CN104134529B - A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet and preparation method and application - Google Patents
A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet and preparation method and application Download PDFInfo
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Abstract
The invention belongs to powder metallurgy and magnet preparation field, disclose a kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet and preparation method and application.Described preparation method comprises the steps: to make the neodymium iron boron powder densification shaping of rich neodymium obtain thermal deformation presoma by high velocity compacted, then described thermal deformation presoma is carried out thermal deformation, obtains described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.Preparation method high velocity compacted shaping efficiency of the present invention is high, and moment makes powder densification, can improve production efficiency；Described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet magnet density and magnetic property are excellent, can be applicable to the fields such as consumer electronics, sound equipment, engine, wind-powered electricity generation, field of traffic, computer and high-performing car motor.
Description
Technical field
The invention belongs to powder metallurgy and magnet preparation field, be specifically related to a kind of anisotropy nanocrystalline neodymium iron
Boron magnet and preparation method and application.
Background technology
With neodymium iron boron magnetic body (Nd2Fe14B) be the third generation rare earth permanent-magnetic material of representative be that magnetic property is the highest, application
Permanent-magnet material the widest, with the fastest developing speed.Owing to neodymium iron boron magnetic body has high saturation and magnetic intensity, high each
The opposite sex advantage such as field and high energy product, audio device, automotive field, oil field paraffin removal, medical device,
The fields such as computer suffer from being widely applied.The global demand to rare-earth Nd-Fe-B series permanent magnetic material is year by year
Being incremented by, every year on average with the speed increment of 1,000,000 tons, development potentiality is big, has good Market Situation.
Although China is rare earth storage capacity big country, but China mainly produces low and middle-end magnet, and high-end magnet will be to
The imports such as the U.S. and Japan.China's a large amount of outlet rare earth mineral products money during 10 years of nineteen ninety-five to 2005 year
Source, causes the loss on foreign exchange of 10,000,000,000 dollars to China.Improve the technology of preparing of China's high performance magnet not only
Only there is great economic worth, more contribute to make China become rare earth power.Nd2Fe14B compound has
There is the strongest unit anisotropy, with Nd2Fe14B is in the compound permanent-magnet material of matrix, works as Nd2Fe14B
Crystal grain c-axis disorientation time, crystal is isotropic, its Jr=0.5Js, (BH)max=0.5 (Js/2)2；When
Nd2Fe14During the crystal grain c-axis rule orientating of B, crystal is anisotropic, its Jr≈Js, (BH)max=0.25Js 2。
Obviously, the magnetic property of anisotropic permanent magnet is more much higher than isotropic permanent magnet.
High velocity compacting technique is SwedenThe Paul Skoglund of AB company proposes, in calendar year 2001
One released June shapes new technology safely and efficiently.The operating process of high velocity compacting technique is unidirectional with routine
Suppress very much like: in the case of speed is 2～30m/s, powder is carried out high energy hammering, strong shock wave
Compacting makes powdered metallurgical material reach high density.Compared with tradition compacting, high velocity compacting technique has high fine and close
The advantages such as degree, low cost and shaping are fast, high velocity compacted powder keeps original crystal grain substantially the most at normal temperatures
Size and structure.Therefore high velocity compacting technique is of great interest, the most successfully apply iron powder,
The preparation of the materials such as titanium valve, 316L stainless steel powder, copper powder and polymer, be also used in preparing soft magnetic materials and
HRRD Magnaglo.
The preparation method of anisotropic neodymium iron boron magnetic body mainly has powder metallurgic method and thermal deformation method, powder metallurgy
The anisotropy magnet of system preparation is owing to inevitably containing cavity and non-magnetic phase, thus can make magnet
Heat endurance.Corrosion resistance and fracture toughness decline.And thermal deformation is first by densified for Magnaglo, so
After by the magnet after densified by jumping-up, extrude and the method such as rolling deforms so that after thermal deformation each to
It is tough that opposite sex magnet has the features such as the most tiny grain structure structure and consistency, its heat endurance and fracture
Degree is higher than traditional sintered magnet.Thermal deformation is in anisotropic neodymium iron boron magnetic body, and the existence of rich neodymium phase rises
Vital effect, if not having rich neodymium phase in magnet, being difficult to even may deformation.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention is to provide a kind of equipment work
Skill is simple, productivity is high, with low cost, save the preparation side of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet of the energy
Method；
Another object of the present invention is to the anisotropy Nano crystal neodymium, boron magnetic providing above-mentioned preparation method to obtain
Body；
It is still another object of the present invention to provide the application of above-mentioned anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of a kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, comprises the steps: by high ram compression
System makes the neodymium iron boron powder densification shaping of rich neodymium obtain thermal deformation presoma, then by described thermal deformation forerunner
Body carries out thermal deformation, obtains described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
Preferably, in the neodymium iron boron powder of described rich neodymium, the mass fraction of neodymium is 29.2～33wt%；
It is furthermore preferred that the content of main element is in the neodymium iron boron powder of described rich neodymium: Nd:29.2～31wt%,
FeCoAl:67.8～70wt%, B:1 ± 0.2wt%；
Preferably, the concretely comprising the following steps of the preparation method of above-mentioned anisotropy nano-crystalline neodymium-iron-boronmagnet magnet:
(1) at mold cavity surface and the surface smear lubricant of upper and lower tringle of compacting tool set；
(2) the neodymium iron boron powder of described rich neodymium is filled in the die cavity of compacting tool set, carries out high velocity compacted,
The demoulding obtains compacting sample, is thermal deformation presoma；
(3) being placed in hot pressing furnace by described thermal deformation presoma and carry out thermal deformation, thermal deformation cools down after completing,
Take out finished product, be described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
In the concrete steps of above-mentioned preparation method:
Preferably, the internal diameter of described compacting tool set is 12～16mm；
Preferably, described lubricating oil be the alcohol suspension of zinc stearate, the alcohol suspension of calcium stearate or
Vaseline；
Preferably, precompressed 2min before carrying out high velocity compacted；
Preferably, described high velocity compacted employing single-impact is compressing or repeat impact is compressing；
Preferably, the quality energy of the neodymium iron boron powder of rich neodymium in controlling the die cavity of compacting tool set in high velocity compacted
Density is more than 160J/g；It is furthermore preferred that the neodymium iron boron of rich neodymium in controlling the die cavity of compacting tool set in high velocity compacted
The quality energy density of powder is 160～300J/g；
Quality energy density, the i.e. rolled-up stock of unit mass impact energy in pressing process, under can passing through
Formula calculates: I=E/m, in formula, I is quality energy density, and unit is J/g；E is the impact energy of compacting, unit
For burnt (J)；M is the loading of the neodymium iron boron powder of described rich neodymium, and unit is gram (g).
Preferably, before described thermal deformation presoma carries out thermal deformation, first carry out jacket with sheath material；
The internal diameter size of sheath material, height and thermal deformation presoma are in the same size, or sheath material internal diameter
Ratio thermal deformation presoma external diameter big 2～3mm, the lowest 2～3mm；
Preferably, described sheath material is H65 brass, fine copper or iron；
Preferably, the temperature of described thermal deformation is 680～900 DEG C, and deflection is 15～80%；
It is furthermore preferred that the deflection of described thermal deformation is 15～40%.
A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet obtained according to above-mentioned preparation method.
Above-mentioned anisotropy nano-crystalline neodymium-iron-boronmagnet magnet can be applicable at consumer electronics, sound equipment, engine, wind
Electricity and field of traffic, be particularly applicable to computer and high-performing car technical field of motors.
The present invention has such advantages as relative to prior art and effect:
(1) generally by conventional sintering, electric spark plasma agglomeration or hot pressing in traditional thermal deformation technique
Make powder densification formed blocks etc. method, then carry out thermal deformation；And preparation method of the present invention uses
Under normal temperature, high velocity compacted shaping, has saved substantial amounts of energy, and in thermal deformation, nanocrystal is substantially without growing up,
Can well keep the institutional framework of starting powder.
(2) preparation method high velocity compacted shaping efficiency of the present invention is high, and moment makes powder densification, can carry
High product production efficiency.
(3) preparation method of the present invention uses high velocity compacted shaping, it is to avoid should in sinter molding method
The decline of the magnetic property that crystal grain is grown up and caused, general sintered magnet be all grain size be all micron order, and
Magnet prepared by high velocity compacted still can keep the nanocrystalline grain size size of original powder.
(4) high velocity compacted that preparation method of the present invention uses is shaped to only be molded, without any bonding
Agent, has more preferable magnetic property than anisotropic Agglutinate neodymium-iron-boron magnet.
(5) preparation method of the present invention is except using the neodymium iron boron powder of rich neodymium to prepare anisotropy nanometer
Brilliant neodymium-iron-boron is external, and the neodymium iron boron powder of routine and lean rare-earth Nd-Fe-B powder also can be used to be prepared.
(6) preparation method technique of the present invention is simple, with low cost, is suitable for producing in enormous quantities.
(7) anisotropy nano-crystalline neodymium-iron-boronmagnet magnet magnet density of the present invention and magnetic property are excellent.From height
The magnet maximum magnetic energy product (BH) that ram compression preparesmax=65 (kJ/m3), maximum magnetic energy product after 40% deflection
(BH)max=120 (kJ/m3) nearly double, heighten the magnetic energy product of magnet greatly, remained in that relatively simultaneously
High coercivity Hci=784 (kA/m).
Accompanying drawing explanation
Fig. 1 is the installation diagram of the compacting tool set of internal diameter Ф=12mm in embodiment 2.
Fig. 2 is the quality energy density I correlation figure to high velocity compacted magnet density.
Fig. 3 is cylindrical magnet and the XRD of 40% heat distortion amount magnet after high velocity compacted.
Fig. 4 is high velocity compacted magnet and 15% deflection magnet hysteresis curve figure.
Fig. 5 is high velocity compacted magnet and 40% deflection magnet hysteresis curve figure.
Fig. 6 is embodiment 2 12mm cylindrical magnet vertical plane SEM figure after high velocity compacted.
Fig. 7 is the SEM figure of embodiment 2 12mm cylindrical magnet horizontal plane after high velocity compacted.
Fig. 8 is the SEM figure that embodiment 2 gained magnet after thermal deformation 40% deflection is parallel to pressure direction.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
This.
The present invention uses high velocity compacted machine, and starting powder is rich neodymium neodymium iron boron powder, and hot pressing furnace is HP-12
× 12 × 12, U.S. Centorr Vacuum Industries.
Embodiment 1
A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, its preparation method is as follows:
(1) preparing neodymium iron boron flakelike powder, essential element mass fraction is respectively 29.2wt%Nd, 69.8wt%
(FeCoAl), 1wt%B；Select the compacting tool set of internal diameter Ф=16mm, uniform at mold cavity and upper and lower tringle
Coat zinc stearate alcoholic solution, until after vaporized alcohol, ready neodymium iron boron flakelike powder carefully
Put mold cavity into, and shake mould and make powder be uniformly distributed as far as possible, filling amount m=12.21g；
(2) according to impact energy E of quality energy Auto-regulating System of Density of Heavy Medium high velocity compacted machine, the upper tringle of record jump bit impact
Spot speed, determine impact energy size.Use twice high velocity compacted, selection impact energy E=320J for the first time,
E=386J carries out high velocity compacted for the second time；Use a high velocity compacted, use successively 1500J, 1581J, 1768J,
Five kinds of impact energys of 1987J and 2113J carry out the high velocity compacted then demoulding and take out compacting examination the mould of step (1)
Sample；
(3) it is wrapped in consistency with the H65 brass of internal diameter 16mm, wall thickness 1mm, highly 9.7mm
High compacting sample, writes hot pressing furnace thermal deformation program.Thermal deformation conditions: 750 DEG C of insulation 10min, deformation speed
Rate is 0.001s-1, take out thermal deformation finished product after hot pressing furnace cooling by the time, now it is observed that specimen height reduces
For 8mm, along pressure method, relatively small deformation occurring, deflection is about 15%；Gained thermal deformation finished product is institute
State anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
Embodiment 2
A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, its preparation method is as follows:
(1) preparing neodymium iron boron flakelike powder, essential element mass fraction is respectively 29.2wt%Nd, 69.8wt%
(FeCoAl), 1wt%B；Select the compacting tool set of internal diameter Ф=12mm, uniform at mold cavity and upper and lower tringle
Coat zinc stearate alcoholic solution, until after vaporized alcohol, ready neodymium iron boron flakelike powder carefully
Put mold cavity into, and shake mould and make powder be uniformly distributed as far as possible, filling amount m=6.91g；Internal diameter Ф=12mm
Compacting tool set installation diagram as shown in Figure 1；
(2) according to impact energy E of quality energy Auto-regulating System of Density of Heavy Medium high velocity compacted machine, the upper tringle of record jump bit impact
Spot speed, determine impact energy size.Use 1227J, 1500J, 1581J, 1768J and 1988J successively
Five kinds of impact energys carry out a high velocity compacted to the mould of step (1), and then compacting sample is taken out in the demoulding；
(3) it is wrapped in compacting consistency with the fine copper of internal diameter 14mm, wall thickness 1mm, highly 6mm the highest
Sample, write hot pressing furnace thermal deformation program.Thermal deformation conditions: 750 DEG C of insulation 8min, hot pressing furnace is cold by the time
Take out thermal deformation finished product the most afterwards, now it is observed that specimen height is reduced to 5mm, occur along pressure method
Substantially deformation, deflection is about 40%；Gained thermal deformation finished product is described anisotropy Nano crystal neodymium, boron magnetic
Body.
Embodiment 3
A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, its preparation method is as follows:
(1) preparing neodymium iron boron flakelike powder, essential element mass fraction is respectively 30.2wt%Nd, 68.8wt%
(FeCoAl), 1wt%B；Select the compacting tool set of internal diameter Ф=16mm, uniform at mold cavity and upper and lower tringle
Coat zinc stearate alcoholic solution, until after vaporized alcohol, ready neodymium iron boron flakelike powder carefully
Put mold cavity into, and shake mould and make powder be uniformly distributed as far as possible, filling amount m=7.69g；
(2) according to impact energy E of quality energy Auto-regulating System of Density of Heavy Medium high velocity compacted machine, the upper tringle of record jump bit impact
Spot speed, determine impact energy size.Use tri-kinds of impact energys of 1191J, 1309J and 1605J to step successively
Suddenly the mould of (1) carries out a high velocity compacted, and then compacting sample is taken out in the demoulding；
(3) do not use jacket, directly in hot pressing furnace to the highest compacting sample of consistency through row thermal deformation,
Write hot pressing furnace thermal deformation program.Thermal deformation conditions: 900 DEG C of insulation 5min, takes out after hot pressing furnace cooling by the time
, now it is observed that specimen height reduces 1mm, there is relatively small deformation along pressure method in thermal deformation finished product,
Deflection is about 18%；Gained thermal deformation finished product is described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
Performance test:
The performance of the anisotropy nano-crystalline neodymium-iron-boronmagnet magnet prepared for above-described embodiment and structure, with scanning
Electronic Speculum, X-ray diffraction, comprehensive physical measurement system etc. characterize and analyze, below in conjunction with accompanying drawing do into
One step explanation.
Fig. 2 is the quality energy density I correlation figure to high velocity compacted magnet density.During high velocity compacted
Dress component and impact energy are all to affect rolled-up stock density important parameter, therefore introduce one and can embody impact energy
The dress component physical quantity quality energy density to rolled-up stock Effects of Density can be embodied again.When I < 160J/g, consistency
Increase along with the increase of quality energy density I, because powder mutual extrusion packing space；When 160 < I < 220J/g,
Consistency is constant, because powder is in compacting equilibrium stage along with the increase of quality energy density I；When
220J/g < I, consistency increases again along with the increase of quality energy density I, because powder is plastically deformed,
Density increases.
Cylindrical magnet and the XRD of 40% heat distortion amount magnet after Fig. 3 high velocity compacted.Essentially all of
Peak is all Nd2Fe14The peak of B phase, when 40% deflection, the crystal face showed increased rotated to c-axis direction,
(004), (105), (314), (006), the peak intensity such as (216) and (008) be remarkably reinforced, embody heat
After deformation, neodymium iron boron magnetic body has anisotropy.
Fig. 4 high velocity compacted magnet and 15% deflection magnet hysteresis curve figure.The magnetic of magnet after high velocity compacted
Can coercivity Hci=1101 (kA/m), remanent magnetism Jr=0.64 (T), maximum magnetic energy product (BH)max=65 (kJ/m3), full
With intensity of magnetization Js,6T=1.13 (T)；The magnetic property coercivity H of 15% heat distortion amount magnetci=965 (kA/m), surplus
Magnetic Jr=0.78 (T), maximum magnetic energy product (BH)max=88 (kJ/m3), saturation magnetization Js,6T=1.34 (T).From figure
In can draw the increase along with deflection, the coercivity H of magnetciReducing, remanent magnetism and saturation magnetization are all
Increasing, magnet starts have anisotropy.
Fig. 5 high velocity compacted magnet and 40% deflection magnet hysteresis curve figure.The magnetic of magnet after high velocity compacted
Can coercivity Hci=1101 (kA/m), remanent magnetism Jr=0.64 (T), maximum magnetic energy product (BH)max=65 (kJ/m3), full
With intensity of magnetization Js,6T=1.13 (T)；40% heat distortion amount magnet magnetic property coercivity Hci=784 (kA/m), remanent magnetism
Jr=0.95 (T), maximum magnetic energy product (BH)max=120 (kJ/m3), saturation magnetization Js,6T=1.47 (T).From height
The magnet maximum magnetic energy product (BH) that ram compression preparesmax=65 (kJ/m3), maximum magnetic energy after 40% deflection
Long-pending (BH)max=120 (kJ/m3) nearly double, heighten the magnetic energy product of magnet greatly, remained in that simultaneously
Higher coercivity Hci=784 (kA/m).This is because during high velocity compacted, powder grain substantially without growing up,
Keep original tissue and structure.
Table 1 starting powder, high velocity compacted magnet, 15% deflection and the magnetic property table of 40% deflection magnet.
Along with the increase of deflection in thermal deformation process, the remanent magnetism of magnet and saturation magnetization increase, and work as deformation
When amount reaches 40%, remanent magnetism Jr=0.64 (T) increases to 0.95 (T), has obvious anisotropy.
Table 1 each sample magnetic parameter
Indicate: 1. this numerical value is the coercivity of the neodymium iron boron powder employed in embodiment 1 and 2, different powder particle sizes
It is slightly different.
Fig. 6 is embodiment 2 12mm cylindrical magnet vertical plane SEM figure after high velocity compacted.Powder is sheet
Shape the most closely is heaped, and the direction of heap is the most parallel with pressure direction.
Fig. 7 is the SEM figure of embodiment 2 12mm cylindrical magnet horizontal plane after high velocity compacted.Powder with
Powder edge compact siro spinning technology, but still have cavity.
Fig. 8 is the SEM figure that embodiment 2 gained magnet after thermal deformation 40% deflection is parallel to pressure direction.?
During thermal deformation, powder grain is vertical and pressure direction grows, and c-axis tends to parallel pressure direction.From microstructure
After thermal deformation is described, magnet has anisotropy, high velocity compacted and thermal deformation and can successfully prepare each to different
Property nano-crystal neodymium iron boron magnetic body.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned enforcement
The restriction of example, the change made, modifies, replaces under other any Spirit Essence without departing from the present invention and principle
In generation, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1. the preparation method of an anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, it is characterised in that include as follows
Step:
(1) at mold cavity surface and the surface smear lubricant of upper and lower tringle of compacting tool set；
(2) the neodymium iron boron powder of rich neodymium is filled in the die cavity of compacting tool set, carries out high velocity compacted, de-
Mould obtains compacting sample, is thermal deformation presoma；
(3) being placed in hot pressing furnace by described thermal deformation presoma and carry out thermal deformation, thermal deformation cools down after completing,
Take out finished product, be described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet；
The matter of the neodymium iron boron powder of rich neodymium in controlling the die cavity of compacting tool set in step (2) described high velocity compacted
Amount can density be 160～300J/g；The temperature of step (3) described thermal deformation is 680～900 DEG C, and deflection is
15～40%；
In the neodymium iron boron powder of described rich neodymium, the content of main element is: Nd:29.2～31wt%, FeCoAl:
67.8～70wt%, B:1 ± 0.2wt%.
The preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet the most according to claim 1, it is special
Levy and be: the internal diameter of described compacting tool set is 12～16mm；Described lubricant is that the alcohol of zinc stearate suspends
Liquid, the alcohol suspension of calcium stearate or vaseline；Precompressed 2min before carrying out high velocity compacted；Described high speed
Compacting employing single-impact is compressing or repeat impact is compressing；Described thermal deformation presoma carries out heat change
Before shape, first carry out jacket with sheath material.
The preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet the most according to claim 2, it is special
Levy and be: described sheath material is H65 brass, fine copper or iron.
4. the anisotropy nanocrystalline neodymium iron obtained according to the preparation method described in any one of claims 1 to 3
Boron magnet.
Anisotropy nano-crystalline neodymium-iron-boronmagnet magnet the most according to claim 4 consumer electronics, sound equipment,
Application in engine, wind-powered electricity generation, field of traffic, computer and high-performing car motor.
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| CN109014187A (en) * | 2018-09-18 | 2018-12-18 | 安徽宁磁电子科技有限公司 | Magnetic ball blank forms whole set of die and its production method |
| CN111403166B (en) * | 2020-04-17 | 2022-08-05 | 成都银河磁体股份有限公司 | Preparation method of hot-pressed magnet and product thereof |
| CN115430836B (en) * | 2022-08-24 | 2023-11-17 | 广东省科学院资源利用与稀土开发研究所 | Preparation method and device of high-abundance rare earth cerium-based anisotropic nanocrystalline magnet |
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