CN103526107B - The method for preparing Sintered NdFeB magnet - Google Patents
The method for preparing Sintered NdFeB magnet Download PDFInfo
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Abstract
The present invention provides a kind of method for preparing Sintered NdFeB magnet, and which comprises the steps：（a）Obtain alloy HREx(Fe0.50Co0.25Cu0.10Al0.15)zZny, wherein, HRE be Dy, Tb and/or Ho, x+y+z=100；（b）Obtain the coarse powder of alloy；（c）Coarse powder is worn into powder of the particle mean size less than 3mm；（d）Powder is added in neodymium iron boron coarse powder by a certain percentage；（e）The powder and neodymium iron boron coarse powder are fully uniformly mixed so as to obtain mixed-powder, by mixed-powder in sealing container heat treatment；（f）After powder cooling to be mixed, fine powder is worn into；（g）By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained；（h）Profiled member is sintered, then carries out timeliness.The method can reduce heavy rare earth usage amount, be applied to large scale function admirable neodymium iron boron magnetic body large-scale production.
Description
Technical field
The present invention relates to a kind of method for preparing Sintered NdFeB magnet.
Background technology
The remanent magnetism and magnetic energy product of the sintered NdFeB being currently known is already close to the 95% of theoretical value.Japanese Neomax companies
Announce, which have developed highest magnetic energy product up to the Sintered NdFeB magnet of 59.5MGOes.German VAC companies report, which have developed
Magnet of the highest magnetic energy product up to 56.7MGOes.Yintai Zhenghai Magnetic Materials Co., Ltd of China announces which is prepared for highest magnetic energy
Product reaches 56MGOes magnets.However, the coercivity highest of the sintered NdFeB being currently known still only has 55% left side of theoretical value
Right.In the magnet product provided on market, Hcj (kOe)+（BH）The magnet product of max (MGOe) ＞ 60 is referred to as high magnetic characteristics magnetic
Body.Domestic minority producer can produce Hcj (kOe)+（BH）The Sintered NdFeB magnet of max (MGOe) ＞ 65.In order to be had
There is sufficiently high coercitive magnet, it usually needs add substantial amounts of heavy rare earth such as dysprosium in magnet（Dy）And terbium（Tb）.However, adding
Although increasing amount Dy or Tb make the coercivity of magnet be improved rapidly, and the remanent magnetism of magnet but drastically declines, so as to fail have
Effect raising Hcj (kOe)+（BH）The value of max (MGOe).
Heavy rare earth element belongs to scarce resource.In the world, heavy rare earth Dy and Tb only have found to be distributed in China at present
The several provinces in south, belong to national strategy resource.In recent years, due to factors such as environmental conservation, China is strengthened to rare earth resources
Protection so that rare earth price be particularly heavy rare earth price escalate, rare earth element has accounted for sintered NdFeB cost
More than 80%, and according to different performance requirements, heavy rare earth element accounts for the 5～50% of Sintered NdFeB magnet cost.It is applied to
The neodymium iron boron magnetic body of the high-end electric system such as automotive hub is required to tolerate 200 celsius temperatures.For this neodymium-iron-boron
Body, heavy rare earth typically constitute from more than the 30% of magnet cost.
Can be seen that from above-mentioned reality, on the one hand, market is to the demand with high-coercive force, the magnet of good temperature-resistance characteristic
It is being continuously increased；On the other hand, the heavy rare earth resource such as Dy, Tb is more and more rare, and price is more and more expensive, in sintered NdFeB
In cost, proportion is increasing.Therefore, in order to environmental protection, save heavy rare earth resource, better adapt to market demand, open
Sending minimizing rare earth particularly usage amount of the heavy rare earth in Sintered NdFeB magnet, the technology of raising heavy rare earth service efficiency is
Vital.
In recent years, countries in the world be particularly Japan to how to reduce usage amount of the heavy rare earth in Sintered NdFeB magnet,
The utilization ratio for improving heavy rare earth has carried out substantial amounts of research.In method disclosed in patent documentation CN1898757A, first will
The powder of the fluoride of rare earth, oxide and oxyfluoride is dispersed in formation serosity, the powder in water solvent or organic solvent
End provides the surface of small-sized or slim magnet as a slurry, then makes the rare earth and fluorine on surface etc. using heat-treating methods
To magnet diffusion inside, do not reduce so as to obtain a kind of remanent magnetism of magnet and magnetic energy product substantially, and coercivity is improved forever
Magnet.Additionally, the method also uses relatively small number of heavy rare earth resource.
Patent documentation CN1905088A discloses one kind and adds nano level heavy rare earth metal in Sintered NdFeB magnet
Powder, the method so as to prepare high-coercivity magnet.
Method disclosed in above-mentioned patent documentation CN1898757 is only applicable to very thin little magnet, it is impossible to for large scale
Magnet, and need special equipment and technique obtain disclosed effect.Disclosed in patent documentation CN1905088A
In method, need to add nanoscale heavy rare earth or heavy rare earth compound powder.However, nanoscale heavy rare earth powder is difficult to obtain,
Few amount can only be obtained in laboratory, be not suitable for large-scale production.Additionally, method effectively cannot be controlled disclosed in above-mentioned document
Distribution of the heavy rare earth processed in magnet, heavy rare earth still major part are entered into inside main phase grain, it is impossible to effectively utilizes heavy rare earth.
Content of the invention
It is an object of the invention to provide a kind of usage amount that can reduce heavy rare earth, the neodymium suitable for large scale function admirable
The method of iron boron magnet large-scale production.
To achieve these goals, the present invention provides a kind of method for preparing Sintered NdFeB magnet, the method include as
Lower step：（a）Obtain alloy HREx(Fe0.50Co0.25Cu0.10Al0.15)zZny, wherein, HRE be Dy, Tb and/or Ho, x+y+z=
100；（b）Obtain the coarse powder of the alloy；（c）The coarse powder is worn into powder of the particle mean size less than 3mm；（d）The powder
End is added in neodymium iron boron coarse powder by a certain percentage；（e）The powder and the neodymium iron boron coarse powder are fully uniformly mixed so as to obtain mixing
Powder, by the mixed-powder in sealing container heat treatment；（f）After mixed-powder cooling, fine powder is worn into；
（g）By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained；（h）The profiled member is sintered,
Timeliness is carried out again.
When the method for the present invention is applied, add weight of the particle mean size less than 3mm in neodymium iron boron powder due to taking
Rare earth alloy powder, then the step of carry out heat treatment to mixed-powder, so as to reaching control magnet micro structure, improving heavy rare earth profit
With rate, the effect of raising Sintered NdFeB magnet magnetic property.Further, since the final neodymium iron boron obtained using the method for the present invention
Magnet is obtained after by powder compacting, and therefore the size and production scale of final products arbitrarily can be set as needed
Fixed.
Description of the drawings
Fig. 1 shows the final Sintered NdFeB magnet for obtaining demagnetizing curve at different temperatures in embodiment 16.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, and embodiments of the invention are merely to illustrate the present invention's
Technical scheme, and the non-limiting present invention.
In following examples and the other parts of the present invention, if no special instructions, the subscript in formula represents respective element
Mass fraction.
Embodiment 1
Alloy Dy is obtained with vacuum induction melting method50(Fe0.50Co0.25Cu0.10Al0.15)47Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 3 hours at 500 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1000 DEG C
Lower sintering 7 hours, then timeliness 5 hours at 450 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=30kOe；Br=0.95kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.9kOe.The composition of the final magnet for obtaining
For Nd27.0Dy5.0Co2.3Al0.9Cu0.5B0.9Zn0.3Febal.
Embodiment 2
Alloy Tb is obtained with vacuum induction melting method50(Fe0.50Co0.25Cu0.10Al0.15)47Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 3 hours at 500 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1000 DEG C
Lower sintering 5 hours, then timeliness 5 hours at 450 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=38kOe；Br=0.96kGs at 180 DEG C, Hcj=11.5kOe, Hk=10.8kOe.The group of the final magnet for obtaining
Become Nd27.0Tb5.0Co2.3Al0.9Cu0.5B0.9Zn0.3Febal.
Embodiment 3
Alloy Ho is obtained with vacuum induction melting method50(Fe0.50Co0.25Cu0.10Al0.15)47Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 3 hours at 500 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1000 DEG C
Lower sintering 7 hours, then timeliness 5 hours at 450 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
11.0kGs, Hcj=17kOe；Br=0.86kGs at 180 DEG C, Hcj=7.5kOe, Hk=6.8kOe.The composition of the final magnet for obtaining
For Nd27.0Ho5.0Co2.3Al0.9Cu0.5B0.9Zn0.3Febal.
Embodiment 4
Alloy Dy is obtained with vacuum induction melting method90(Fe0.50Co0.25Cu0.10Al0.15)7Zn3.Then by hydrogen crush method,
Obtain the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is added by a certain percentage
To the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully uniformly mixed so as to obtain mixed
Close powder, by mixed-powder in sealing container heat treatment 3 hours at 500 DEG C.After powder cooling to be mixed, will with airflow milling
Which wears into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.Profiled member is burnt at 1000 DEG C
Knot 7 hours, then timeliness 5 hours at 450 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.6kGs, Hcj=27kOe；Br=0.98kGs at 180 DEG C, Hcj=9.2kOe, Hk=8.5kOe.The composition of the final magnet for obtaining
For Nd28.5Dy4.5Co1.2Al0.2Cu0.1B0.95Zn0.15Febal.
Embodiment 5
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 3 hours at 500 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1000 DEG C
Lower sintering 7 hours, then timeliness 5 hours at 450 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.0kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The composition of the final magnet for obtaining
For Nd27.6Dy5.6Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 6
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 1000 DEG C.After powder cooling to be mixed, gas is used
Stream is worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1100
Sinter 3 hours at DEG C, then timeliness 5 hours at 650 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Under room temperature
Br=12.0kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The final magnet for obtaining
Consist of Nd27.6Dy5.6Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 7
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050 DEG C
Lower sintering 3 hours, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The composition of the final magnet for obtaining
For Nd27.6Dy5.6Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 8
Alloy Dy is obtained with vacuum induction melting method50Tb20(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Broken method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is pressed a definite proportion
Example is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Obtain mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, gas is used
Stream is worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050
Sinter 3 hours at DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Under room temperature
Br=12.5kGs, Hcj=33kOe；Br=0.96kGs at 180 DEG C, Hcj=10.5kOe, Hk=9.4kOe.The final magnet for obtaining
Consist of Nd27.6Dy4.0Tb1.6Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 9
Alloy Dy is obtained with vacuum induction melting method50Ho20(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Broken method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is pressed a definite proportion
Example is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Obtain mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, gas is used
Stream is worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050
Sinter 3 hours at DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Under room temperature
Br=12.0kGs, Hcj=27kOe；Br=0.93kGs at 180 DEG C, Hcj=9.2kOe, Hk=8.3kOe.The final magnet for obtaining
Consist of Nd27.6Dy4.0Ho1.6Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 10
Alloy Dy is obtained with vacuum induction melting method50Tb10Ho10(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then pass through
Hydrogen crush method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is pressed one
Certainty ratio is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Will be abundant for two kinds of powder
Be uniformly mixed so as to obtain mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed,
Fine powder is worn into airflow milling.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in
Sinter 3 hours at 1050 DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Often
Temperature lower Br=12.3kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The final magnetic for obtaining
Body consists of Nd27.6Dy4.0Tb0.8Ho0.8Co1.6Al0.5Cu0.3B0.92Zn0.24Febal.
Embodiment 11
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)21Zn9.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
To mixed-powder, mixed-powder heat treatment 1 hour at 700 DEG C in sealing container will be stated.After powder cooling to be mixed, gas is used
Stream is worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050
Sinter 3 hours at DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Under room temperature
Br=12.6kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The final magnet for obtaining
Consist of Nd27.9Dy4.9Co1.5Al0.4Cu0.24B0.93Zn0.6Febal.
Embodiment 12
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)23Zn7.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050 DEG C
Lower sintering 3 hours, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The composition of the final magnet for obtaining
For Nd27.9Dy4.9Co1.5Al0.4Cu0.25B0.93Zn0.5Febal.
Embodiment 13
Alloy Dy is obtained with vacuum induction melting method50(Fe0.50Co0.25Cu0.10Al0.15)47Sn3.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050 DEG C
Lower sintering 3 hours, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The composition of the final magnet for obtaining
For Nd27.0Dy5.0Co2.3Al0.9Cu0.5B0.9Sn0.3Febal.
Embodiment 14
Alloy Dy is obtained with vacuum induction melting method90(Fe0.50Co0.25Cu0.10Al0.15)7Sn3.Then by hydrogen crush method,
Obtain the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is added by a certain percentage
To the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully uniformly mixed so as to obtain mixed
Close powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, will with airflow milling
Which wears into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.Profiled member is burnt at 1050 DEG C
Knot 3 hours, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.6kGs, Hcj=27kOe；Br=0.98kGs at 180 DEG C, Hcj=9.2kOe, Hk=8.5kOe.The composition of the final magnet for obtaining
For Nd28.5Dy4.5Co1.2Al0.2Cu0.1B0.95Sn0.15Febal.
Embodiment 15
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)21Sn9.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen30Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Two kinds of powder are fully mixed
Arrive mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed, air-flow is used
Worn into fine powder.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in 1050 DEG C
Lower sintering 3 hours, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Br=under room temperature
12.3kGs, Hcj=30kOe；Br=0.96kGs at 180 DEG C, Hcj=9.5kOe, Hk=8.8kOe.The composition of the final magnet for obtaining
For Nd27.9Dy4.9Co1.5Al0.4Cu0.24B0.93Sn0.6Febal.
Embodiment 16
Alloy Dy is obtained with vacuum induction melting method60Tb10(Fe0.50Co0.25Cu0.10Al0.15)27Zn3.Then broken by hydrogen
Broken method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.Powder is pressed a definite proportion
Example is added to the neodymium iron boron Nd obtained with the broken method of hydrogen26Dy4Co1.2Al0.2Cu0.1B1.0FebalCoarse powder in.Will be abundant for two kinds of powder
Be uniformly mixed so as to obtain mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed,
Fine powder is worn into airflow milling.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in
Sinter 3 hours at 1050 DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Often
Temperature lower Br=12.3kGs, Hcj=33kOe；Br=0.99kGs at 180 DEG C, Hcj=10.5kOe, Hk=9.0kOe.Finally obtain
Magnet consist of Nd24.7Dy6.3Tb1.0Co1.5Al0.4Cu0.21B0.95Zn0.15Febal.
Embodiment 17
Alloy Dy is obtained with vacuum induction melting method70(Fe0.50Co0.25Cu0.10Al0.15)21Zn9.Then broken by hydrogen
Method, obtains the coarse powder of alloy.Coarse powder is worn into powder of the particle mean size less than 3mm with ball-milling method again.By powder by a certain percentage
It is added to the neodymium iron boron Nd obtained with the broken method of hydrogen25.8Dy4.2Co1.3Al0.3Cu0.1B1.0FebalCoarse powder in.Will be abundant for two kinds of powder
Be uniformly mixed so as to obtain mixed-powder, by mixed-powder in sealing container heat treatment 1 hour at 700 DEG C.After powder cooling to be mixed,
Fine powder is worn into airflow milling.By fine powder molding in the sealing system for having nitrogen protection, profiled member is obtained.By profiled member in
Sinter 3 hours at 1050 DEG C, then timeliness 5 hours at 600 DEG C.The following Sintered NdFeB magnet of final acquisition magnetic property：Often
Temperature lower Br=12.2kGs, Hcj=35kOe；Br=0.98kGs at 180 DEG C, Hcj=11.5kOe, Hk=10.3kOe.Final acquisition
Magnet consists of Nd24.5Dy7.5Co1.5Al0.4Cu0.21B0.95Zn0.4Febal.
Comparative example 1
Using the i.e. direct smelting process of the traditional method for preparing following Sintered NdFeB magnets, prepare and averagely consist of
Nd24.7Dy6.3Tb1.0Co1.5Al0.4Cu0.21B0.95Ga0.15FebalMagnet：Raw material is prepared according to above-mentioned formula, is put into together
Induction melting furnace melting, then crushes ingot casting, molding, and 1060 DEG C sinter 5 hours, and 500 DEG C of timeliness 5 hours finally obtain hair
Base finished product.
The magnetic property of neodymium iron boron magnetic body prepared by the traditional method is：Br=11.9kGs under room temperature, Hcj=28kOe；180
Br=0.92kGs at DEG C, Hcj=9.5kOe, Hk=8.0kOe.
Comparative example 2
Using the traditional method for preparing following Sintered NdFeB magnets, preparation is consisted of
Nd22.5Dy9.5Co1.5Al0.4Cu0.21B0.95Ga0.3FebalMagnet：Raw material is prepared according to above-mentioned formula, sensing is put into together molten
Furnace melting, then crushes ingot casting, molding, and 1060 DEG C sinter 5 hours, and 500 DEG C of timeliness 5 hours finally obtain blank finished product,
Finally the magnet performance of acquisition is：Br=11.4kGs under room temperature, Hcj=30kOe；Br=0.95kGs, Hcj=at 180 DEG C
9.8kOe, Hk=8.7kOe.
From embodiment 1～17 as can be seen that the good neodymium iron boron magnetic body of magnetic property can be obtained with the method for the present invention.These
Most of embodiment in embodiment can obtain the following magnet of performance：Br >=12.2kGs under room temperature, Hcj >=30kOe；180℃
Lower Br >=0.96kGs, Hcj >=9.5kOe, Hk >=8.8kOe.
From comparative example 1 and embodiment 16 as can be seen that the composition of the neodymium iron boron magnetic body finally obtained in two is except comparing
Ga in example 1 replaces outside the Zn in embodiment 16, and other compositions are basically identical, however, the magnetic property difference of two kinds of magnets is larger,
The magnet performance obtained in embodiment 16 is more excellent.
From comparative example 2 and embodiment 17 as can be seen that the composition of the magnet product finally obtained in two is close to, rare earth is total
Amount is identical.However, the magnet of 2 final acquisition of comparative example is N33EH magnets, and the magnet of 17 final acquisition of embodiment is N38EH
Magnet, that is to say, that the magnetic property of the magnet that embodiment 17 is obtained is more excellent.And, the magnet obtained in embodiment 17
Dy contents are 7.5wt.%, and the Dy contents of the magnet obtained in comparative example 2 reach 9.5wt.%, based on current price
Calculate, embodiment 17 obtains magnet escapable cost 20% or so.
Although it should be noted that embodiment used above illustrates the present invention, the invention is not restricted to embodiment.Ability
Field technique personnel within the spirit and scope of the present invention, can carry out various modifications, replacement or improvement to the present invention.The guarantor of the present invention
Shield scope is defined by claims.
Claims (9)
1. a kind of method for preparing Sintered NdFeB magnet, it is characterised in that methods described comprises the steps：
A () obtains alloy HREx(Fe0.50Co0.25Cu0.10Al0.15)zZny, wherein, HRE be Dy, Tb and/or Ho, x+y+z=100,
50≤x≤90,3≤y≤9；
B () obtains the coarse powder of the alloy；
C the coarse powder is worn into powder of the particle mean size less than 3mm by ()；
D () is added to the powder in neodymium iron boron coarse powder by a certain percentage；
E the powder and the neodymium iron boron coarse powder are fully uniformly mixed so as to obtain mixed-powder by (), the mixed-powder is held in sealing
Heat treatment in device；
F () is worn into fine powder after mixed-powder cooling；
G fine powder molding in the sealing system for having nitrogen protection is obtained profiled member by ()；
H the profiled member is sintered by (), then carry out timeliness.
2. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that step (a) adopts vacuum
Induction melting.
3. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that step (b) is broken using hydrogen
Broken method.
4. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that step (c) adopts ball milling
Method.
5. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that in step (d), described
Neodymium iron boron coarse powder is obtained with hydrogen crush method.
6. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that in step (f), described
Fine powder is worn into airflow milling.
7. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that the heat treatment is 500
Carry out at～1000 DEG C 1～3 hour.
8. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that described be sintered in 1000～
Carry out at 1100 DEG C 3～7 hours.
9. the method for preparing Sintered NdFeB magnet according to claim 1, it is characterised in that the timeliness 450～
Carry out at 650 DEG C 5 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0517179A1 (en) * | 1991-06-04 | 1992-12-09 | Shin-Etsu Chemical Co., Ltd. | Method of making two phase Rare Earth permanent magnets |
| EP0789367A1 (en) * | 1996-02-09 | 1997-08-13 | Crucible Materials Corporation | Method for producing selected grades of rare earth magnets using a plurality of particle batches |
| CN1628182A (en) * | 2002-02-05 | 2005-06-15 | 株式会社新王磁材 | Sinter magnet made from rare earth-iron-boron alloy powder for magnet |
| CN102473515A (en) * | 2009-07-15 | 2012-05-23 | 日立金属株式会社 | Process for production of r-t-b based sintered magnets and r-t-b based sintered magnets |
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| JP4529180B2 (en) * | 2005-03-30 | 2010-08-25 | Ｔｄｋ株式会社 | Rare earth permanent magnet |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0517179A1 (en) * | 1991-06-04 | 1992-12-09 | Shin-Etsu Chemical Co., Ltd. | Method of making two phase Rare Earth permanent magnets |
| EP0789367A1 (en) * | 1996-02-09 | 1997-08-13 | Crucible Materials Corporation | Method for producing selected grades of rare earth magnets using a plurality of particle batches |
| CN1628182A (en) * | 2002-02-05 | 2005-06-15 | 株式会社新王磁材 | Sinter magnet made from rare earth-iron-boron alloy powder for magnet |
| CN102473515A (en) * | 2009-07-15 | 2012-05-23 | 日立金属株式会社 | Process for production of r-t-b based sintered magnets and r-t-b based sintered magnets |
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