invention are preferably liquid-phase sintering or solid-phase sintering, more preferably liquid-phase sintering.The present invention does not have the protective gas
There is special limitation, it is of the present invention with the protective gas well known to those skilled in the art for Sintered NdFeB magnet
Protective gas is preferably inert gas and/or nitrogen, more preferably argon gas and/or nitrogen, most preferably argon gas or nitrogen；This hair
The bright pressure to the vacuum is not particularly limited, with the vacuum pressure of Sintered NdFeB magnet well known to those skilled in the art
, vacuum pressure of the invention, which is preferably less than, is equal to 10Pa, is more preferably less than equal to 1Pa, is more preferably less than equal to
0.3Pa, most preferably 0.01~0.3Pa.
The sintering temperature is not particularly limited in the present invention, with Sintered NdFeB magnet well known to those skilled in the art
Temperature, the present invention is preferably 1000~1100 DEG C, more preferably 1010~1090 DEG C, more preferably 1030~1070
DEG C, most preferably 1040~1060 DEG C.The equipment of the sintering is not particularly limited in the present invention, ripe with those skilled in the art
The equipment for the Sintered NdFeB magnet known, the present invention are preferably vacuum sintering furnace.The present invention gives birth to the neodymium iron boron magnetic body
Preparation process early period of base is not particularly limited, can also root with conventional production practices well known to those skilled in the art
It is adjusted according to practical condition or quality requirement, present invention preferably comprises dispensing, melting, hydrogen is quick-fried, powder processed and is orientated compacting
Equal main process, obtain neodymium iron boron magnetic body green compact.
The present invention is the magnetic property of the firing effect and neodymium iron boron magnetic body that improve neodymium iron boron magnetic body green compact, preferably above-mentioned steps
The rate of the heating is not particularly limited in specially continuous warming, the present invention, with neodymium iron well known to those skilled in the art
Heating rate in boron magnet sintering process, those skilled in the art can according to batch, the specific size of product with
And properties of product carry out selective control, the rate of continuous warming of the present invention is preferably 0.5~3 DEG C/min, more preferably 1
~2.5 DEG C/min, most preferably 1.5~2 DEG C/min；The time of the continuous warming is preferably 15~120min, more preferably
30~100min, most preferably 50~70min.
The present invention is the magnetic property of the firing effect and neodymium iron boron magnetic body that improve neodymium iron boron magnetic body green compact, preferably above-mentioned steps
Also preferably ladder-elevating temperature, it is specific more preferably first under conditions of vacuum or protective gas, neodymium iron boron magnetic body green compact are carried out
After first time constant temperature is fired, the first intermediate is obtained；Then the first intermediate above-mentioned steps obtained carries out second of constant temperature
After firing, the second intermediate is obtained；After the second intermediate that above-mentioned steps are obtained again carries out third time constant temperature firing, neodymium is obtained
Iron boron magnet intermediate.
The present invention is not special to the actual temp of neodymium iron boron magnetic body green compact progress first time constant temperature firing and time
Limitation, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can basis
Batch and the specific size of product carry out selective control, and the present invention is to improve to fire effect and properties of product, and described first
The temperature that secondary constant temperature is fired is preferably 200~250 DEG C, more preferably 210~240 DEG C, most preferably 220~230 DEG C；Described
The time that constant temperature is fired is preferably 90~150min, more preferably 100~140min, most preferably 110~130min.This
The other conditions that the first time constant temperature is fired in invention are not particularly limited, with sintering neodymium iron well known to those skilled in the art
The condition of boron magnet.The present invention has carried out the neodymium iron boron magnetic body green compact for the first time under the conditions of above-mentioned temperature and time
Constant temperature is fired, and neodymium iron boron magnetic body green compact generated steam in sintering procedure has been discharged in thermostatic process.
The present invention is not special to the actual temp of the neodymium iron boron magnetic body green compact second of constant temperature firing of progress and time
Limitation, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can basis
Batch and the specific size of product carry out selective control, and the present invention is to improve to fire effect and properties of product, and described second
The temperature that secondary constant temperature is fired is preferably 450~550 DEG C, more preferably 460~540 DEG C, most preferably 480~510 DEG C；Described
The time that secondary constant temperature is fired is preferably 60~120min, more preferably 70~110min, most preferably 80~100min.This hair
The bright other conditions fired to second of the constant temperature are not particularly limited, with sintered NdFeB well known to those skilled in the art
The condition of magnet.The neodymium iron boron magnetic body green compact have been carried out second of perseverance by the present invention under the conditions of above-mentioned temperature and time
Temperature is fired, and the organic matter contained in neodymium iron boron magnetic body green compact has effectively been discharged.
The present invention is not special to the actual temp of neodymium iron boron magnetic body green compact progress third time constant temperature firing and time
Limitation, with neodymium iron boron magnetic body green sintering process well known to those skilled in the art, those skilled in the art can basis
Batch and the specific size of product carry out selective control, and the present invention is to improve to fire effect and properties of product, the third
The temperature that secondary constant temperature is fired is preferably 750~850 DEG C, more preferably 760~840 DEG C, most preferably 780~810 DEG C；Described
The time that secondary constant temperature is fired is preferably 90~120min, more preferably 80~110min, most preferably 60~90min.This hair
The bright other conditions fired to the third time constant temperature are not particularly limited, with sintered NdFeB well known to those skilled in the art
The condition of magnet.The neodymium iron boron magnetic body green compact have been carried out third time perseverance by the present invention under the conditions of above-mentioned temperature and time
Temperature is fired, and neodymium iron boron magnetic body green compact generated hydrogen in sintering procedure has been discharged in thermostatic process.The present invention is to institute
The process for stating firing is especially limited without other, with the process of Sintered NdFeB magnet well known to those skilled in the art.
The present invention obtains neodymium iron boron magnetic body intermediate after above-mentioned continuous firing or the three times firing of ladder-elevating temperature constant temperature,
Then under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, neodymium iron boron is obtained
Magnet blank.
Concrete operations under conditions of hydrogen are not particularly limited in the present invention, with well known to those skilled in the art normal
Operating procedure is advised, it is under vacuum or under conditions of protective gas, such as that the present invention, which preferably depends on abovementioned steps,
Fruit abovementioned steps are under vacuum, then hydrogen to be preferably directly filled with into equipment；If abovementioned steps are the items in protective gas
Under part, then the protective gas in agglomerating plant is first preferably evacuated to vacuum, then hydrogen is filled with into agglomerating plant.The present invention is to institute
It states and is evacuated to the pressure of vacuum and is not particularly limited, the vacuum pressure with Sintered NdFeB magnet well known to those skilled in the art is
Can, the pressure for being evacuated to vacuum of the invention, which is preferably less than, is equal to 10Pa, is more preferably less than equal to 1Pa, more preferably less than
Equal to 0.3Pa, most preferably 0.01~0.3Pa.
The pressure of the hydrogen is not particularly limited in the present invention, and those skilled in the art can be according to batch, product
Specific size and properties of product carry out selective control, the present invention is preferably 0.030~0.098MPa, more preferably
0.040~0.090MPa, more preferably 0.050~0.080MPa, most preferably 0.060~0.070MPa.Perseverance of the present invention
The temperature that temperature is fired is preferably 1000~1100 DEG C, and more preferably 1010~1090 DEG C, more preferably 1030~1070 DEG C are optimal
It is selected as 1040~1060 DEG C preferably 1020~1050 DEG C；More preferably 1030~1040 DEG C, most preferably 1035 DEG C.The present invention
To the constant temperature fire time be not particularly limited, field technology personnel can according to batch, the specific size of product with
And properties of product carry out selective control, the present invention is preferably 180~600min, more preferably 250~550min, more preferably
300~500min, most preferably 350~450min.
Technique is not particularly limited after the present invention fires the constant temperature, with conventional steps well known to those skilled in the art
, the present invention is preferably cooling step；The concrete technology of the cooling step is not particularly limited in the present invention, this field skill
Art personnel can carry out selective control according to actual production process, batch, the specific size of product and properties of product, this
Invention is improves the magnetic property of the firing effect and neodymium iron boron magnetic body of neodymium iron boron magnetic body green compact, and the present invention is preferably in the condition of hydrogen
Under cooled down；The present invention is preferably 6.0~8.5 DEG C/min to the rate of the cooling, more preferably 6.3~8.2 DEG C/min,
More preferably 6.5~8.0 DEG C/min, most preferably 7.0~7.5 DEG C/min.The present invention is to above-mentioned temperature after cooling without spy
It does not limit, with the cooling temperature of correlation step in neodymium iron boron magnetic body sintering process well known to those skilled in the art, this hair
It is bright preferably 100 DEG C hereinafter, more preferably 90 DEG C hereinafter, most preferably 20~80 DEG C；The present invention does not have the time of above-mentioned cooling
There are special limitation, those skilled in the art that can accordingly be adjusted according to the batch and product size of sintering furnace.
The present invention is filled with hydrogen into system by the specific high temperature sintering stage in sintering process, plays deoxygenation and goes back
The effect of primary oxide, be further flushed with hydrogen after firing gas carry out it is air-cooled, keep blank material richness neodymium distributed mutually uniform, prevent rare earth
It is mutually consumed, avoids and generate rare earth phase oxide, be not only not necessarily to add a little rare earths in component design, saved cost, and
And also improve the coercivity of product.
The present invention obtains neodymium iron boron magnetic body blank after above-mentioned steps are by neodymium iron boron magnetic body green sintering, and the present invention exists
Although front narration in use substep narration method, those skilled in the art can correct understanding, the present invention it is above-mentioned
Step is the process of a whole set of continuous firing, has continuous sintering curre.Continuous sintering curre of the present invention is referring to figure
1, Fig. 1 is neodymium iron boron magnetic body green sintering technological temperature curve synoptic diagram in the present invention.As shown in Figure 1, deflation curve (a) and burning
The temperature curve (b) of continuous warming curve or staged heating when knot, wherein T1For the temperature that first time constant temperature is fired, T2For
The temperature that second of constant temperature is fired, T3For the temperature that third time constant temperature is fired, TIt burnsFor sintering temperature, the stage for being flushed with hydrogen gas is to burn
During carrying out constant temperature firing under junction temperature and in cooling procedure.
The present invention has obtained neodymium iron boron magnetic body blank by above-mentioned steps, is processed using Post isothermal treatment and post-processing
Afterwards, finished product neodymium iron boron magnetic body is obtained.Selection, specific steps and technique of the present invention to above-mentioned Post isothermal treatment and post-processing processing
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 field skill
Art personnel can be in optimized selection according to practical condition and quality requirement.
The present invention provides a kind of neodymium iron boron magnetic body, the neodymium iron boron magnetic body be by neodymium iron boron magnetic body green compact hydrogen item
Under part, obtained after liquid-phase sintering or solid-phase sintering.
The neodymium iron boron magnetic body is not particularly limited in the present invention, is with neodymium iron boron magnetic body well known to those skilled in the art
Can, the present invention is preferably Sintered NdFeB magnet；The concrete composition of the neodymium iron boron magnetic body is not particularly limited in the present invention, with
Routine neodymium iron boron magnetic body composition well known to those skilled in the art.The present invention does not have other processing steps of the sintering
Especially limitation, with the processing step in the sintering process of neodymium iron boron magnetic body well known to those skilled in the art.
Performance detection is carried out to the neodymium iron boron magnetic body that above-mentioned steps of the present invention obtain, the experimental results showed that, using the present invention
The sintering method of the neodymium iron boron magnetic body of offer, when composition of raw materials calculates, compared to needing additionally to add in original actual production
0.5%~2% rare earth, the method that the present invention aoxidizes phase by hydrogenation protecting and logical hydrogen reduction, saves 0.5%~3%
Rare earth.
To the neodymium iron boron magnetic body for preparing of the present invention respectively under conditions of 20 DEG C (room temperature) and 150 DEG C (high temperature), progress magnetic
Body performance detection, referring to table 1, table 1 is the neodymium iron boron magnetic body that is prepared with common process of the neodymium iron boron magnetic body for preparing of the present invention normal
Magnetic property correction data under mild hot conditions.
The neodymium iron boron magnetic body that neodymium iron boron magnetic body prepared by 1 present invention of table is prepared with common process is in room temperature and hot conditions
Under magnetic property correction data
As shown in Table 1, the neodymium iron boron magnetic body that prepared by the present invention compares prior art, neodymium iron in room temperature (20 DEG C) magnet performance
Boron magnet remanent magnetism (Br) improves about 1.63%, and intrinsic coercivity (Hcj) improves about 9.17%, and squareness (HK/Hcj) improves
About 1.04%；Neodymium iron boron magnetic body remanent magnetism (Br) improves about 10.5% in high temperature (150 DEG C) magnet performance, intrinsic coercivity
(Hcj) about 21% is improved, squareness (HK/Hcj) improves about 1.04%.
It being computed and learns, the high-temperature temperature coefficient (α) of neodymium iron boron magnetic body Hcj prepared by the present invention is increased to -0.420~-
0.527%/DEG C, and the Hcj high-temperature temperature coefficients of common process only -0.55~-0.78%/DEG C, this shows the burning of the present invention
Knot method can significantly improve the temperature stability of material.
The neodymium iron boron magnetic body prepared to the present invention carries out other performance detections, and referring to table 2, table 2 is neodymium prepared by the present invention
The neodymium iron boron magnetic body that iron boron magnet is prepared with common process subtracts magnetic situation.
Subtract magnetic stripe part：120 DEG C × 2h, equipment：High temperature drying case.
The neodymium iron boron magnetic body that neodymium iron boron magnetic body prepared by 2 present invention of table is prepared with common process subtracts magnetic situation
| Subtract magnetic | |
| Strong magnetic sintering process | 0.5%~2.8% |
| Normal process | 5%~10% |
As shown in Table 2, the neodymium iron boron magnetic body that prepared by the present invention compares prior art, magnet to subtract magnetic situation preferable.
Referring to table 3, table 3 is the aging feelings for the neodymium iron boron magnetic body that neodymium iron boron magnetic body prepared by the present invention is prepared with common process
Condition.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar；
Equipment：HAST ageing ovens
The aging conditions for the neodymium iron boron magnetic body that neodymium iron boron magnetic body prepared by 3 present invention of table is prepared with common process
| Weightlessness/mg/cm2 | |
| It is flushed with hydrogen sintering process | 0.8~1.5 |
| Normal process | 2.0~8.0 |
In order to further illustrate the present invention, with reference to embodiment to the sintering method of neodymium iron boron magnetic body provided by the invention
It is described in detail, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Prepare 38SH sintered NdFeBs
First, Pr and Nd are weighed according to mass percentage composition：25.1wt%, Dy：2wt%, Ho：4wt%, Al：
0.44wt%, B：0.94wt%, Cu：0.15wt%, Co：1.5wt%, Zr：0.15wt%, Ga：0.2wt% and surplus
Fe obtains neodymium iron boron green compact by ingot casting, broken, milling, magnetic field orientating, compression moulding.
Then green compact are packed into vacuum sintering furnace, are evacuated to vacuum degree to 0.3Pa, by neodymium iron boron magnetic body green compact 200
DEG C carry out first time constant temperature fire 90min after, obtain the first intermediate；Then the first intermediate that above-mentioned steps obtain is existed
After 500 DEG C carry out second of constant temperature firing 60min, the second intermediate is obtained；The second intermediate that above-mentioned steps obtain is existed again
After 750 DEG C carry out third time constant temperature firing 90min, neodymium iron boron magnetic body intermediate is obtained.
It is right after the neodymium iron boron magnetic body intermediate that above-mentioned steps are obtained again carries out constant temperature liquid-phase sintering 30min at 1020 DEG C
Above-mentioned neodymium iron boron magnetic body intermediate is flushed with hydrogen gas 0.052MPa, it is above-mentioned be flushed with hydrogen effect under, closed after logical hydrogen constant temperature liquid-phase sintering 30min
Close hydrogen charging valve, liquid-phase sintering intermediate；
Then continue to be sintered 60min at this temperature, stop heating, into cooling stage, gas is flushed with hydrogen into sintering furnace extremely
0.085-0.098MPa, machine air blast of blowing in are cooled to 60 DEG C and come out of the stove, and it is that (differently- oriented directivity is 29 rulers to 51.2*51*29mm to obtain specification
It is very little) neodymium iron boron magnetic body blank.
Finally, with surface grinding machine that oriented surface one side 60% is light-exposed, it is glued on iron staff with 502, is cut with inside diameter slicer
At 9.59*6.69*0.88 (M) black-film, with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.2mm with automatic chamfering machine, go
Fall burrs on edges, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 8 μm to obtain zinc coating thickness, and size is
The neodymium iron boron magnetic body finished product of (9.95*6.69*0.88 M).
The neodymium iron boron magnetic body that above-mentioned steps obtain is observed using XJ-63 type metallographic microscopes, as a result such as Fig. 2 institutes
Show, Fig. 2 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1；It is common process system referring to Fig. 3, Fig. 3
The metallurgical microstructrue figure of standby neodymium iron boron magnetic body.From Fig. 2 with the comparison of Fig. 3 as can be seen that comparing the agglomerant not being flushed with hydrogen
Skill, the neodymium iron boron magnetic body crystal grain that the present embodiment is prepared significantly are densified, through survey calculation, prepared by the embodiment of the present invention 1
The crystal grain average value of neodymium iron boron magnetic body is 4.62 μm, and the crystal grain average value of neodymium iron boron magnetic body prepared by common process is 6.78 μ
M, the present invention have refined 31.8% compared to the crystallite dimension of common process.
The magnetic property and magnet density of the neodymium iron boron magnetic body product obtained to above-mentioned steps are detected, experimental result ginseng
See that Fig. 4, Fig. 4 are the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.Referring to table 4, table 4 is to implement
The magnetic property data of neodymium iron boron magnetic body prepared by example 1 at ambient and elevated temperatures.
The magnetic property data of neodymium iron boron magnetic body prepared by 4 embodiment 1 of table at ambient and elevated temperatures
Other performance detections are carried out to neodymium iron boron magnetic body manufactured in the present embodiment, referring to table 5, table 5 is the embodiment of the present invention 1
The magnet ingredient situation of the neodymium iron boron magnetic body of preparation.
Equipment：ICP.
The ingredient situation of neodymium iron boron magnetic body prepared by 5 embodiment of the present invention 1 of table
| Total amount of rare earth | |
| Formula | 31.1 |
| It is flushed with hydrogen sintering process | 31.0 |
| Normal sintering process | 29.2 |
As shown in Table 5, the neodymium iron boron magnetic body that prepared by the embodiment of the present invention 1 compares prior art, and the rare earth of magnet consumes feelings
Condition is especially few.
Referring to table 6, table 6 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar；
Equipment：HAST ageing ovens
The aging conditions of neodymium iron boron magnetic body prepared by 6 embodiment of the present invention 1 of table
| Weightlessness/mg/cm2 | |
| It is flushed with hydrogen sintering process | 1.5 |
Can be, it is evident that neodymium iron boron magnetic body sintering method provided by the invention by above-mentioned testing result, it can be apparent
The magnet performances such as remanent magnetism, coercivity, maximum magnetic energy product, the squareness of magnet are improved, and there is preferable high-temperature stability.
Embodiment 2
Prepare 42SH sintered NdFeBs
First, it is formulated dispensing by 42SH, by ingot casting, broken, milling, magnetic field orientating, compression moulding, obtains neodymium iron boron life
Base.
Then green compact are packed into vacuum sintering furnace, are evacuated to vacuum degree and are less than 0.3Pa, neodymium iron boron magnetic body green compact is existed
After 230 DEG C carry out first time constant temperature firing 70min, the first intermediate is obtained；Then the first intermediate above-mentioned steps obtained
After carrying out second of constant temperature firing 80min at 520 DEG C, the second intermediate is obtained；The second intermediate that above-mentioned steps are obtained again
After carrying out third time constant temperature firing 120min at 780 DEG C, neodymium iron boron magnetic body intermediate is obtained.
It is right after the neodymium iron boron magnetic body intermediate that above-mentioned steps are obtained again carries out constant temperature liquid-phase sintering 30min at 1040 DEG C
Above-mentioned neodymium iron boron magnetic body intermediate 0.065MPa is flushed with hydrogen after constant temperature liquid-phase sintering 40min to close and fill under the action of above-mentioned hydrogen
Air valve, liquid-phase sintering intermediate；
Then continue to be sintered 60min at this temperature, stop heating, into cooling stage, gas is flushed with hydrogen into sintering furnace extremely
0.085-0.098Mpa, machine air blast of blowing in are cooled to 60 DEG C and come out of the stove, and it is that (differently- oriented directivity is 29 rulers to 51*44*31mm to obtain specification
It is very little) neodymium iron boron magnetic body blank.
Finally, with surface grinding machine that oriented surface one side 60% is light-exposed, it is glued on iron staff with 502, is cut with inside diameter slicer
At 17*8*1.4 (M) black-film, with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.2mm with automatic chamfering machine, remove edge
Burr, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 10 μm to obtain zinc coating thickness, size 17*8*1.4
(M) neodymium iron boron magnetic body finished product.
The neodymium iron boron magnetic body that above-mentioned steps obtain is observed using XJ-63 type metallographic microscopes, as a result such as Fig. 5 institutes
Show, Fig. 5 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2；From fig. 5, it can be seen that the present embodiment
The neodymium iron boron magnetic body crystal grain being prepared significantly is densified, the neodymium iron boron magnetic body prepared through survey calculation, the embodiment of the present invention 2
Crystal grain average value is 4.83 μm.
The magnetic property and magnet density of the neodymium iron boron magnetic body product obtained to above-mentioned steps are detected, experimental result ginseng
See that Fig. 6, Fig. 6 are the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.Referring to table 7, table 7 is to implement
The magnetic property data of neodymium iron boron magnetic body prepared by example 2 at ambient and elevated temperatures.
The magnetic property data of neodymium iron boron magnetic body prepared by 7 embodiment 2 of table at ambient and elevated temperatures
Other performance detections are carried out to neodymium iron boron magnetic body manufactured in the present embodiment, referring to table 8, table 8 is the embodiment of the present invention 2
The ingredient situation of the neodymium iron boron magnetic body of preparation.
Equipment：ICP.
Neodymium iron boron magnetic body prepared by 8 embodiment of the present invention 2 of table subtracts magnetic situation
| Total amount of rare earth | |
| Formula | 31.6 |
| It is flushed with hydrogen sintering process | 31.3 |
| Normal sintering process | 29.4 |
As shown in Table 8, the neodymium iron boron magnetic body that prepared by the embodiment of the present invention 2 compares prior art, and the rare earth consumption of magnet is special
It is not few.
Referring to table 9, table 9 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar；
Equipment：HAST ageing ovens
The aging conditions of neodymium iron boron magnetic body prepared by 9 embodiment of the present invention 2 of table
| Weightlessness/mg/cm2 | |
| It is flushed with hydrogen sintering process | 0.8 |
Can be, it is evident that neodymium iron boron magnetic body sintering method provided by the invention by above-mentioned testing result, it can be apparent
The magnet performances such as remanent magnetism, coercivity, maximum magnetic energy product, the squareness of magnet are improved, and there is preferable high-temperature stability.
Embodiment 3
Prepare 52M sintered NdFeBs
First, it is formulated dispensing by 52M, by ingot casting, broken, milling, magnetic field orientating, compression moulding, obtains neodymium iron boron life
Base.
Then green compact are packed into vacuum sintering furnace, are evacuated to vacuum degree and are less than 0.2Pa, neodymium iron boron magnetic body green compact is existed
After 180 DEG C carry out first time constant temperature firing 80min, the first intermediate is obtained；Then the first intermediate above-mentioned steps obtained
After carrying out second of constant temperature firing 70min at 480 DEG C, the second intermediate is obtained；The second intermediate that above-mentioned steps are obtained again
After carrying out third time constant temperature firing 150min at 790 DEG C, neodymium iron boron magnetic body intermediate is obtained.
It is right after the neodymium iron boron magnetic body intermediate that above-mentioned steps are obtained again carries out constant temperature liquid-phase sintering 30min at 1038 DEG C
Above-mentioned neodymium iron boron magnetic body intermediate is flushed with hydrogen 0.08MPa, under the action of above-mentioned be flushed with hydrogen, is closed after logical hydrogen constant temperature liquid-phase sintering 35min
Close charge valve, liquid-phase sintering intermediate；
Then continue to be sintered 60min at this temperature, stop heating, into cooling stage, gas is flushed with hydrogen into sintering furnace extremely
0.085-0.98Mpa, machine air blast of blowing in are cooled to 60 DEG C and come out of the stove, and it is 53*37*32mm to obtain specification (differently- oriented directivity is 32 sizes)
Neodymium iron boron magnetic body blank.
Finally, with surface grinding machine that oriented surface one side 60% is light-exposed, it is glued on iron staff with 502, is cut with inside diameter slicer
At 14*6*3.2 (M) black-film, with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.2mm with automatic chamfering machine, remove edge
Burr, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 10 μm to obtain zinc coating thickness, size 14*6*3.2
(M) neodymium iron boron magnetic body finished product.
The neodymium iron boron magnetic body that above-mentioned steps obtain is observed using XJ-63 type metallographic microscopes, as a result such as Fig. 7 institutes
Show, Fig. 7 is the metallurgical microstructrue figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3；From figure 7 it can be seen that the present embodiment
The neodymium iron boron magnetic body crystal grain being prepared significantly is densified, the neodymium iron boron magnetic body prepared through survey calculation, the embodiment of the present invention 3
Crystal grain average value is 4.63 μm.
The magnetic property and magnet density of the neodymium iron boron magnetic body product obtained to above-mentioned steps are detected, experimental result ginseng
See that Fig. 8, Fig. 8 are the normal temperature magnetic performance data figure of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.Referring to table 10, table 10 is real
Apply the magnetic property data of the neodymium iron boron magnetic body of the preparation of example 3 at ambient and elevated temperatures.
The magnetic property data of neodymium iron boron magnetic body prepared by 10 embodiment 3 of table at ambient and elevated temperatures
Other performance detections are carried out to neodymium iron boron magnetic body manufactured in the present embodiment, referring to table 11, table 11 is that the present invention is implemented
The ingredient situation of neodymium iron boron magnetic body prepared by example 3.
Equipment：ICP.
The ingredient situation of neodymium iron boron magnetic body prepared by 11 embodiment of the present invention 3 of table
| Total amount of rare earth | |
| Formula | 30 |
| It is flushed with hydrogen sintering process | 29.8 |
| Normal sintering process | 28.6 |
As shown in Table 11, the neodymium iron boron magnetic body that prepared by the embodiment of the present invention 3 compares prior art, and the rare earth consumption of magnet is special
It is not few.
Referring to table 12, table 12 is the aging conditions of neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar；
Equipment：HAST ageing ovens
The aging conditions of neodymium iron boron magnetic body prepared by 12 embodiment of the present invention 3 of table
| Weightlessness/mg/cm2 | |
| It is flushed with hydrogen sintering process | 0.6 |
Can be, it is evident that neodymium iron boron magnetic body sintering method provided by the invention by above-mentioned testing result, it can be apparent
The magnet performances such as remanent magnetism, coercivity, maximum magnetic energy product, the squareness of magnet are improved, and there is preferable high-temperature stability.
A kind of sintering method of neodymium iron boron magnetic body provided by the present invention is described in detail above.It is used herein
Principle and implementation of the present invention are described for a specific example, and the explanation of above example is only intended to help to manage
Solve the method and its core concept of the present invention.It should be pointed out that for those skilled in the art, not departing from
, can be with several improvements and modifications are made to the present invention under the premise of the principle of the invention, these improvement and modification also fall into this hair
In bright scope of the claims.
Claims (8)
1. a kind of sintering method of neodymium iron boron magnetic body, comprises the steps of：
A it) under conditions of vacuum or protective gas, by neodymium iron boron magnetic body green compact after continuous warming or ladder-elevating temperature, reaches
Sintering temperature obtains neodymium iron boron magnetic body intermediate；
B) under conditions of hydrogen, after the neodymium iron boron magnetic body intermediate progress constant temperature firing that above-mentioned steps are obtained, neodymium iron is obtained
Boron magnet blank；
The pressure of the hydrogen is 0.052~0.098MPa；
The step B) further include that the neodymium iron boron magnetic body intermediate after firing constant temperature is cooled down under conditions of hydrogen, obtained
To neodymium iron boron magnetic body blank.
2. sintering method according to claim 1, which is characterized in that the sintering temperature is 1000~1100 DEG C.
3. sintering method according to claim 1, which is characterized in that the heating rate of the continuous warming is 0.5~3
℃/min；The time of the continuous warming is 15~120min.
4. sintering method according to claim 1, which is characterized in that the ladder-elevating temperature the specific steps are：
A1) under conditions of vacuum or protective gas, after neodymium iron boron magnetic body green compact are carried out first time constant temperature firing, first is obtained
Intermediate；
A2 after the first intermediate) and then by above-mentioned steps obtained carries out second of constant temperature firing, the second intermediate is obtained；
A3 after) the second intermediate for again obtaining above-mentioned steps carries out third time constant temperature firing, neodymium iron boron magnetic body intermediate is obtained.
5. sintering method according to claim 4, which is characterized in that the temperature that the first time constant temperature is fired is 200~
250℃；The time that the first time constant temperature is fired is 90~150min；
The temperature that second of the constant temperature is fired is 450~550 DEG C；The time that second of the constant temperature is fired is 60~
120min；
The temperature that the third time constant temperature is fired is 750~850 DEG C；The time that second of the constant temperature is fired is 90~
120min。
6. sintering method according to claim 1, which is characterized in that described to be specially under conditions of hydrogen：
It is directly filled with hydrogen into equipment, or the protective gas in agglomerating plant is first evacuated to vacuum, then into agglomerating plant
It is filled with hydrogen.
7. sintering method according to claim 6, which is characterized in that the pressure of the vacuum is less than or equal to 10Pa.
8. sintering method according to claim 1, which is characterized in that the rate of the cooling is 6.0~8.5 DEG C/min.
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| CN113593799B (en) * | 2020-04-30 | 2023-06-13 | 烟台正海磁性材料股份有限公司 | Fine-grain high-coercivity sintered NdFeB magnet and preparation method thereof |
| CN114171314B (en) * | 2022-02-10 | 2022-04-26 | 京磁材料科技股份有限公司 | Preparation method of high-performance sintered neodymium-iron-boron permanent magnet |
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| EP1486989A1 (en) * | 2000-09-19 | 2004-12-15 | Neomax Co., Ltd. | Method for manufacturing a rear earth magnet |
| CN101246773A (en) * | 2007-02-12 | 2008-08-20 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
| CN102601367A (en) * | 2011-01-24 | 2012-07-25 | 北京中科三环高技术股份有限公司 | Heat treatment method of radiation or multi-pole orientation magnet ring |
| CN105097261A (en) * | 2015-08-20 | 2015-11-25 | 京磁新材料有限公司 | Neodymium-iron-boron magnet sintering method |
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| CN103422012A (en) * | 2012-11-13 | 2013-12-04 | 宁波宏垒磁业有限公司 | Preparation method of NdFeB magnetic material |
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| EP1486989A1 (en) * | 2000-09-19 | 2004-12-15 | Neomax Co., Ltd. | Method for manufacturing a rear earth magnet |
| CN101246773A (en) * | 2007-02-12 | 2008-08-20 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
| CN102601367A (en) * | 2011-01-24 | 2012-07-25 | 北京中科三环高技术股份有限公司 | Heat treatment method of radiation or multi-pole orientation magnet ring |
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